# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Xiu-Feng Hou ' _publ_contact_author_email 'xfhou@fudan.edu.cn ' _publ_author_name 'Xiu-Feng Hou' data_mo_10519b_0ma _database_code_depnum_ccdc_archive 'CCDC 872878' #TrackingRef 'Crystallographic Information__ File.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H23 Cl2 N3 Pd' _chemical_formula_weight 494.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.9571(17) _cell_length_b 14.9440(15) _cell_length_c 19.461(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4931.6(9) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9820 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 27.57 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.333 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2000 _exptl_absorpt_coefficient_mu 0.978 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8284 _exptl_absorpt_correction_T_max 0.8752 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker 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_% 4.33 _diffrn_reflns_number 34264 _diffrn_reflns_av_R_equivalents 0.0229 _diffrn_reflns_av_sigmaI/netI 0.0156 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 27.58 _reflns_number_total 5681 _reflns_number_gt 5022 _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. In asymmetric unit of 4a, there were disordered CH3CN molecules which could not be restrained properly. Therefore, SQUEEZE algorithm was used to omit them. ; _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^)+(0.0408P)^2^+6.5506P] 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 5681 _refine_ls_number_parameters 249 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0354 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0875 _refine_ls_wR_factor_gt 0.0842 _refine_ls_goodness_of_fit_ref 1.122 _refine_ls_restrained_S_all 1.122 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 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 0.289 0.146 0.242 115.1 21.3 2 0.789 0.146 0.258 115.2 21.3 3 0.289 0.354 0.742 115.0 21.1 4 0.789 0.354 0.758 115.2 21.4 5 0.211 0.646 0.242 115.0 21.6 6 0.711 0.646 0.258 115.2 21.4 7 0.211 0.854 0.742 115.2 21.3 8 0.711 0.854 0.758 115.1 21.3 _platon_squeeze_details ; ; 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 Pd1 Pd 0.145461(9) 0.378257(11) 0.320518(8) 0.01909(7) Uani 1 1 d . . . Cl1 Cl 0.02431(3) 0.35126(4) 0.37346(3) 0.02838(13) Uani 1 1 d . . . Cl2 Cl 0.08624(4) 0.38257(5) 0.21465(3) 0.03513(15) Uani 1 1 d . . . N1 N 0.20409(11) 0.38228(12) 0.41246(10) 0.0205(4) Uani 1 1 d . . . N2 N 0.30805(11) 0.38885(13) 0.34077(10) 0.0231(4) Uani 1 1 d . . . N3 N 0.29902(12) 0.39058(15) 0.23104(11) 0.0294(4) Uani 1 1 d . . . C1 C 0.16575(13) 0.37936(15) 0.47872(11) 0.0212(4) Uani 1 1 d . . . C2 C 0.12805(13) 0.45738(16) 0.50197(12) 0.0241(4) Uani 1 1 d . . . C3 C 0.08596(14) 0.45289(18) 0.56337(13) 0.0294(5) Uani 1 1 d . . . H3 H 0.0607 0.5052 0.5802 0.035 Uiso 1 1 calc R . . C4 C 0.08007(14) 0.37403(18) 0.60043(13) 0.0303(5) Uani 1 1 d . . . C5 C 0.11721(15) 0.29788(18) 0.57582(12) 0.0302(5) Uani 1 1 d . . . H5 H 0.1135 0.2438 0.6012 0.036 Uiso 1 1 calc R . . C6 C 0.16017(14) 0.29887(17) 0.51431(12) 0.0251(5) Uani 1 1 d . . . C7 C 0.13042(15) 0.54265(17) 0.46098(14) 0.0317(5) Uani 1 1 d . . . H7A H 0.1046 0.5331 0.4165 0.048 Uiso 1 1 calc R . . H7B H 0.1854 0.5604 0.4535 0.048 Uiso 1 1 calc R . . H7C H 0.1028 0.5900 0.4862 0.048 Uiso 1 1 calc R . . C8 C 0.03088(19) 0.3699(2) 0.66569(16) 0.0462(8) Uani 1 1 d . . . H8A H 0.0299 0.4290 0.6875 0.069 Uiso 1 1 calc R . . H8B H 0.0541 0.3263 0.6974 0.069 Uiso 1 1 calc R . . H8C H -0.0231 0.3516 0.6542 0.069 Uiso 1 1 calc R . . C9 C 0.19673(18) 0.21420(18) 0.48714(14) 0.0372(6) Uani 1 1 d . . . H9A H 0.1876 0.2102 0.4375 0.056 Uiso 1 1 calc R . . H9B H 0.1728 0.1625 0.5100 0.056 Uiso 1 1 calc R . . H9C H 0.2536 0.2148 0.4962 0.056 Uiso 1 1 calc R . . C10 C 0.27979(13) 0.38538(14) 0.40832(12) 0.0210(4) Uani 1 1 d . . . C11 C 0.33859(13) 0.38698(16) 0.46415(12) 0.0234(4) Uani 1 1 d . . . C12 C 0.33883(14) 0.45701(17) 0.51137(12) 0.0265(5) Uani 1 1 d . . . H12 H 0.2989 0.5015 0.5096 0.032 Uiso 1 1 calc R . . C13 C 0.39757(15) 0.46171(17) 0.56099(13) 0.0307(5) Uani 1 1 d . . . H13 H 0.3977 0.5100 0.5928 0.037 Uiso 1 1 calc R . . C14 C 0.45624(14) 0.39660(17) 0.56482(13) 0.0285(5) Uani 1 1 d . . . C15 C 0.45450(15) 0.32605(18) 0.51823(13) 0.0316(5) Uani 1 1 d . . . H15 H 0.4932 0.2803 0.5212 0.038 Uiso 1 1 calc R . . C16 C 0.39710(15) 0.32149(17) 0.46755(13) 0.0307(5) Uani 1 1 d . . . H16 H 0.3976 0.2739 0.4352 0.037 Uiso 1 1 calc R . . C17 C 0.52055(17) 0.4027(2) 0.61799(16) 0.0404(6) Uani 1 1 d . . . H17A H 0.5676 0.4298 0.5974 0.061 Uiso 1 1 calc R . . H17B H 0.5334 0.3426 0.6347 0.061 Uiso 1 1 calc R . . H17C H 0.5025 0.4398 0.6565 0.061 Uiso 1 1 calc R . . C18 C 0.25447(14) 0.38833(16) 0.28794(12) 0.0246(5) Uani 1 1 d . . . C19 C 0.27150(18) 0.3909(2) 0.15949(15) 0.0455(8) Uani 1 1 d . . . H19A H 0.2225 0.3564 0.1560 0.068 Uiso 1 1 calc R . . H19B H 0.3118 0.3638 0.1300 0.068 Uiso 1 1 calc R . . H19C H 0.2619 0.4526 0.1447 0.068 Uiso 1 1 calc R . . C20 C 0.37897(16) 0.3935(2) 0.24756(14) 0.0343(6) Uani 1 1 d . . . H20 H 0.4214 0.3960 0.2157 0.041 Uiso 1 1 calc R . . C21 C 0.38562(15) 0.39214(18) 0.31582(13) 0.0290(5) Uani 1 1 d . . . H21 H 0.4329 0.3932 0.3420 0.035 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 Pd1 0.01586(10) 0.02390(11) 0.01750(10) 0.00144(6) 0.00010(5) 0.00021(6) Cl1 0.0183(2) 0.0414(3) 0.0255(3) 0.0030(2) 0.0010(2) -0.0012(2) Cl2 0.0255(3) 0.0586(4) 0.0213(3) 0.0027(2) -0.0036(2) -0.0013(3) N1 0.0180(8) 0.0237(9) 0.0197(9) 0.0005(7) 0.0001(7) 0.0000(7) N2 0.0171(9) 0.0308(10) 0.0214(9) -0.0011(7) 0.0019(7) -0.0008(7) N3 0.0247(10) 0.0426(12) 0.0209(10) -0.0009(8) 0.0040(8) -0.0020(8) C1 0.0162(9) 0.0296(12) 0.0179(10) 0.0008(8) -0.0002(8) 0.0011(8) C2 0.0215(10) 0.0257(11) 0.0252(11) -0.0029(9) -0.0018(9) 0.0001(8) C3 0.0206(10) 0.0380(13) 0.0296(12) -0.0074(10) 0.0016(9) 0.0048(9) C4 0.0216(11) 0.0460(15) 0.0234(12) -0.0031(10) 0.0028(9) 0.0010(10) C5 0.0318(12) 0.0354(13) 0.0234(11) 0.0063(10) 0.0030(9) -0.0009(10) C6 0.0235(10) 0.0293(12) 0.0223(11) 0.0008(9) -0.0005(8) 0.0014(9) C7 0.0299(12) 0.0251(12) 0.0402(14) 0.0028(10) -0.0002(10) 0.0040(9) C8 0.0372(15) 0.074(2) 0.0275(13) -0.0002(13) 0.0098(12) 0.0060(14) C9 0.0471(16) 0.0274(12) 0.0371(14) 0.0042(10) 0.0106(12) 0.0059(11) C10 0.0208(10) 0.0214(10) 0.0207(10) 0.0001(8) -0.0014(8) 0.0021(8) C11 0.0177(10) 0.0290(11) 0.0235(11) -0.0006(9) -0.0009(8) -0.0009(8) C12 0.0240(10) 0.0290(12) 0.0265(12) -0.0031(9) -0.0015(9) 0.0029(9) C13 0.0298(12) 0.0322(13) 0.0302(12) -0.0083(10) -0.0045(10) -0.0002(10) C14 0.0240(11) 0.0360(13) 0.0256(12) 0.0004(10) -0.0054(9) -0.0034(9) C15 0.0253(11) 0.0356(13) 0.0339(13) 0.0000(10) -0.0060(10) 0.0073(10) C16 0.0293(12) 0.0312(12) 0.0314(13) -0.0055(10) -0.0045(10) 0.0045(10) C17 0.0315(14) 0.0493(16) 0.0403(15) -0.0034(13) -0.0125(12) -0.0045(12) C18 0.0226(11) 0.0311(12) 0.0201(11) 0.0007(9) 0.0018(9) 0.0002(9) C19 0.0358(15) 0.079(2) 0.0216(13) 0.0007(13) 0.0042(11) -0.0057(14) C20 0.0231(11) 0.0487(16) 0.0311(13) -0.0006(11) 0.0091(10) -0.0035(11) C21 0.0168(11) 0.0408(14) 0.0293(12) -0.0017(10) 0.0040(9) 0.0001(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 Pd1 C18 1.960(2) . ? Pd1 N1 2.0478(19) . ? Pd1 Cl2 2.2929(6) . ? Pd1 Cl1 2.3335(6) . ? N1 C10 1.287(3) . ? N1 C1 1.445(3) . ? N2 C18 1.372(3) . ? N2 C10 1.400(3) . ? N2 C21 1.403(3) . ? N3 C18 1.341(3) . ? N3 C20 1.394(3) . ? N3 C19 1.469(3) . ? C1 C6 1.391(3) . ? C1 C2 1.405(3) . ? C2 C3 1.393(3) . ? C2 C7 1.504(3) . ? C3 C4 1.385(4) . ? C3 H3 0.9500 . ? C4 C5 1.386(4) . ? C4 C8 1.521(4) . ? C5 C6 1.401(3) . ? C5 H5 0.9500 . ? C6 C9 1.505(3) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.475(3) . ? C11 C12 1.393(3) . ? C11 C16 1.395(3) . ? C12 C13 1.389(3) . ? C12 H12 0.9500 . ? C13 C14 1.394(4) . ? C13 H13 0.9500 . ? C14 C15 1.391(4) . ? C14 C17 1.506(3) . ? C15 C16 1.388(3) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.333(4) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? 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 C18 Pd1 N1 79.78(9) . . ? C18 Pd1 Cl2 96.91(7) . . ? N1 Pd1 Cl2 175.50(6) . . ? C18 Pd1 Cl1 170.56(7) . . ? N1 Pd1 Cl1 92.67(6) . . ? Cl2 Pd1 Cl1 90.92(2) . . ? C10 N1 C1 120.38(19) . . ? C10 N1 Pd1 115.51(15) . . ? C1 N1 Pd1 124.09(14) . . ? C18 N2 C10 118.47(19) . . ? C18 N2 C21 111.2(2) . . ? C10 N2 C21 130.3(2) . . ? C18 N3 C20 111.0(2) . . ? C18 N3 C19 127.2(2) . . ? C20 N3 C19 121.8(2) . . ? C6 C1 C2 121.8(2) . . ? C6 C1 N1 120.1(2) . . ? C2 C1 N1 117.9(2) . . ? C3 C2 C1 118.0(2) . . ? C3 C2 C7 120.6(2) . . ? C1 C2 C7 121.3(2) . . ? C4 C3 C2 121.6(2) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C3 C4 C5 119.1(2) . . ? C3 C4 C8 120.6(2) . . ? C5 C4 C8 120.3(2) . . ? C4 C5 C6 121.5(2) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C1 C6 C5 118.0(2) . . ? C1 C6 C9 121.6(2) . . ? C5 C6 C9 120.4(2) . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N1 C10 N2 113.7(2) . . ? N1 C10 C11 129.0(2) . . ? N2 C10 C11 117.4(2) . . ? C12 C11 C16 119.6(2) . . ? C12 C11 C10 120.0(2) . . ? C16 C11 C10 120.3(2) . . ? C13 C12 C11 119.9(2) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C14 120.9(2) . . ? C12 C13 H13 119.5 . . ? C14 C13 H13 119.5 . . ? C15 C14 C13 118.6(2) . . ? C15 C14 C17 120.6(2) . . ? C13 C14 C17 120.7(2) . . ? C16 C15 C14 121.0(2) . . ? C16 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C15 C16 C11 119.9(2) . . ? C15 C16 H16 120.1 . . ? C11 C16 H16 120.1 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N3 C18 N2 104.2(2) . . ? N3 C18 Pd1 143.17(19) . . ? N2 C18 Pd1 112.50(16) . . ? N3 C19 H19A 109.5 . . ? N3 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N3 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 N3 108.2(2) . . ? C21 C20 H20 125.9 . . ? N3 C20 H20 125.9 . . ? C20 C21 N2 105.4(2) . . ? C20 C21 H21 127.3 . . ? N2 C21 H21 127.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C18 Pd1 N1 C10 -2.69(17) . . . . ? Cl2 Pd1 N1 C10 -45.5(8) . . . . ? Cl1 Pd1 N1 C10 171.59(16) . . . . ? C18 Pd1 N1 C1 179.06(18) . . . . ? Cl2 Pd1 N1 C1 136.2(6) . . . . ? Cl1 Pd1 N1 C1 -6.65(16) . . . . ? C10 N1 C1 C6 -80.5(3) . . . . ? Pd1 N1 C1 C6 97.7(2) . . . . ? C10 N1 C1 C2 105.8(2) . . . . ? Pd1 N1 C1 C2 -76.0(2) . . . . ? C6 C1 C2 C3 1.6(3) . . . . ? N1 C1 C2 C3 175.2(2) . . . . ? C6 C1 C2 C7 -176.3(2) . . . . ? N1 C1 C2 C7 -2.7(3) . . . . ? C1 C2 C3 C4 -0.9(3) . . . . ? C7 C2 C3 C4 177.1(2) . . . . ? C2 C3 C4 C5 0.2(4) . . . . ? C2 C3 C4 C8 -177.4(2) . . . . ? C3 C4 C5 C6 -0.3(4) . . . . ? C8 C4 C5 C6 177.3(3) . . . . ? C2 C1 C6 C5 -1.7(3) . . . . ? N1 C1 C6 C5 -175.2(2) . . . . ? C2 C1 C6 C9 176.4(2) . . . . ? N1 C1 C6 C9 3.0(3) . . . . ? C4 C5 C6 C1 1.0(4) . . . . ? C4 C5 C6 C9 -177.1(2) . . . . ? C1 N1 C10 N2 -179.39(18) . . . . ? Pd1 N1 C10 N2 2.3(2) . . . . ? C1 N1 C10 C11 -0.3(4) . . . . ? Pd1 N1 C10 C11 -178.64(18) . . . . ? C18 N2 C10 N1 -0.2(3) . . . . ? C21 N2 C10 N1 -179.5(2) . . . . ? C18 N2 C10 C11 -179.4(2) . . . . ? C21 N2 C10 C11 1.3(3) . . . . ? N1 C10 C11 C12 -61.1(3) . . . . ? N2 C10 C11 C12 118.0(2) . . . . ? N1 C10 C11 C16 122.8(3) . . . . ? N2 C10 C11 C16 -58.1(3) . . . . ? C16 C11 C12 C13 0.6(4) . . . . ? C10 C11 C12 C13 -175.5(2) . . . . ? C11 C12 C13 C14 -0.7(4) . . . . ? C12 C13 C14 C15 -0.6(4) . . . . ? C12 C13 C14 C17 179.0(3) . . . . ? C13 C14 C15 C16 1.9(4) . . . . ? C17 C14 C15 C16 -177.7(3) . . . . ? C14 C15 C16 C11 -1.9(4) . . . . ? C12 C11 C16 C15 0.7(4) . . . . ? C10 C11 C16 C15 176.8(2) . . . . ? C20 N3 C18 N2 -0.7(3) . . . . ? C19 N3 C18 N2 179.8(3) . . . . ? C20 N3 C18 Pd1 -175.9(3) . . . . ? C19 N3 C18 Pd1 4.6(5) . . . . ? C10 N2 C18 N3 -179.0(2) . . . . ? C21 N2 C18 N3 0.5(3) . . . . ? C10 N2 C18 Pd1 -2.0(3) . . . . ? C21 N2 C18 Pd1 177.39(16) . . . . ? N1 Pd1 C18 N3 177.4(3) . . . . ? Cl2 Pd1 C18 N3 -5.7(3) . . . . ? Cl1 Pd1 C18 N3 140.1(3) . . . . ? N1 Pd1 C18 N2 2.40(16) . . . . ? Cl2 Pd1 C18 N2 179.31(16) . . . . ? Cl1 Pd1 C18 N2 -34.9(6) . . . . ? C18 N3 C20 C21 0.6(3) . . . . ? C19 N3 C20 C21 -179.8(3) . . . . ? N3 C20 C21 N2 -0.3(3) . . . . ? C18 N2 C21 C20 -0.1(3) . . . . ? C10 N2 C21 C20 179.3(2) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.608 _refine_diff_density_min -1.007 _refine_diff_density_rms 0.083 #===END #compound 5a data_a10517c _database_code_depnum_ccdc_archive 'CCDC 872879' #TrackingRef 'Crystallographic Information__ File.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C31 H38 Cl Ir N3), 0.5(C H2 Cl2),(Cl),1.5(H2 O)' _chemical_formula_sum 'C31.50 H42 Cl3 Ir N3 O1.50' _chemical_formula_weight 785.23 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' Cl Cl 0.1484 0.1585 '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 C2/c _symmetry_space_group_name_Hall '-C 2yc' 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 41.54(3) _cell_length_b 11.423(5) _cell_length_c 32.26(2) _cell_angle_alpha 90.00 _cell_angle_beta 113.60(4) _cell_angle_gamma 90.00 _cell_volume 14025(14) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 938 _cell_measurement_theta_min 2.388 _cell_measurement_theta_max 23.689 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.488 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6272 _exptl_absorpt_coefficient_mu 4.065 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5807 _exptl_absorpt_correction_T_max 0.7369 _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_reflns_number 24896 _diffrn_reflns_av_R_equivalents 0.0627 _diffrn_reflns_av_sigmaI/netI 0.0801 _diffrn_reflns_limit_h_min -49 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 25.01 _reflns_number_total 12350 _reflns_number_gt 7897 _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, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. There is a large largest residual density peak near the Ir1 because of the terminal effect of heavy atom. The hydrogen atoms on water molecules were not located due to the partial occupations. Command "isor" is used to restraint C61 and C62 due to the disorders in their terminal positions. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1023P)^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 12350 _refine_ls_number_parameters 765 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0972 _refine_ls_R_factor_gt 0.0596 _refine_ls_wR_factor_ref 0.1784 _refine_ls_wR_factor_gt 0.1544 _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_restrained_S_all 0.992 _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 0.112041(10) 0.97140(4) 0.058790(13) 0.04771(14) Uani 1 1 d . . . Ir2 Ir 0.134430(12) 0.54847(3) 0.415330(16) 0.05711(16) Uani 1 1 d . . . N1 N 0.1516(2) 0.5344(6) 0.3610(3) 0.0483(19) Uani 1 1 d . . . N2 N 0.0762(3) 0.3586(8) 0.3722(4) 0.074(3) Uani 1 1 d . . . N3 N 0.1061(2) 0.4066(7) 0.3347(3) 0.059(2) Uani 1 1 d . . . N4 N 0.0582(2) 1.1690(8) 0.0514(3) 0.059(2) Uani 1 1 d . . . N5 N 0.0883(2) 1.1024(7) 0.1177(3) 0.0493(19) Uani 1 1 d . . . N6 N 0.13160(18) 0.9734(6) 0.1307(2) 0.0391(17) Uani 1 1 d . . . Cl1 Cl 0.14370(8) 1.1488(3) 0.05896(10) 0.0707(8) Uani 1 1 d . . . Cl2 Cl 0.16551(9) 0.3714(3) 0.44917(12) 0.0786(9) Uani 1 1 d . . . Cl3 Cl 0.01931(12) 0.8954(5) 0.10764(19) 0.154(2) Uani 1 1 d . . . Cl4 Cl 0.00889(17) 0.4719(6) 0.4608(3) 0.182(3) Uani 1 1 d . . . Cl5 Cl 0.22883(13) 0.0580(5) 0.4525(2) 0.156(2) Uani 1 1 d . . . Cl6 Cl 0.24542(11) 0.1956(4) 0.38882(15) 0.1211(14) Uani 1 1 d . . . C1 C 0.0806(3) 1.0838(9) 0.0722(4) 0.053(3) Uani 1 1 d . . . C2 C 0.0454(3) 1.1981(12) 0.0027(4) 0.077(4) Uani 1 1 d . . . H2A H 0.0580 1.1527 -0.0109 0.116 Uiso 1 1 calc R . . H2B H 0.0490 1.2799 -0.0007 0.116 Uiso 1 1 calc R . . H2C H 0.0207 1.1805 -0.0118 0.116 Uiso 1 1 calc R . . C3 C 0.0506(3) 1.2363(10) 0.0834(4) 0.065(3) Uani 1 1 d . . . H3 H 0.0348 1.2982 0.0767 0.077 Uiso 1 1 calc R . . C4 C 0.0696(3) 1.1969(9) 0.1236(4) 0.057(3) Uani 1 1 d . . . H4 H 0.0704 1.2262 0.1509 0.069 Uiso 1 1 calc R . . C5 C 0.1161(2) 1.0398(7) 0.1488(3) 0.041(2) Uani 1 1 d . . . C6 C 0.1246(3) 1.0544(8) 0.1979(3) 0.047(2) Uani 1 1 d . . . C7 C 0.0974(3) 1.0423(9) 0.2129(4) 0.060(3) Uani 1 1 d . . . H7 H 0.0746 1.0269 0.1923 0.072 Uiso 1 1 calc R . . C8 C 0.1049(3) 1.0538(9) 0.2589(4) 0.058(3) Uani 1 1 d . . . H8 H 0.0872 1.0441 0.2693 0.069 Uiso 1 1 calc R . . C9 C 0.1385(3) 1.0792(9) 0.2890(4) 0.062(3) Uani 1 1 d . . . C10 C 0.1641(3) 1.0888(9) 0.2736(3) 0.054(3) Uani 1 1 d . . . H10 H 0.1870 1.1031 0.2943 0.065 Uiso 1 1 calc R . . C11 C 0.1578(3) 1.0781(8) 0.2278(3) 0.050(2) Uani 1 1 d . . . H11 H 0.1760 1.0870 0.2181 0.060 Uiso 1 1 calc R . . C12 C 0.1470(4) 1.0921(13) 0.3398(4) 0.094(4) Uani 1 1 d . . . H12A H 0.1651 1.0375 0.3565 0.141 Uiso 1 1 calc R . . H12B H 0.1263 1.0766 0.3451 0.141 Uiso 1 1 calc R . . H12C H 0.1550 1.1704 0.3493 0.141 Uiso 1 1 calc R . . C13 C 0.1580(2) 0.8901(8) 0.1593(3) 0.044(2) Uani 1 1 d . . . C14 C 0.1460(2) 0.7923(8) 0.1772(3) 0.042(2) Uani 1 1 d . . . C15 C 0.1715(3) 0.7109(9) 0.2028(4) 0.057(3) Uani 1 1 d . . . H15 H 0.1647 0.6466 0.2151 0.069 Uiso 1 1 calc R . . C16 C 0.2075(3) 0.7245(9) 0.2104(4) 0.062(3) Uani 1 1 d . . . C17 C 0.2169(2) 0.8182(9) 0.1923(4) 0.058(3) Uani 1 1 d . . . H17 H 0.2404 0.8274 0.1976 0.069 Uiso 1 1 calc R . . C18 C 0.1932(2) 0.9018(9) 0.1659(4) 0.052(2) Uani 1 1 d . . . C19 C 0.1094(2) 0.7759(9) 0.1713(3) 0.053(3) Uani 1 1 d . . . H19A H 0.1042 0.6937 0.1700 0.080 Uiso 1 1 calc R . . H19B H 0.0940 0.8126 0.1436 0.080 Uiso 1 1 calc R . . H19C H 0.1060 0.8105 0.1963 0.080 Uiso 1 1 calc R . . C20 C 0.2332(3) 0.6334(12) 0.2384(5) 0.090(4) Uani 1 1 d . . . H20A H 0.2279 0.5597 0.2227 0.136 Uiso 1 1 calc R . . H20B H 0.2314 0.6255 0.2670 0.136 Uiso 1 1 calc R . . H20C H 0.2566 0.6568 0.2432 0.136 Uiso 1 1 calc R . . C21 C 0.2053(3) 1.0028(11) 0.1469(4) 0.068(3) Uani 1 1 d . . . H21A H 0.2305 1.0081 0.1612 0.101 Uiso 1 1 calc R . . H21B H 0.1951 1.0736 0.1521 0.101 Uiso 1 1 calc R . . H21C H 0.1982 0.9917 0.1149 0.101 Uiso 1 1 calc R . . C22 C 0.0946(3) 0.7916(8) 0.0403(4) 0.055(3) Uani 1 1 d . . . C23 C 0.1306(3) 0.7985(9) 0.0447(4) 0.058(3) Uani 1 1 d . . . C24 C 0.1314(3) 0.8811(11) 0.0122(4) 0.069(3) Uani 1 1 d . . . C25 C 0.0975(3) 0.9301(10) -0.0115(3) 0.061(3) Uani 1 1 d . . . C26 C 0.0740(3) 0.8706(10) 0.0036(3) 0.060(3) Uani 1 1 d . . . C27 C 0.0781(3) 0.7024(10) 0.0593(4) 0.080(4) Uani 1 1 d . . . H27A H 0.0656 0.6462 0.0363 0.119 Uiso 1 1 calc R . . H27B H 0.0620 0.7403 0.0696 0.119 Uiso 1 1 calc R . . H27C H 0.0960 0.6632 0.0843 0.119 Uiso 1 1 calc R . . C28 C 0.1595(3) 0.7232(11) 0.0752(5) 0.092(4) Uani 1 1 d . . . H28A H 0.1619 0.6560 0.0588 0.138 Uiso 1 1 calc R . . H28B H 0.1543 0.6983 0.1002 0.138 Uiso 1 1 calc R . . H28C H 0.1811 0.7668 0.0863 0.138 Uiso 1 1 calc R . . C29 C 0.1642(4) 0.9108(14) 0.0050(6) 0.116(6) Uani 1 1 d . . . H29A H 0.1844 0.8817 0.0299 0.174 Uiso 1 1 calc R . . H29B H 0.1660 0.9942 0.0031 0.174 Uiso 1 1 calc R . . H29C H 0.1630 0.8754 -0.0226 0.174 Uiso 1 1 calc R . . C30 C 0.0875(4) 1.0056(14) -0.0512(4) 0.105(5) Uani 1 1 d . . . H30A H 0.1025 1.0731 -0.0440 0.157 Uiso 1 1 calc R . . H30B H 0.0635 1.0300 -0.0601 0.157 Uiso 1 1 calc R . . H30C H 0.0898 0.9633 -0.0755 0.157 Uiso 1 1 calc R . . C31 C 0.0347(3) 0.8769(12) -0.0145(4) 0.089(4) Uani 1 1 d . . . H31A H 0.0264 0.9392 -0.0362 0.134 Uiso 1 1 calc R . . H31B H 0.0276 0.8915 0.0099 0.134 Uiso 1 1 calc R . . H31C H 0.0248 0.8041 -0.0288 0.134 Uiso 1 1 calc R . . C32 C 0.1008(3) 0.4338(8) 0.3726(4) 0.056(3) Uani 1 1 d . . . C33 C 0.0635(4) 0.3443(13) 0.4077(5) 0.097(5) Uani 1 1 d . . . H33A H 0.0831 0.3451 0.4366 0.146 Uiso 1 1 calc R . . H33B H 0.0513 0.2711 0.4037 0.146 Uiso 1 1 calc R . . H33C H 0.0478 0.4073 0.4062 0.146 Uiso 1 1 calc R . . C34 C 0.0665(3) 0.2884(11) 0.3349(5) 0.087(4) Uani 1 1 d . . . H34 H 0.0497 0.2292 0.3276 0.105 Uiso 1 1 calc R . . C35 C 0.0846(3) 0.3177(10) 0.3108(5) 0.075(4) Uani 1 1 d . . . H35 H 0.0831 0.2851 0.2836 0.090 Uiso 1 1 calc R . . C36 C 0.1337(3) 0.4663(8) 0.3283(4) 0.053(3) Uani 1 1 d . . . C37 C 0.1387(3) 0.4403(8) 0.2859(4) 0.052(3) Uani 1 1 d . . . C38 C 0.1112(3) 0.4468(10) 0.2453(4) 0.067(3) Uani 1 1 d . . . H38 H 0.0889 0.4653 0.2434 0.081 Uiso 1 1 calc R . . C39 C 0.1171(4) 0.4253(10) 0.2066(5) 0.075(3) Uani 1 1 d . . . H39 H 0.0979 0.4281 0.1790 0.090 Uiso 1 1 calc R . . C40 C 0.1485(3) 0.4007(10) 0.2061(4) 0.063(3) Uani 1 1 d . . . C41 C 0.1754(3) 0.3919(9) 0.2477(5) 0.071(3) Uani 1 1 d . . . H41 H 0.1976 0.3723 0.2493 0.085 Uiso 1 1 calc R . . C42 C 0.1713(3) 0.4108(9) 0.2874(4) 0.059(3) Uani 1 1 d . . . H42 H 0.1903 0.4036 0.3150 0.070 Uiso 1 1 calc R . . C43 C 0.1524(4) 0.3782(12) 0.1620(5) 0.092(4) Uani 1 1 d . . . H43A H 0.1615 0.4470 0.1535 0.137 Uiso 1 1 calc R . . H43B H 0.1299 0.3592 0.1388 0.137 Uiso 1 1 calc R . . H43C H 0.1683 0.3141 0.1660 0.137 Uiso 1 1 calc R . . C44 C 0.1763(2) 0.6142(7) 0.3544(3) 0.043(2) Uani 1 1 d . . . C45 C 0.1633(3) 0.7029(8) 0.3216(4) 0.052(3) Uani 1 1 d . . . C46 C 0.1873(3) 0.7810(9) 0.3175(4) 0.067(3) Uani 1 1 d . . . H46 H 0.1794 0.8402 0.2959 0.081 Uiso 1 1 calc R . . C47 C 0.2238(4) 0.7728(11) 0.3454(5) 0.077(4) Uani 1 1 d . . . C48 C 0.2350(3) 0.6902(10) 0.3764(4) 0.064(3) Uani 1 1 d . . . H48 H 0.2588 0.6862 0.3948 0.077 Uiso 1 1 calc R . . C49 C 0.2116(3) 0.6060(9) 0.3825(4) 0.056(3) Uani 1 1 d . . . C50 C 0.2261(3) 0.5136(11) 0.4183(4) 0.078(3) Uani 1 1 d . . . H50A H 0.2256 0.5414 0.4461 0.117 Uiso 1 1 calc R . . H50B H 0.2499 0.4962 0.4228 0.117 Uiso 1 1 calc R . . H50C H 0.2121 0.4439 0.4089 0.117 Uiso 1 1 calc R . . C51 C 0.1252(3) 0.7158(9) 0.2890(4) 0.069(3) Uani 1 1 d . . . H51A H 0.1190 0.7972 0.2854 0.103 Uiso 1 1 calc R . . H51B H 0.1104 0.6749 0.3007 0.103 Uiso 1 1 calc R . . H51C H 0.1221 0.6833 0.2602 0.103 Uiso 1 1 calc R . . C52 C 0.2495(4) 0.8597(12) 0.3393(6) 0.114(5) Uani 1 1 d . . . H52A H 0.2448 0.9369 0.3472 0.170 Uiso 1 1 calc R . . H52B H 0.2468 0.8591 0.3083 0.170 Uiso 1 1 calc R . . H52C H 0.2731 0.8377 0.3584 0.170 Uiso 1 1 calc R . . C53 C 0.0980(3) 0.6659(10) 0.4277(4) 0.068(3) Uani 1 1 d . . . C54 C 0.1201(3) 0.6087(10) 0.4696(4) 0.060(3) Uani 1 1 d . . . C55 C 0.1551(3) 0.6463(12) 0.4808(5) 0.079(4) Uani 1 1 d . . . C56 C 0.1541(5) 0.7221(12) 0.4450(7) 0.097(5) Uani 1 1 d . . . C57 C 0.1203(5) 0.7307(10) 0.4124(5) 0.080(4) Uani 1 1 d . . . C58 C 0.0592(3) 0.6631(13) 0.4061(4) 0.095(4) Uani 1 1 d . . . H58A H 0.0503 0.7417 0.3998 0.143 Uiso 1 1 calc R . . H58B H 0.0503 0.6263 0.4261 0.143 Uiso 1 1 calc R . . H58C H 0.0518 0.6196 0.3784 0.143 Uiso 1 1 calc R . . C59 C 0.1075(4) 0.5447(11) 0.5015(4) 0.084(4) Uani 1 1 d . . . H59A H 0.1158 0.4654 0.5052 0.126 Uiso 1 1 calc R . . H59B H 0.0822 0.5449 0.4891 0.126 Uiso 1 1 calc R . . H59C H 0.1163 0.5833 0.5303 0.126 Uiso 1 1 calc R . . C60 C 0.1854(4) 0.6135(15) 0.5229(6) 0.118(6) Uani 1 1 d . . . H60A H 0.1793 0.6241 0.5483 0.178 Uiso 1 1 calc R . . H60B H 0.2051 0.6622 0.5264 0.178 Uiso 1 1 calc R . . H60C H 0.1913 0.5330 0.5211 0.178 Uiso 1 1 calc R . . C61 C 0.1860(5) 0.7931(17) 0.4448(6) 0.140(7) Uani 1 1 d U . . H61A H 0.1871 0.7859 0.4158 0.211 Uiso 1 1 calc R . . H61B H 0.2072 0.7632 0.4678 0.211 Uiso 1 1 calc R . . H61C H 0.1833 0.8740 0.4508 0.211 Uiso 1 1 calc R . . C62 C 0.1094(5) 0.8152(15) 0.3750(6) 0.122(6) Uani 1 1 d U . . H62A H 0.1013 0.8855 0.3840 0.183 Uiso 1 1 calc R . . H62B H 0.0907 0.7822 0.3491 0.183 Uiso 1 1 calc R . . H62C H 0.1290 0.8331 0.3675 0.183 Uiso 1 1 calc R . . C63 C 0.2426(6) 0.1880(16) 0.4432(6) 0.143(7) Uani 1 1 d . . . H63A H 0.2655 0.2040 0.4668 0.171 Uiso 1 1 calc R . . H63B H 0.2265 0.2479 0.4447 0.171 Uiso 1 1 calc R . . O2 O 0.0299(3) 0.2618(19) 0.1994(6) 0.099(7) Uani 0.50 1 d P . . O3 O 0.0128(4) 0.501(2) 0.1950(7) 0.113(7) Uani 0.50 1 d P . . H1O3 H 0.0087 0.5240 0.2176 0.135 Uiso 0.50 1 d PR . . H2O3 H 0.0082 0.5580 0.1765 0.135 Uiso 0.50 1 d PR . . O4 O 0.0429(5) 0.5949(19) 0.2834(7) 0.110(6) Uani 0.50 1 d P . . O5 O 0.0315(4) 0.600(2) 0.1243(6) 0.121(8) Uani 0.50 1 d P . . H1O5 H 0.0263 0.5465 0.1043 0.145 Uiso 0.50 1 d PR . . H2O5 H 0.0252 0.5758 0.1450 0.145 Uiso 0.50 1 d PR . . O6 O 0.9914(5) 0.0708(19) 0.1478(7) 0.123(8) Uani 0.50 1 d P . . H1O6 H 1.0064 0.1010 0.1719 0.147 Uiso 0.50 1 d PR . . H2O6 H 1.0004 0.0703 0.1283 0.147 Uiso 0.50 1 d PR . . O1 O 0.0000 0.113(3) 0.2500 0.143(12) Uiso 0.50 2 d SP . . O1' O 0.0295(10) 0.801(3) 0.2098(13) 0.102(12) Uiso 0.25 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.0427(2) 0.0592(3) 0.0458(2) -0.00278(18) 0.02249(17) -0.01113(18) Ir2 0.0651(3) 0.0453(2) 0.0793(3) -0.0003(2) 0.0482(3) -0.00200(19) N1 0.050(5) 0.038(4) 0.063(5) -0.001(4) 0.030(4) 0.001(4) N2 0.072(6) 0.057(6) 0.115(9) -0.007(6) 0.063(6) -0.010(5) N3 0.060(5) 0.043(5) 0.087(7) -0.009(4) 0.042(5) -0.005(4) N4 0.048(5) 0.063(5) 0.059(6) 0.013(5) 0.014(4) 0.002(4) N5 0.044(5) 0.050(5) 0.053(5) -0.004(4) 0.017(4) -0.001(4) N6 0.028(4) 0.050(4) 0.039(4) -0.004(3) 0.013(3) -0.009(3) Cl1 0.0677(18) 0.0678(17) 0.080(2) 0.0092(15) 0.0327(15) -0.0218(14) Cl2 0.089(2) 0.0593(16) 0.099(2) 0.0209(16) 0.0497(19) 0.0096(16) Cl3 0.091(3) 0.183(5) 0.154(5) -0.024(4) 0.015(3) 0.007(3) Cl4 0.160(5) 0.178(6) 0.228(7) -0.002(5) 0.097(5) -0.031(4) Cl5 0.107(3) 0.168(5) 0.189(6) 0.078(4) 0.057(3) 0.004(3) Cl6 0.111(3) 0.150(4) 0.113(3) -0.007(3) 0.057(3) -0.025(3) C1 0.043(6) 0.063(6) 0.057(7) 0.005(5) 0.024(5) -0.011(5) C2 0.066(8) 0.099(9) 0.063(8) 0.019(7) 0.024(6) 0.008(7) C3 0.054(7) 0.056(6) 0.077(9) -0.003(6) 0.020(6) 0.007(5) C4 0.052(6) 0.058(6) 0.061(7) -0.008(5) 0.023(5) 0.007(5) C5 0.033(5) 0.041(5) 0.049(6) -0.003(4) 0.017(4) -0.003(4) C6 0.054(6) 0.041(5) 0.050(6) -0.001(4) 0.023(5) 0.000(4) C7 0.055(6) 0.062(7) 0.062(7) -0.011(5) 0.023(5) 0.004(5) C8 0.069(7) 0.063(7) 0.057(7) -0.004(5) 0.042(6) -0.001(6) C9 0.096(9) 0.038(5) 0.060(7) -0.002(5) 0.038(7) 0.009(6) C10 0.053(6) 0.055(6) 0.046(6) -0.009(5) 0.011(5) 0.011(5) C11 0.053(6) 0.044(5) 0.052(6) 0.001(4) 0.021(5) -0.005(5) C12 0.126(12) 0.098(10) 0.071(9) 0.001(8) 0.053(9) 0.001(9) C13 0.049(6) 0.043(5) 0.049(6) -0.001(4) 0.029(5) 0.004(4) C14 0.035(5) 0.045(5) 0.051(6) -0.004(4) 0.021(4) -0.001(4) C15 0.064(7) 0.049(6) 0.067(7) -0.001(5) 0.034(6) 0.002(5) C16 0.049(6) 0.057(6) 0.074(8) 0.006(6) 0.018(6) 0.014(5) C17 0.027(5) 0.071(7) 0.074(8) -0.009(6) 0.019(5) 0.002(5) C18 0.041(5) 0.052(6) 0.065(7) -0.016(5) 0.025(5) -0.010(5) C19 0.048(6) 0.062(6) 0.055(6) 0.001(5) 0.025(5) -0.005(5) C20 0.057(7) 0.092(9) 0.105(11) 0.018(8) 0.014(7) 0.025(7) C21 0.039(6) 0.082(7) 0.079(8) 0.009(6) 0.020(5) -0.019(6) C22 0.078(7) 0.046(5) 0.060(7) -0.007(5) 0.047(6) -0.003(5) C23 0.050(6) 0.061(6) 0.068(7) -0.029(6) 0.029(5) -0.006(5) C24 0.067(8) 0.085(8) 0.076(8) -0.025(7) 0.051(7) -0.037(7) C25 0.071(8) 0.084(8) 0.031(6) 0.001(5) 0.023(5) -0.033(6) C26 0.046(6) 0.082(8) 0.049(6) -0.016(6) 0.016(5) -0.022(6) C27 0.092(9) 0.067(8) 0.089(10) -0.013(7) 0.047(8) -0.020(7) C28 0.079(9) 0.082(9) 0.099(11) -0.044(8) 0.018(8) 0.010(7) C29 0.119(12) 0.132(13) 0.152(15) -0.071(11) 0.112(12) -0.053(11) C30 0.137(13) 0.128(12) 0.059(8) -0.016(8) 0.050(9) -0.043(11) C31 0.067(8) 0.107(10) 0.074(9) 0.001(8) 0.008(6) -0.021(8) C32 0.055(6) 0.035(5) 0.099(9) -0.002(5) 0.055(6) -0.008(4) C33 0.090(9) 0.098(10) 0.139(13) -0.010(9) 0.083(10) -0.028(8) C34 0.069(8) 0.066(8) 0.132(13) -0.026(8) 0.047(9) -0.023(7) C35 0.067(8) 0.071(8) 0.108(10) -0.024(7) 0.056(7) -0.027(6) C36 0.050(6) 0.042(5) 0.077(8) -0.001(5) 0.036(5) -0.001(5) C37 0.045(6) 0.045(5) 0.070(7) -0.006(5) 0.029(5) -0.007(4) C38 0.050(7) 0.083(8) 0.079(9) -0.018(6) 0.036(6) -0.008(6) C39 0.077(9) 0.067(7) 0.082(9) -0.014(6) 0.032(7) -0.018(7) C40 0.056(7) 0.064(7) 0.076(8) -0.011(6) 0.034(6) -0.015(6) C41 0.060(7) 0.054(7) 0.117(11) -0.012(7) 0.055(8) 0.000(6) C42 0.056(6) 0.049(6) 0.088(9) -0.009(5) 0.046(6) 0.000(5) C43 0.108(11) 0.094(10) 0.105(11) -0.020(8) 0.078(9) -0.012(8) C44 0.047(5) 0.037(5) 0.064(6) -0.005(4) 0.041(5) -0.007(4) C45 0.062(7) 0.043(5) 0.066(7) 0.001(5) 0.040(6) 0.004(5) C46 0.101(10) 0.045(6) 0.082(9) 0.003(5) 0.064(8) -0.003(6) C47 0.088(9) 0.068(8) 0.110(11) -0.009(7) 0.077(9) -0.024(7) C48 0.062(7) 0.057(7) 0.086(9) -0.007(6) 0.042(6) -0.007(6) C49 0.045(6) 0.051(6) 0.080(8) -0.005(5) 0.033(6) -0.001(5) C50 0.071(8) 0.070(8) 0.095(10) 0.011(7) 0.036(7) 0.004(6) C51 0.080(8) 0.054(6) 0.079(8) 0.012(6) 0.039(7) 0.017(6) C52 0.131(12) 0.081(10) 0.169(15) -0.023(10) 0.102(12) -0.052(9) C53 0.086(9) 0.067(7) 0.070(8) -0.003(6) 0.053(7) 0.015(7) C54 0.054(6) 0.075(7) 0.065(7) 0.006(6) 0.037(6) 0.011(6) C55 0.061(8) 0.098(10) 0.082(9) -0.036(8) 0.032(7) 0.002(7) C56 0.132(13) 0.064(8) 0.156(16) -0.054(9) 0.123(13) -0.041(9) C57 0.138(13) 0.037(6) 0.096(10) -0.003(6) 0.078(10) -0.006(7) C58 0.095(10) 0.111(11) 0.068(9) -0.002(8) 0.021(7) 0.036(9) C59 0.106(10) 0.082(9) 0.071(9) 0.020(7) 0.042(8) 0.003(8) C60 0.071(9) 0.130(14) 0.147(16) -0.037(12) 0.036(10) -0.002(9) C61 0.143(8) 0.140(8) 0.147(8) -0.012(5) 0.067(5) -0.008(5) C62 0.137(7) 0.118(7) 0.122(7) -0.005(5) 0.065(5) 0.008(5) C63 0.193(19) 0.119(14) 0.147(17) -0.008(12) 0.100(15) -0.027(14) O2 0.031(8) 0.181(19) 0.078(12) -0.070(12) 0.012(7) 0.007(10) O3 0.072(12) 0.159(18) 0.117(16) 0.064(15) 0.047(11) 0.021(13) O4 0.085(13) 0.129(16) 0.108(16) -0.010(13) 0.029(11) 0.005(12) O5 0.045(9) 0.24(3) 0.096(14) -0.043(15) 0.046(10) -0.044(13) O6 0.092(14) 0.17(2) 0.104(16) -0.063(15) 0.038(12) 0.015(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 C1 1.997(11) . ? Ir1 N6 2.129(7) . ? Ir1 C25 2.153(10) . ? Ir1 C26 2.177(10) . ? Ir1 C22 2.180(10) . ? Ir1 C24 2.224(11) . ? Ir1 C23 2.233(10) . ? Ir1 Cl1 2.414(3) . ? Ir2 C32 2.005(11) . ? Ir2 N1 2.146(8) . ? Ir2 C57 2.154(12) . ? Ir2 C54 2.173(10) . ? Ir2 C53 2.175(11) . ? Ir2 C56 2.212(12) . ? Ir2 C55 2.236(12) . ? Ir2 Cl2 2.412(3) . ? N1 C36 1.281(13) . ? N1 C44 1.452(11) . ? N2 C32 1.332(12) . ? N2 C34 1.366(15) . ? N2 C33 1.445(15) . ? N3 C32 1.362(13) . ? N3 C35 1.369(13) . ? N3 C36 1.416(12) . ? N4 C1 1.328(13) . ? N4 C3 1.421(14) . ? N4 C2 1.479(13) . ? N5 C5 1.386(11) . ? N5 C4 1.387(12) . ? N5 C1 1.388(12) . ? N6 C5 1.276(11) . ? N6 C13 1.466(11) . ? Cl5 C63 1.661(17) . ? Cl6 C63 1.805(17) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 C4 1.298(14) . ? C3 H3 0.9300 . ? C4 H4 0.9300 . ? C5 C6 1.489(13) . ? C6 C11 1.357(13) . ? C6 C7 1.403(14) . ? C7 C8 1.397(14) . ? C7 H7 0.9300 . ? C8 C9 1.373(16) . ? C8 H8 0.9300 . ? C9 C10 1.347(15) . ? C9 C12 1.538(15) . ? C10 C11 1.400(13) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C18 1.393(13) . ? C13 C14 1.434(12) . ? C14 C15 1.401(13) . ? C14 C19 1.469(12) . ? C15 C16 1.427(14) . ? C15 H15 0.9300 . ? C16 C17 1.350(15) . ? C16 C20 1.504(14) . ? C17 C18 1.390(14) . ? C17 H17 0.9300 . ? C18 C21 1.488(14) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C23 1.447(14) . ? C22 C26 1.462(15) . ? C22 C27 1.491(15) . ? C23 C24 1.421(16) . ? C23 C28 1.484(16) . ? C24 C25 1.422(16) . ? C24 C29 1.507(15) . ? C25 C26 1.425(14) . ? C25 C30 1.457(16) . ? C26 C31 1.502(15) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 C35 1.325(17) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 C37 1.495(15) . ? C37 C38 1.352(16) . ? C37 C42 1.374(13) . ? C38 C39 1.387(16) . ? C38 H38 0.9300 . ? C39 C40 1.339(16) . ? C39 H39 0.9300 . ? C40 C41 1.364(16) . ? C40 C43 1.514(16) . ? C41 C42 1.377(15) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 C49 1.384(13) . ? C44 C45 1.408(13) . ? C45 C46 1.383(14) . ? C45 C51 1.514(14) . ? C46 C47 1.425(17) . ? C46 H46 0.9300 . ? C47 C48 1.315(17) . ? C47 C52 1.529(15) . ? C48 C49 1.436(14) . ? C48 H48 0.9300 . ? C49 C50 1.502(15) . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 C57 1.418(17) . ? C53 C54 1.448(15) . ? C53 C58 1.480(17) . ? C54 C55 1.418(16) . ? C54 C59 1.517(15) . ? C55 C56 1.43(2) . ? C55 C60 1.481(19) . ? C56 C57 1.38(2) . ? C56 C61 1.55(2) . ? C57 C62 1.468(19) . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? C60 H60A 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 0.9600 . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? C63 H63A 0.9700 . ? C63 H63B 0.9700 . ? O3 H1O3 0.8500 . ? O3 H2O3 0.8500 . ? O5 H1O5 0.8501 . ? O5 H2O5 0.8499 . ? O6 H1O6 0.8501 . ? O6 H2O6 0.8499 . ? 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 C1 Ir1 N6 75.8(4) . . ? C1 Ir1 C25 115.9(5) . . ? N6 Ir1 C25 166.9(4) . . ? C1 Ir1 C26 101.2(4) . . ? N6 Ir1 C26 137.1(3) . . ? C25 Ir1 C26 38.4(4) . . ? C1 Ir1 C22 119.4(4) . . ? N6 Ir1 C22 104.4(3) . . ? C25 Ir1 C22 65.3(4) . . ? C26 Ir1 C22 39.2(4) . . ? C1 Ir1 C24 152.8(5) . . ? N6 Ir1 C24 131.2(4) . . ? C25 Ir1 C24 37.9(4) . . ? C26 Ir1 C24 62.7(4) . . ? C22 Ir1 C24 63.1(4) . . ? C1 Ir1 C23 157.2(4) . . ? N6 Ir1 C23 102.7(4) . . ? C25 Ir1 C23 64.2(4) . . ? C26 Ir1 C23 64.0(4) . . ? C22 Ir1 C23 38.3(4) . . ? C24 Ir1 C23 37.2(4) . . ? C1 Ir1 Cl1 82.1(3) . . ? N6 Ir1 Cl1 91.1(2) . . ? C25 Ir1 Cl1 96.3(3) . . ? C26 Ir1 Cl1 131.4(3) . . ? C22 Ir1 Cl1 155.8(3) . . ? C24 Ir1 Cl1 92.7(3) . . ? C23 Ir1 Cl1 120.7(3) . . ? C32 Ir2 N1 76.0(4) . . ? C32 Ir2 C57 119.9(6) . . ? N1 Ir2 C57 102.2(4) . . ? C32 Ir2 C54 114.8(4) . . ? N1 Ir2 C54 165.7(4) . . ? C57 Ir2 C54 64.6(4) . . ? C32 Ir2 C53 100.7(4) . . ? N1 Ir2 C53 132.8(4) . . ? C57 Ir2 C53 38.2(5) . . ? C54 Ir2 C53 38.9(4) . . ? C32 Ir2 C56 156.6(6) . . ? N1 Ir2 C56 103.6(4) . . ? C57 Ir2 C56 36.8(5) . . ? C54 Ir2 C56 62.6(4) . . ? C53 Ir2 C56 62.0(5) . . ? C32 Ir2 C55 151.0(5) . . ? N1 Ir2 C55 133.0(4) . . ? C57 Ir2 C55 63.4(5) . . ? C54 Ir2 C55 37.5(4) . . ? C53 Ir2 C55 63.3(5) . . ? C56 Ir2 C55 37.5(5) . . ? C32 Ir2 Cl2 82.1(3) . . ? N1 Ir2 Cl2 90.8(2) . . ? C57 Ir2 Cl2 156.4(5) . . ? C54 Ir2 Cl2 99.8(3) . . ? C53 Ir2 Cl2 136.0(3) . . ? C56 Ir2 Cl2 121.2(6) . . ? C55 Ir2 Cl2 93.3(4) . . ? C36 N1 C44 118.2(9) . . ? C36 N1 Ir2 116.4(7) . . ? C44 N1 Ir2 123.9(6) . . ? C32 N2 C34 110.0(10) . . ? C32 N2 C33 125.9(11) . . ? C34 N2 C33 123.9(11) . . ? C32 N3 C35 111.9(9) . . ? C32 N3 C36 116.8(8) . . ? C35 N3 C36 131.1(10) . . ? C1 N4 C3 110.1(9) . . ? C1 N4 C2 125.7(10) . . ? C3 N4 C2 124.0(9) . . ? C5 N5 C4 130.8(9) . . ? C5 N5 C1 117.3(8) . . ? C4 N5 C1 111.0(8) . . ? C5 N6 C13 119.1(8) . . ? C5 N6 Ir1 117.5(6) . . ? C13 N6 Ir1 122.8(6) . . ? N4 C1 N5 103.9(9) . . ? N4 C1 Ir1 138.4(8) . . ? N5 C1 Ir1 115.7(7) . . ? N4 C2 H2A 109.5 . . ? N4 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N4 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 N4 108.4(10) . . ? C4 C3 H3 125.8 . . ? N4 C3 H3 125.8 . . ? C3 C4 N5 106.4(10) . . ? C3 C4 H4 126.8 . . ? N5 C4 H4 126.8 . . ? N6 C5 N5 113.8(8) . . ? N6 C5 C6 127.2(8) . . ? N5 C5 C6 119.1(8) . . ? C11 C6 C7 120.4(10) . . ? C11 C6 C5 121.3(9) . . ? C7 C6 C5 118.4(9) . . ? C8 C7 C6 119.3(10) . . ? C8 C7 H7 120.4 . . ? C6 C7 H7 120.4 . . ? C9 C8 C7 120.1(10) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C10 C9 C8 119.2(10) . . ? C10 C9 C12 120.3(11) . . ? C8 C9 C12 120.5(11) . . ? C9 C10 C11 122.7(10) . . ? C9 C10 H10 118.7 . . ? C11 C10 H10 118.7 . . ? C6 C11 C10 118.3(10) . . ? C6 C11 H11 120.8 . . ? C10 C11 H11 120.8 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C18 C13 C14 121.5(9) . . ? C18 C13 N6 120.6(8) . . ? C14 C13 N6 117.7(8) . . ? C15 C14 C13 117.0(8) . . ? C15 C14 C19 119.3(9) . . ? C13 C14 C19 123.8(8) . . ? C14 C15 C16 121.4(9) . . ? C14 C15 H15 119.3 . . ? C16 C15 H15 119.3 . . ? C17 C16 C15 118.4(9) . . ? C17 C16 C20 123.5(10) . . ? C15 C16 C20 118.1(10) . . ? C16 C17 C18 123.6(9) . . ? C16 C17 H17 118.2 . . ? C18 C17 H17 118.2 . . ? C17 C18 C13 118.0(9) . . ? C17 C18 C21 120.7(9) . . ? C13 C18 C21 121.2(9) . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C16 C20 H20A 109.5 . . ? C16 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C16 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C26 107.0(9) . . ? C23 C22 C27 128.7(11) . . ? C26 C22 C27 122.6(10) . . ? C23 C22 Ir1 72.8(6) . . ? C26 C22 Ir1 70.3(6) . . ? C27 C22 Ir1 133.5(7) . . ? C24 C23 C22 107.0(10) . . ? C24 C23 C28 128.5(11) . . ? C22 C23 C28 124.3(11) . . ? C24 C23 Ir1 71.1(6) . . ? C22 C23 Ir1 68.9(5) . . ? C28 C23 Ir1 129.2(7) . . ? C23 C24 C25 110.3(9) . . ? C23 C24 C29 123.5(13) . . ? C25 C24 C29 126.2(13) . . ? C23 C24 Ir1 71.7(6) . . ? C25 C24 Ir1 68.4(6) . . ? C29 C24 Ir1 126.4(8) . . ? C24 C25 C26 107.2(9) . . ? C24 C25 C30 125.3(11) . . ? C26 C25 C30 126.0(12) . . ? C24 C25 Ir1 73.7(6) . . ? C26 C25 Ir1 71.7(6) . . ? C30 C25 Ir1 130.9(9) . . ? C25 C26 C22 108.2(9) . . ? C25 C26 C31 129.2(11) . . ? C22 C26 C31 122.5(10) . . ? C25 C26 Ir1 69.9(5) . . ? C22 C26 Ir1 70.5(5) . . ? C31 C26 Ir1 127.8(8) . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C26 C31 H31A 109.5 . . ? C26 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C26 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N2 C32 N3 104.1(9) . . ? N2 C32 Ir2 138.5(9) . . ? N3 C32 Ir2 116.6(6) . . ? N2 C33 H33A 109.5 . . ? N2 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? N2 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C35 C34 N2 109.4(11) . . ? C35 C34 H34 125.3 . . ? N2 C34 H34 125.3 . . ? C34 C35 N3 104.6(11) . . ? C34 C35 H35 127.7 . . ? N3 C35 H35 127.7 . . ? N1 C36 N3 114.2(10) . . ? N1 C36 C37 128.7(9) . . ? N3 C36 C37 117.1(9) . . ? C38 C37 C42 119.0(11) . . ? C38 C37 C36 120.1(10) . . ? C42 C37 C36 120.9(10) . . ? C37 C38 C39 118.4(11) . . ? C37 C38 H38 120.8 . . ? C39 C38 H38 120.8 . . ? C40 C39 C38 124.9(12) . . ? C40 C39 H39 117.5 . . ? C38 C39 H39 117.5 . . ? C39 C40 C41 114.9(11) . . ? C39 C40 C43 121.2(12) . . ? C41 C40 C43 123.8(11) . . ? C40 C41 C42 123.0(11) . . ? C40 C41 H41 118.5 . . ? C42 C41 H41 118.5 . . ? C37 C42 C41 119.6(11) . . ? C37 C42 H42 120.2 . . ? C41 C42 H42 120.2 . . ? C40 C43 H43A 109.5 . . ? C40 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C49 C44 C45 122.0(8) . . ? C49 C44 N1 119.2(9) . . ? C45 C44 N1 118.7(8) . . ? C46 C45 C44 117.4(10) . . ? C46 C45 C51 117.6(10) . . ? C44 C45 C51 124.9(9) . . ? C45 C46 C47 121.5(11) . . ? C45 C46 H46 119.2 . . ? C47 C46 H46 119.2 . . ? C48 C47 C46 119.4(10) . . ? C48 C47 C52 120.8(13) . . ? C46 C47 C52 119.8(13) . . ? C47 C48 C49 122.1(11) . . ? C47 C48 H48 119.0 . . ? C49 C48 H48 119.0 . . ? C44 C49 C48 117.5(10) . . ? C44 C49 C50 123.0(9) . . ? C48 C49 C50 119.4(10) . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C45 C51 H51A 109.5 . . ? C45 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C45 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C47 C52 H52A 109.5 . . ? C47 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C47 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C57 C53 C54 107.6(12) . . ? C57 C53 C58 125.9(13) . . ? C54 C53 C58 126.4(11) . . ? C57 C53 Ir2 70.1(7) . . ? C54 C53 Ir2 70.5(6) . . ? C58 C53 Ir2 127.4(9) . . ? C55 C54 C53 107.7(11) . . ? C55 C54 C59 124.8(12) . . ? C53 C54 C59 125.9(10) . . ? C55 C54 Ir2 73.7(6) . . ? C53 C54 Ir2 70.6(6) . . ? C59 C54 Ir2 132.4(9) . . ? C54 C55 C56 106.3(12) . . ? C54 C55 C60 124.4(14) . . ? C56 C55 C60 129.2(15) . . ? C54 C55 Ir2 68.8(7) . . ? C56 C55 Ir2 70.3(7) . . ? C60 C55 Ir2 127.1(10) . . ? C57 C56 C55 110.5(11) . . ? C57 C56 C61 124.7(16) . . ? C55 C56 C61 124.6(17) . . ? C57 C56 Ir2 69.3(7) . . ? C55 C56 Ir2 72.2(7) . . ? C61 C56 Ir2 129.3(10) . . ? C56 C57 C53 107.7(12) . . ? C56 C57 C62 123.9(15) . . ? C53 C57 C62 126.8(16) . . ? C56 C57 Ir2 73.9(8) . . ? C53 C57 Ir2 71.7(6) . . ? C62 C57 Ir2 131.3(10) . . ? C53 C58 H58A 109.5 . . ? C53 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C53 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C54 C59 H59A 109.5 . . ? C54 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C54 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C55 C60 H60A 109.5 . . ? C55 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C55 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C56 C61 H61A 109.5 . . ? C56 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C56 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C57 C62 H62A 109.5 . . ? C57 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C57 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? Cl5 C63 Cl6 112.3(10) . . ? Cl5 C63 H63A 109.1 . . ? Cl6 C63 H63A 109.1 . . ? Cl5 C63 H63B 109.1 . . ? Cl6 C63 H63B 109.1 . . ? H63A C63 H63B 107.9 . . ? H1O3 O3 H2O3 107.7 . . ? H1O5 O5 H2O5 107.7 . . ? H1O6 O6 H2O6 107.7 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.396 _refine_diff_density_min -1.537 _refine_diff_density_rms 0.206 #===END #compound 6cntf2 data_11129c _database_code_depnum_ccdc_archive 'CCDC 872880' #TrackingRef 'Crystallographic Information__ File.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H31 Cl F6 N4 O4 Ru S2' _chemical_formula_weight 826.23 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' S S 0.1246 0.1234 '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' N N 0.0061 0.0033 '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' _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 8.8397(12) _cell_length_b 11.0339(15) _cell_length_c 17.918(2) _cell_angle_alpha 91.615(2) _cell_angle_beta 102.572(2) _cell_angle_gamma 96.477(2) _cell_volume 1692.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9169 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 27.42 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.621 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 836 _exptl_absorpt_coefficient_mu 0.740 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8971 _exptl_absorpt_correction_T_max 0.9297 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 10193 _diffrn_reflns_av_R_equivalents 0.0183 _diffrn_reflns_av_sigmaI/netI 0.0322 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 25.50 _reflns_number_total 6170 _reflns_number_gt 5508 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0547P)^2^+7.8981P] 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 6170 _refine_ls_number_parameters 539 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0611 _refine_ls_R_factor_gt 0.0531 _refine_ls_wR_factor_ref 0.1441 _refine_ls_wR_factor_gt 0.1330 _refine_ls_goodness_of_fit_ref 1.133 _refine_ls_restrained_S_all 1.161 _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 Ru1 Ru 0.69577(4) 0.72338(3) 0.71353(2) 0.02252(14) Uani 1 1 d . . . Cl1 Cl 0.79849(13) 0.55186(10) 0.66599(6) 0.0268(2) Uani 1 1 d . . . N1 N 0.4612(5) 0.6637(4) 0.5536(2) 0.0269(8) Uani 1 1 d . . . N2 N 0.4049(4) 0.5740(3) 0.6513(2) 0.0215(7) Uani 1 1 d . . . N3 N 0.5676(4) 0.5962(3) 0.7664(2) 0.0203(7) Uani 1 1 d . . . C1 C 0.5398(7) 0.7409(5) 0.5054(3) 0.0361(12) Uani 1 1 d . . . H1A H 0.4976 0.8194 0.5011 0.054 Uiso 1 1 calc R . . H1B H 0.5227 0.7004 0.4543 0.054 Uiso 1 1 calc R . . H1C H 0.6520 0.7546 0.5282 0.054 Uiso 1 1 calc R . . C2 C 0.5084(5) 0.6617(4) 0.6299(3) 0.0226(9) Uani 1 1 d . . . C3 C 0.3329(6) 0.5784(4) 0.5274(3) 0.0288(10) Uani 1 1 d . . . H3 H 0.2797 0.5628 0.4753 0.035 Uiso 1 1 calc R . . C4 C 0.2952(6) 0.5214(4) 0.5863(3) 0.0262(9) Uani 1 1 d . . . H4 H 0.2118 0.4585 0.5848 0.031 Uiso 1 1 calc R . . C5 C 0.4403(5) 0.5384(4) 0.7265(2) 0.0205(9) Uani 1 1 d . . . C6 C 0.6260(5) 0.5740(4) 0.8457(3) 0.0228(9) Uani 1 1 d . . . C7 C 0.7479(6) 0.5050(5) 0.8649(3) 0.0312(11) Uani 1 1 d . . . H7 H 0.7902 0.4702 0.8261 0.037 Uiso 1 1 calc R . . C8 C 0.8080(6) 0.4867(5) 0.9411(3) 0.0373(12) Uani 1 1 d . . . H8 H 0.8903 0.4376 0.9548 0.045 Uiso 1 1 calc R . . C9 C 0.7475(7) 0.5404(5) 0.9974(3) 0.0411(13) Uani 1 1 d . . . H9 H 0.7893 0.5286 1.0498 0.049 Uiso 1 1 calc R . . C10 C 0.6273(7) 0.6106(5) 0.9776(3) 0.0373(12) Uani 1 1 d . . . H10 H 0.5873 0.6476 1.0166 0.045 Uiso 1 1 calc R . . C11 C 0.5641(6) 0.6278(5) 0.9015(3) 0.0286(10) Uani 1 1 d . . . H11 H 0.4802 0.6753 0.8877 0.034 Uiso 1 1 calc R . . C12 C 0.3326(5) 0.4445(4) 0.7515(2) 0.0189(8) Uani 1 1 d . . . C13 C 0.3878(5) 0.3460(4) 0.7922(2) 0.0205(9) Uani 1 1 d . . . H13 H 0.4962 0.3379 0.8034 0.025 Uiso 1 1 calc R . . C14 C 0.2842(6) 0.2608(4) 0.8159(3) 0.0264(10) Uani 1 1 d . . . H14 H 0.3222 0.1932 0.8425 0.032 Uiso 1 1 calc R . . C15 C 0.1247(6) 0.2715(4) 0.8017(3) 0.0285(10) Uani 1 1 d . . . C16 C 0.0721(5) 0.3695(4) 0.7619(3) 0.0258(9) Uani 1 1 d . . . H16 H -0.0359 0.3786 0.7522 0.031 Uiso 1 1 calc R . . C17 C 0.1728(5) 0.4548(4) 0.7356(3) 0.0220(9) Uani 1 1 d . . . H17 H 0.1334 0.5200 0.7070 0.026 Uiso 1 1 calc R . . C18 C 0.0127(7) 0.1794(6) 0.8290(4) 0.0490(15) Uani 1 1 d . . . H18A H -0.0943 0.1983 0.8103 0.074 Uiso 1 1 calc R . . H18B H 0.0373 0.1826 0.8851 0.074 Uiso 1 1 calc R . . H18C H 0.0221 0.0975 0.8094 0.074 Uiso 1 1 calc R . . C19 C 1.0801(6) 0.7488(5) 0.8056(4) 0.0515(17) Uani 1 1 d . . . H19A H 1.1706 0.8110 0.8220 0.077 Uiso 1 1 calc R . . H19B H 1.0978 0.6946 0.7649 0.077 Uiso 1 1 calc R . . H19C H 1.0651 0.7009 0.8493 0.077 Uiso 1 1 calc R . . C20 C 0.9354(3) 0.8105(3) 0.77576(19) 0.0358(12) Uani 1 1 d G . . C21 C 0.8285(3) 0.8247(3) 0.82297(18) 0.0298(10) Uani 1 1 d G . . H21 H 0.8399 0.7823 0.8721 0.036 Uiso 1 1 calc R . . C22 C 0.6896(3) 0.8769(3) 0.79405(17) 0.0255(9) Uani 1 1 d G . . H22 H 0.6058 0.8727 0.8238 0.031 Uiso 1 1 calc R . . C23 C 0.6576(4) 0.9148(3) 0.71792(17) 0.0261(10) Uani 1 1 d G . . C24 C 0.7645(4) 0.9006(3) 0.67072(18) 0.0315(11) Uani 1 1 d G . . H24 H 0.7333 0.9138 0.6147 0.038 Uiso 1 1 calc R . . C25 C 0.9034(4) 0.8485(3) 0.6996(2) 0.0355(12) Uani 1 1 d GU . . H25 H 0.9673 0.8233 0.6635 0.043 Uiso 1 1 calc R . . C26 C 0.5097(6) 0.9744(4) 0.6845(3) 0.0290(10) Uani 1 1 d . . . H26 H 0.4765 0.9494 0.6287 0.035 Uiso 1 1 calc R . . C27 C 0.3740(7) 0.9347(6) 0.7215(4) 0.0466(15) Uani 1 1 d . . . H27A H 0.3542 0.8453 0.7188 0.070 Uiso 1 1 calc R . . H27B H 0.2805 0.9681 0.6944 0.070 Uiso 1 1 calc R . . H27C H 0.4000 0.9651 0.7753 0.070 Uiso 1 1 calc R . . C28 C 0.5522(7) 1.1135(5) 0.6921(3) 0.0420(13) Uani 1 1 d . . . H28A H 0.5841 1.1405 0.7464 0.063 Uiso 1 1 calc R . . H28B H 0.4612 1.1528 0.6678 0.063 Uiso 1 1 calc R . . H28C H 0.6384 1.1363 0.6669 0.063 Uiso 1 1 calc R . . C29 C 0.0149(5) 0.8138(4) 0.4152(3) 0.0386(13) Uani 1 1 d D . . S1 S 0.10000(18) 0.90947(12) 0.50483(9) 0.0420(4) Uani 1 1 d . . . N4 N -0.0303(9) 0.9592(7) 0.5312(4) 0.0231(16) Uani 0.50 1 d P . . O1 O 0.1593(9) 0.8149(6) 0.5681(4) 0.0333(16) Uani 0.50 1 d P A 1 O2 O 0.2495(10) 0.9199(9) 0.5004(5) 0.0370(19) Uani 0.50 1 d P B 1 F1 F 0.0403(8) 0.7017(5) 0.4226(4) 0.0392(14) Uani 0.50 1 d P C 1 F2 F -0.1444(6) 0.8026(6) 0.3952(4) 0.0399(14) Uani 0.50 1 d PD C 1 F3 F 0.0489(9) 0.8532(6) 0.3516(3) 0.0389(15) Uani 0.50 1 d PD C 1 O1' O 0.0175(10) 0.8600(7) 0.5547(4) 0.0390(18) Uani 0.50 1 d P C 2 O2' O 0.2383(9) 0.9888(8) 0.4978(4) 0.0299(17) Uani 0.50 1 d P D 2 F1' F 0.1358(7) 0.7587(7) 0.4034(4) 0.0455(16) Uani 0.50 1 d PD C 2 F2' F -0.0854(9) 0.7315(6) 0.4314(4) 0.0492(18) Uani 0.50 1 d PD C 2 F3' F -0.0205(8) 0.8921(6) 0.3661(4) 0.0379(15) Uani 0.50 1 d PD C 2 N5 N 0.4999(11) -0.0298(10) 0.9552(5) 0.037(2) Uani 0.50 1 d P . . S2 S 0.6622(3) 0.0041(3) 1.01737(18) 0.0395(6) Uani 0.50 1 d P . 1 C30 C 0.776(2) 0.0203(19) 0.9990(12) 0.081(5) Uiso 0.50 1 d P E 1 O3 O 0.721(3) 0.0144(9) 1.0940(6) 0.137(9) Uani 0.50 1 d P E 1 O4 O 0.706(3) -0.0961(11) 0.9810(8) 0.125(8) Uani 0.50 1 d P E 1 F4 F 0.8328(9) 0.0225(7) 1.0670(4) 0.0511(19) Uani 0.50 1 d P E 1 F5 F 0.8456(13) 0.060(3) 0.9527(11) 0.230(16) Uani 0.50 1 d P E 1 F6 F 0.791(3) -0.066(3) 0.9742(14) 0.35(2) Uani 0.50 1 d P E 1 S2' S 0.5975(5) 0.0899(5) 0.9728(2) 0.093(2) Uani 0.50 1 d P . 2 C30' C 0.7251(13) 0.1483(10) 0.9804(5) 0.033(2) Uani 0.50 1 d P F 2 O3' O 0.5058(18) 0.0283(17) 0.9088(9) 0.112(5) Uani 0.50 1 d P . 2 O4' O 0.6129(10) 0.1976(9) 1.0103(8) 0.056(3) Uani 0.50 1 d P F 2 F4' F 0.6525(13) 0.1538(7) 0.9020(4) 0.079(3) Uani 0.50 1 d P F 2 F5' F 0.690(2) 0.2413(10) 1.0141(10) 0.134(8) Uani 0.50 1 d P F 2 F6' F 0.8935(9) 0.1690(7) 1.0013(5) 0.055(2) Uani 0.50 1 d P F 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0195(2) 0.0188(2) 0.0300(2) 0.00250(14) 0.00820(15) -0.00025(13) Cl1 0.0257(5) 0.0248(5) 0.0293(6) -0.0008(4) 0.0039(4) 0.0057(4) N1 0.034(2) 0.0220(19) 0.028(2) 0.0080(16) 0.0112(17) 0.0093(16) N2 0.0207(18) 0.0199(18) 0.0228(18) 0.0021(14) 0.0024(15) 0.0018(14) N3 0.0190(18) 0.0192(18) 0.0216(18) 0.0017(14) 0.0023(14) 0.0014(14) C1 0.047(3) 0.037(3) 0.031(3) 0.012(2) 0.017(2) 0.010(2) C2 0.023(2) 0.021(2) 0.025(2) 0.0070(17) 0.0053(18) 0.0087(17) C3 0.032(3) 0.029(2) 0.024(2) 0.0016(19) 0.0005(19) 0.010(2) C4 0.027(2) 0.024(2) 0.025(2) 0.0011(18) 0.0004(18) 0.0020(18) C5 0.021(2) 0.016(2) 0.025(2) 0.0008(16) 0.0049(17) 0.0045(16) C6 0.018(2) 0.024(2) 0.022(2) 0.0014(17) 0.0013(17) -0.0062(17) C7 0.025(2) 0.036(3) 0.030(2) -0.001(2) 0.003(2) -0.001(2) C8 0.029(3) 0.045(3) 0.033(3) 0.004(2) -0.005(2) 0.003(2) C9 0.037(3) 0.047(3) 0.032(3) 0.006(2) -0.003(2) -0.007(2) C10 0.041(3) 0.044(3) 0.026(3) -0.002(2) 0.011(2) -0.004(2) C11 0.022(2) 0.032(3) 0.030(2) 0.004(2) 0.0068(19) -0.0023(19) C12 0.018(2) 0.018(2) 0.020(2) -0.0004(16) 0.0039(16) 0.0019(16) C13 0.019(2) 0.019(2) 0.022(2) -0.0010(16) 0.0015(17) 0.0011(16) C14 0.030(2) 0.020(2) 0.028(2) 0.0066(18) 0.0042(19) 0.0030(18) C15 0.024(2) 0.030(2) 0.030(2) 0.0028(19) 0.0066(19) -0.0041(19) C16 0.018(2) 0.028(2) 0.030(2) -0.0004(19) 0.0041(18) -0.0006(18) C17 0.022(2) 0.017(2) 0.027(2) -0.0010(17) 0.0038(18) 0.0038(16) C18 0.035(3) 0.049(4) 0.062(4) 0.025(3) 0.012(3) -0.009(3) C19 0.022(3) 0.033(3) 0.093(5) -0.013(3) 0.002(3) 0.003(2) C20 0.019(2) 0.021(2) 0.065(4) -0.007(2) 0.007(2) -0.0022(18) C21 0.027(2) 0.020(2) 0.039(3) -0.0044(19) 0.002(2) -0.0019(18) C22 0.020(2) 0.021(2) 0.035(2) 0.0010(18) 0.0059(19) -0.0021(17) C23 0.026(2) 0.020(2) 0.034(2) 0.0028(18) 0.013(2) -0.0009(18) C24 0.041(3) 0.018(2) 0.041(3) 0.0031(19) 0.024(2) -0.003(2) C25 0.027(2) 0.024(2) 0.058(3) -0.003(2) 0.022(2) -0.0067(19) C26 0.031(3) 0.029(2) 0.029(2) 0.0038(19) 0.008(2) 0.009(2) C27 0.028(3) 0.069(4) 0.050(3) 0.022(3) 0.016(3) 0.019(3) C28 0.052(3) 0.029(3) 0.046(3) 0.004(2) 0.007(3) 0.018(2) C29 0.050(3) 0.024(3) 0.047(3) -0.001(2) 0.027(3) -0.002(2) S1 0.0521(9) 0.0248(6) 0.0557(9) -0.0096(6) 0.0354(7) -0.0097(6) N4 0.027(4) 0.022(4) 0.022(4) 0.004(3) 0.011(3) -0.002(3) O1 0.050(4) 0.025(3) 0.029(4) 0.007(3) 0.014(3) 0.010(3) O2 0.030(4) 0.039(5) 0.035(4) -0.007(4) -0.006(3) 0.004(4) F1 0.046(4) 0.020(3) 0.051(4) 0.001(3) 0.007(3) 0.005(3) F2 0.034(3) 0.032(3) 0.049(4) -0.009(3) 0.007(3) -0.006(3) F3 0.058(5) 0.024(3) 0.030(3) -0.004(3) 0.007(3) -0.011(3) O1' 0.059(5) 0.034(4) 0.027(4) 0.012(3) 0.014(3) 0.003(4) O2' 0.027(4) 0.033(4) 0.028(4) 0.002(4) 0.007(3) -0.005(4) F1' 0.054(4) 0.054(4) 0.030(3) -0.011(3) 0.007(3) 0.018(4) F2' 0.061(5) 0.031(4) 0.055(4) -0.008(3) 0.026(4) -0.020(3) F3' 0.042(4) 0.036(4) 0.031(3) -0.001(3) -0.002(3) 0.003(3) N5 0.045(5) 0.063(6) 0.009(4) 0.008(4) 0.008(4) 0.019(5) S2 0.0285(13) 0.0331(14) 0.0558(17) 0.0221(12) 0.0057(12) 0.0016(10) O3 0.36(3) 0.033(5) 0.025(5) 0.004(4) 0.069(10) -0.001(9) O4 0.27(2) 0.053(7) 0.061(8) -0.029(6) 0.107(12) -0.065(11) F4 0.057(5) 0.059(5) 0.030(4) -0.002(3) -0.017(3) 0.029(4) F5 0.032(6) 0.54(5) 0.146(15) 0.21(2) 0.048(8) 0.056(14) F6 0.25(2) 0.50(4) 0.23(2) -0.30(3) -0.213(19) 0.34(3) S2' 0.070(3) 0.113(4) 0.078(3) -0.068(3) -0.047(2) 0.073(3) C30' 0.036(6) 0.042(6) 0.018(4) 0.012(4) -0.001(4) 0.009(5) O3' 0.081(10) 0.153(15) 0.093(11) -0.024(10) -0.004(8) 0.031(10) O4' 0.028(4) 0.028(5) 0.097(9) -0.010(5) -0.016(5) 0.008(4) F4' 0.152(9) 0.046(4) 0.028(4) 0.028(3) 0.014(4) -0.033(5) F5' 0.27(2) 0.035(6) 0.170(14) 0.049(7) 0.171(15) 0.058(9) F6' 0.042(4) 0.045(4) 0.068(5) 0.020(4) 0.005(4) -0.023(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C2 2.015(5) . ? Ru1 N3 2.081(4) . ? Ru1 C23 2.178(3) . ? Ru1 C24 2.191(3) . ? Ru1 C22 2.207(3) . ? Ru1 C25 2.232(3) . ? Ru1 C21 2.247(3) . ? Ru1 C20 2.260(3) . ? Ru1 Cl1 2.4011(11) . ? N1 C2 1.341(6) . ? N1 C3 1.377(7) . ? N1 C1 1.457(6) . ? N2 C2 1.377(6) . ? N2 C5 1.394(6) . ? N2 C4 1.407(6) . ? N3 C5 1.283(6) . ? N3 C6 1.441(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C3 C4 1.328(7) . ? C3 H3 0.9500 . ? C4 H4 0.9500 . ? C5 C12 1.473(6) . ? C6 C7 1.378(7) . ? C6 C11 1.388(7) . ? C7 C8 1.382(7) . ? C7 H7 0.9500 . ? C8 C9 1.389(8) . ? C8 H8 0.9500 . ? C9 C10 1.376(8) . ? C9 H9 0.9500 . ? C10 C11 1.385(7) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C17 1.397(6) . ? C12 C13 1.400(6) . ? C13 C14 1.379(6) . ? C13 H13 0.9500 . ? C14 C15 1.396(7) . ? C14 H14 0.9500 . ? C15 C16 1.381(7) . ? C15 C18 1.505(7) . ? C16 C17 1.385(6) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.518(6) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C25 1.417(2) . ? C20 C21 1.417(2) . ? C21 C22 1.417(2) . ? C21 H21 1.0000 . ? C22 C23 1.417(2) . ? C22 H22 1.0000 . ? C23 C24 1.417(2) . ? C23 C26 1.540(6) . ? C24 C25 1.417(2) . ? C24 H24 1.0000 . ? C25 H25 1.0000 . ? C26 C27 1.521(7) . ? C26 C28 1.534(7) . ? C26 H26 1.0000 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 F1 1.286(7) . ? C29 F3 1.314(5) . ? C29 F2 1.365(4) . ? C29 S1 1.860(5) . ? S1 O2 1.334(9) . ? S1 N4 1.489(8) . ? S1 O1 1.606(7) . ? S1 N4 1.725(8) 2_576 ? N4 N4 1.600(13) 2_576 ? N4 S1 1.725(8) 2_576 ? N5 S2 1.612(10) . ? N5 S2 1.663(9) 2_657 ? N5 N5 1.717(16) 2_657 ? S2 C30 1.13(2) . ? S2 O3 1.355(12) . ? S2 O4 1.401(15) . ? S2 F4 1.563(7) . ? S2 N5 1.663(10) 2_657 ? S2 F6 1.747(19) . ? C30 F6 1.07(3) . ? C30 F5 1.20(2) . ? C30 F4 1.21(2) . ? C30 O4 1.36(2) . ? C30 O3 1.87(2) . ? O3 F4 1.19(2) . ? O4 F6 0.82(4) . ? F5 F6 1.51(4) . ? S2' C30' 1.212(12) . ? S2' O4' 1.327(11) . ? S2' O3' 1.364(15) . ? S2' F4' 1.607(9) . ? S2' F5' 1.835(17) . ? C30' F5' 1.279(16) . ? C30' O4' 1.380(16) . ? C30' F4' 1.418(12) . ? C30' F6' 1.443(13) . ? O4' F5' 0.778(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Ru1 N3 76.29(16) . . ? C2 Ru1 C23 98.10(15) . . ? N3 Ru1 C23 119.82(13) . . ? C2 Ru1 C24 100.25(15) . . ? N3 Ru1 C24 157.36(13) . . ? C23 Ru1 C24 37.84(6) . . ? C2 Ru1 C22 121.31(15) . . ? N3 Ru1 C22 94.51(13) . . ? C23 Ru1 C22 37.69(6) . . ? C24 Ru1 C22 67.83(9) . . ? C2 Ru1 C25 126.01(16) . . ? N3 Ru1 C25 156.83(14) . . ? C23 Ru1 C25 67.60(10) . . ? C24 Ru1 C25 37.35(6) . . ? C22 Ru1 C25 79.33(11) . . ? C2 Ru1 C21 157.05(15) . . ? N3 Ru1 C21 95.19(13) . . ? C23 Ru1 C21 67.33(9) . . ? C24 Ru1 C21 79.33(11) . . ? C22 Ru1 C21 37.08(5) . . ? C25 Ru1 C21 66.43(9) . . ? C2 Ru1 C20 162.24(16) . . ? N3 Ru1 C20 120.37(13) . . ? C23 Ru1 C20 79.33(11) . . ? C24 Ru1 C20 66.89(10) . . ? C22 Ru1 C20 66.64(9) . . ? C25 Ru1 C20 36.76(6) . . ? C21 Ru1 C20 36.64(5) . . ? C2 Ru1 Cl1 82.04(13) . . ? N3 Ru1 Cl1 86.08(10) . . ? C23 Ru1 Cl1 153.55(8) . . ? C24 Ru1 Cl1 115.88(8) . . ? C22 Ru1 Cl1 156.15(8) . . ? C25 Ru1 Cl1 90.78(9) . . ? C21 Ru1 Cl1 119.08(8) . . ? C20 Ru1 Cl1 92.50(8) . . ? C2 N1 C3 110.2(4) . . ? C2 N1 C1 124.6(4) . . ? C3 N1 C1 125.1(4) . . ? C2 N2 C5 117.6(4) . . ? C2 N2 C4 109.8(4) . . ? C5 N2 C4 131.4(4) . . ? C5 N3 C6 122.1(4) . . ? C5 N3 Ru1 118.7(3) . . ? C6 N3 Ru1 119.2(3) . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 N2 105.2(4) . . ? N1 C2 Ru1 139.1(3) . . ? N2 C2 Ru1 114.5(3) . . ? C4 C3 N1 109.3(4) . . ? C4 C3 H3 125.3 . . ? N1 C3 H3 125.3 . . ? C3 C4 N2 105.5(4) . . ? C3 C4 H4 127.3 . . ? N2 C4 H4 127.3 . . ? N3 C5 N2 112.9(4) . . ? N3 C5 C12 128.0(4) . . ? N2 C5 C12 119.2(4) . . ? C7 C6 C11 121.3(4) . . ? C7 C6 N3 119.1(4) . . ? C11 C6 N3 119.4(4) . . ? C6 C7 C8 119.5(5) . . ? C6 C7 H7 120.3 . . ? C8 C7 H7 120.3 . . ? C7 C8 C9 119.7(5) . . ? C7 C8 H8 120.1 . . ? C9 C8 H8 120.1 . . ? C10 C9 C8 120.3(5) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C11 120.6(5) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C10 C11 C6 118.6(5) . . ? C10 C11 H11 120.7 . . ? C6 C11 H11 120.7 . . ? C17 C12 C13 119.3(4) . . ? C17 C12 C5 119.6(4) . . ? C13 C12 C5 121.1(4) . . ? C14 C13 C12 119.7(4) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C13 C14 C15 121.5(4) . . ? C13 C14 H14 119.3 . . ? C15 C14 H14 119.3 . . ? C16 C15 C14 118.1(4) . . ? C16 C15 C18 120.6(5) . . ? C14 C15 C18 121.2(5) . . ? C15 C16 C17 121.6(4) . . ? C15 C16 H16 119.2 . . ? C17 C16 H16 119.2 . . ? C16 C17 C12 119.7(4) . . ? C16 C17 H17 120.1 . . ? C12 C17 H17 120.1 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 H19A 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C20 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C25 C20 C21 120.0 . . ? C25 C20 C19 120.1(4) . . ? C21 C20 C19 119.8(4) . . ? C25 C20 Ru1 70.55(10) . . ? C21 C20 Ru1 71.20(9) . . ? C19 C20 Ru1 128.3(3) . . ? C22 C21 C20 120.0 . . ? C22 C21 Ru1 69.90(9) . . ? C20 C21 Ru1 72.16(10) . . ? C22 C21 H21 119.4 . . ? C20 C21 H21 119.4 . . ? Ru1 C21 H21 119.4 . . ? C21 C22 C23 120.0 . . ? C21 C22 Ru1 73.03(10) . . ? C23 C22 Ru1 70.06(10) . . ? C21 C22 H22 119.5 . . ? C23 C22 H22 119.5 . . ? Ru1 C22 H22 119.5 . . ? C24 C23 C22 120.0 . . ? C24 C23 C26 118.1(2) . . ? C22 C23 C26 121.9(3) . . ? C24 C23 Ru1 71.57(10) . . ? C22 C23 Ru1 72.24(10) . . ? C26 C23 Ru1 129.4(3) . . ? C25 C24 C23 120.0 . . ? C25 C24 Ru1 72.90(10) . . ? C23 C24 Ru1 70.59(10) . . ? C25 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? Ru1 C24 H24 119.6 . . ? C20 C25 C24 120.0 . . ? C20 C25 Ru1 72.69(10) . . ? C24 C25 Ru1 69.76(10) . . ? C20 C25 H25 119.4 . . ? C24 C25 H25 119.4 . . ? Ru1 C25 H25 119.4 . . ? C27 C26 C28 111.4(5) . . ? C27 C26 C23 113.1(4) . . ? C28 C26 C23 108.4(4) . . ? C27 C26 H26 107.9 . . ? C28 C26 H26 107.9 . . ? C23 C26 H26 107.9 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? F3' C29 F2' 123.2(6) . . ? F1 C29 F3 110.2(6) . . ? F3' C29 F1' 111.4(6) . . ? F2' C29 F1' 107.6(6) . . ? F1 C29 F2 101.8(5) . . ? F3 C29 F2 100.2(6) . . ? F1 C29 S1 111.9(4) . . ? F3 C29 S1 117.3(4) . . ? F2 C29 S1 113.7(4) . . ? O1' S1 O2' 144.9(5) . . ? O2 S1 N4 150.0(5) . . ? O2 S1 O1 81.7(5) . . ? N4 S1 O1 104.1(4) . . ? O2 S1 N4 105.7(5) . 2_576 ? N4 S1 N4 59.1(4) . 2_576 ? O1 S1 N4 157.8(4) . 2_576 ? O2 S1 C29 98.6(4) . . ? N4 S1 C29 107.9(3) . . ? O1 S1 C29 105.2(3) . . ? N4 S1 C29 94.5(3) 2_576 . ? S1 N4 N4 67.8(5) . 2_576 ? S1 N4 S1 120.9(4) . 2_576 ? N4 N4 S1 53.0(4) 2_576 2_576 ? O3' N5 S2' 62.2(11) . . ? S2 N5 S2 116.8(5) . 2_657 ? S2 N5 N5 59.9(6) . 2_657 ? S2 N5 N5 56.9(5) 2_657 2_657 ? O3' N5 S2' 150.8(12) . 2_657 ? S2' N5 S2' 117.9(6) . 2_657 ? C30 S2 O3 97.6(14) . . ? C30 S2 O4 64.0(12) . . ? O3 S2 O4 113.4(11) . . ? C30 S2 F4 50.4(11) . . ? O3 S2 F4 47.3(10) . . ? O4 S2 F4 86.5(10) . . ? C30 S2 N5 121.0(11) . . ? O3 S2 N5 141.3(11) . . ? O4 S2 N5 83.2(10) . . ? F4 S2 N5 169.1(5) . . ? C30 S2 N5 161.2(12) . 2_657 ? O3 S2 N5 81.7(11) . 2_657 ? O4 S2 N5 133.6(8) . 2_657 ? F4 S2 N5 127.3(5) . 2_657 ? N5 S2 N5 63.2(5) . 2_657 ? C30 S2 F6 36.4(17) . . ? O3 S2 F6 108.4(11) . . ? O4 S2 F6 27.6(13) . . ? F4 S2 F6 67.7(6) . . ? N5 S2 F6 101.5(6) . . ? N5 S2 F6 160.8(12) 2_657 . ? F6 C30 S2 105(3) . . ? F6 C30 F5 83(3) . . ? S2 C30 F5 148(2) . . ? F6 C30 F4 108(2) . . ? S2 C30 F4 83.9(14) . . ? F5 C30 F4 124(2) . . ? F6 C30 O4 37(2) . . ? S2 C30 O4 67.9(14) . . ? F5 C30 O4 114(2) . . ? F4 C30 O4 104.6(16) . . ? F6 C30 O3 115(3) . . ? S2 C30 O3 45.8(10) . . ? F5 C30 O3 156(2) . . ? F4 C30 O3 38.2(10) . . ? O4 C30 O3 89.5(12) . . ? F4 O3 S2 75.6(6) . . ? F4 O3 C30 39.1(7) . . ? S2 O3 C30 36.6(7) . . ? F6 O4 C30 52.2(17) . . ? F6 O4 S2 100.3(18) . . ? C30 O4 S2 48.1(10) . . ? O3 F4 C30 102.7(14) . . ? O3 F4 S2 57.1(8) . . ? C30 F4 S2 45.7(10) . . ? C30 F5 F6 45.0(13) . . ? O4 F6 C30 91(2) . . ? O4 F6 F5 131(2) . . ? C30 F6 F5 52(2) . . ? O4 F6 S2 52.1(13) . . ? C30 F6 S2 38.4(15) . . ? F5 F6 S2 86.3(11) . . ? C30' S2' O4' 65.7(7) . . ? C30' S2' O3' 128.7(10) . . ? O4' S2' O3' 139.0(9) . . ? C30' S2' F4' 58.4(6) . . ? O4' S2' F4' 90.8(8) . . ? O3' S2' F4' 74.7(9) . . ? C30' S2' F5' 44.0(7) . . ? O4' S2' F5' 21.8(7) . . ? O3' S2' F5' 144.2(11) . . ? F4' S2' F5' 76.9(6) . . ? S2' C30' F5' 94.9(12) . . ? S2' C30' O4' 61.2(7) . . ? F5' C30' O4' 33.8(8) . . ? S2' C30' F4' 74.9(7) . . ? F5' C30' F4' 105.4(12) . . ? O4' C30' F4' 97.2(9) . . ? S2' C30' F6' 155.8(9) . . ? F5' C30' F6' 100.9(13) . . ? O4' C30' F6' 131.4(10) . . ? F4' C30' F6' 117.5(9) . . ? F5' O4' S2' 119.0(18) . . ? F5' O4' C30' 66.0(15) . . ? S2' O4' C30' 53.2(7) . . ? C30' F4' S2' 46.7(5) . . ? O4' F5' C30' 80.3(17) . . ? O4' F5' S2' 39.2(13) . . ? C30' F5' S2' 41.2(7) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.167 _refine_diff_density_min -1.151 _refine_diff_density_rms 0.126 #===END