# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Shigeki Kuwata' _publ_contact_author_email SKUWATA@APC.TITECH.AC.JP _publ_section_title ; Synthesis of parent amido (NH2)-bridged dinuclear complexes of ruthenium and iridium by stepwise transfer hydrogenation of mu-azido complexes ; loop_ _publ_author_name 'Shigeki Kuwata' 'Hiroko Arita' 'Takao Ikariya' 'Koji Ishiwata' 'Takashi Kimura' # Attachment 'Kuwata_CIF.cif' data___1a _database_code_depnum_ccdc_archive 'CCDC 713187' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C20 H30 Cl2 N4 Ru2 ' _chemical_formula_moiety 'C20 H30 Cl2 N4 Ru2 ' _chemical_formula_weight 599.53 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 1/2+X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 8.893(4) _cell_length_b 23.022(9) _cell_length_c 11.361(5) _cell_angle_alpha 90.0000 _cell_angle_beta 102.618(5) _cell_angle_gamma 90.0000 _cell_volume 2269.8(16) _cell_formula_units_Z 4 _cell_measurement_reflns_used 8189 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 31.5 _cell_measurement_temperature 193.1 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.754 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200.00 _exptl_absorpt_coefficient_mu 1.580 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.593 _exptl_absorpt_correction_T_max 0.729 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 20751 _diffrn_reflns_av_R_equivalents 0.065 _diffrn_reflns_theta_max 31.39 _diffrn_measured_fraction_theta_max 0.890 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.989 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 5164 _reflns_number_gt 3242 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_ref 0.1087 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 5163 _refine_ls_number_parameters 283 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0004Fo^2^ + 0.5000\s(Fo^2^)]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 1.07 _refine_diff_density_min -1.02 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ru Ru -1.259 0.836 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Ru(1) Ru 0.18757(5) 0.39176(2) 0.47512(4) 0.01993(11) Uani 1.00 1 d . . . Ru(2) Ru 0.12526(5) 0.27320(2) 0.62673(4) 0.02080(11) Uani 1.00 1 d . . . Cl(1) Cl -0.08969(16) 0.39173(6) 0.41703(14) 0.0311(3) Uani 1.00 1 d . . . Cl(2) Cl 0.40348(17) 0.26816(6) 0.69008(16) 0.0370(4) Uani 1.00 1 d . . . N(1) N 0.1547(5) 0.36466(18) 0.6464(4) 0.0267(13) Uani 1.00 1 d . . . N(2) N 0.1452(7) 0.3947(2) 0.7294(5) 0.0444(17) Uani 1.00 1 d . . . N(3) N 0.1334(11) 0.4248(3) 0.8080(6) 0.093(3) Uani 1.00 1 d . . . N(4) N 0.1678(5) 0.30130(17) 0.4625(4) 0.0248(12) Uani 1.00 1 d . . . C(1) C 0.2234(6) 0.4349(2) 0.3134(5) 0.0244(14) Uani 1.00 1 d . . . C(2) C 0.1921(6) 0.4777(2) 0.3969(5) 0.0284(15) Uani 1.00 1 d . . . C(3) C 0.2769(6) 0.4808(2) 0.5150(5) 0.0298(16) Uani 1.00 1 d . . . C(4) C 0.3966(6) 0.4391(2) 0.5578(5) 0.0303(15) Uani 1.00 1 d . . . C(5) C 0.4301(6) 0.3976(2) 0.4754(5) 0.0274(15) Uani 1.00 1 d . . . C(6) C 0.3428(6) 0.3961(2) 0.3549(5) 0.0238(14) Uani 1.00 1 d . . . C(7) C 0.1278(7) 0.4331(2) 0.1842(5) 0.0315(16) Uani 1.00 1 d . . . C(8) C 0.1791(7) 0.4830(2) 0.1129(6) 0.0428(19) Uani 1.00 1 d . . . C(9) C 0.1345(8) 0.3752(2) 0.1223(6) 0.046(2) Uani 1.00 1 d . . . C(10) C 0.4809(7) 0.4384(2) 0.6861(5) 0.0428(19) Uani 1.00 1 d . . . C(11) C 0.0853(6) 0.1799(2) 0.6314(5) 0.0233(14) Uani 1.00 1 d . . . C(12) C 0.1044(6) 0.2029(2) 0.7492(5) 0.0259(14) Uani 1.00 1 d . . . C(13) C 0.0152(6) 0.2498(2) 0.7763(5) 0.0270(15) Uani 1.00 1 d . . . C(14) C -0.0942(6) 0.2767(2) 0.6813(6) 0.0324(16) Uani 1.00 1 d . . . C(15) C -0.1162(6) 0.2537(2) 0.5649(5) 0.0293(15) Uani 1.00 1 d . . . C(16) C -0.0285(6) 0.2062(2) 0.5387(5) 0.0263(14) Uani 1.00 1 d . . . C(17) C 0.1874(7) 0.1306(2) 0.6070(5) 0.0317(16) Uani 1.00 1 d . . . C(18) C 0.1150(9) 0.0726(2) 0.6277(8) 0.064(2) Uani 1.00 1 d . . . C(19) C 0.2207(9) 0.1339(3) 0.4815(6) 0.050(2) Uani 1.00 1 d . . . C(20) C -0.1820(7) 0.3295(2) 0.7063(6) 0.045(2) Uani 1.00 1 d . . . H(1) H 0.0848 0.2907 0.3981 0.031 Uiso 1.00 1 c R . . H(2) H 0.2607 0.2847 0.4496 0.031 Uiso 1.00 1 c R . . H(3) H 0.1112 0.5048 0.3707 0.034 Uiso 1.00 1 c R . . H(4) H 0.2559 0.5104 0.5674 0.036 Uiso 1.00 1 c R . . H(5) H 0.5115 0.3706 0.5009 0.034 Uiso 1.00 1 c R . . H(6) H 0.3668 0.3677 0.3012 0.030 Uiso 1.00 1 c R . . H(7) H 0.0234 0.4400 0.1873 0.038 Uiso 1.00 1 c R . . H(8) H 0.1649 0.4722 0.0305 0.051 Uiso 1.00 1 c R . . H(9) H 0.1194 0.5165 0.1194 0.051 Uiso 1.00 1 c R . . H(10) H 0.2849 0.4911 0.1447 0.051 Uiso 1.00 1 c R . . H(11) H 0.2176 0.3755 0.0820 0.054 Uiso 1.00 1 c R . . H(12) H 0.0406 0.3689 0.0652 0.054 Uiso 1.00 1 c R . . H(13) H 0.1497 0.3449 0.1805 0.054 Uiso 1.00 1 c R . . H(14) H 0.4150 0.4519 0.7357 0.049 Uiso 1.00 1 c R . . H(15) H 0.5687 0.4628 0.6959 0.050 Uiso 1.00 1 c R . . H(16) H 0.5128 0.3998 0.7087 0.049 Uiso 1.00 1 c R . . H(17) H 0.1800 0.1863 0.8122 0.031 Uiso 1.00 1 c R . . H(18) H 0.0280 0.2632 0.8569 0.034 Uiso 1.00 1 c R . . H(19) H -0.1923 0.2702 0.5021 0.035 Uiso 1.00 1 c R . . H(20) H -0.0451 0.1917 0.4586 0.031 Uiso 1.00 1 c R . . H(21) H 0.2831 0.1337 0.6633 0.039 Uiso 1.00 1 c R . . H(22) H 0.1510 0.0613 0.7094 0.082 Uiso 1.00 1 c R . . H(23) H 0.0060 0.0763 0.6108 0.082 Uiso 1.00 1 c R . . H(24) H 0.1434 0.0440 0.5763 0.082 Uiso 1.00 1 c R . . H(25) H 0.1305 0.1464 0.4261 0.063 Uiso 1.00 1 c R . . H(26) H 0.2500 0.0966 0.4583 0.063 Uiso 1.00 1 c R . . H(27) H 0.3018 0.1607 0.4816 0.063 Uiso 1.00 1 c R . . H(28) H -0.1209 0.3510 0.7706 0.058 Uiso 1.00 1 c R . . H(29) H -0.2747 0.3177 0.7279 0.058 Uiso 1.00 1 c R . . H(30) H -0.2059 0.3530 0.6360 0.058 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru(1) 0.0216(2) 0.0154(2) 0.0234(2) 0.00157(17) 0.00637(18) 0.00018(17) Ru(2) 0.0207(2) 0.0184(2) 0.0233(2) -0.00002(17) 0.00489(18) 0.00122(17) Cl(1) 0.0250(7) 0.0250(6) 0.0419(9) 0.0021(5) 0.0044(6) 0.0027(6) Cl(2) 0.0237(7) 0.0332(7) 0.0512(10) -0.0010(5) 0.0017(6) 0.0079(7) N(1) 0.034(2) 0.022(2) 0.026(2) -0.0012(19) 0.012(2) -0.0023(19) N(2) 0.063(4) 0.043(3) 0.031(3) -0.017(2) 0.019(2) -0.005(2) N(3) 0.173(9) 0.064(4) 0.065(5) -0.033(5) 0.075(5) -0.033(4) N(4) 0.034(2) 0.017(2) 0.026(2) 0.0024(18) 0.011(2) -0.0018(18) C(1) 0.026(2) 0.021(2) 0.028(3) -0.002(2) 0.010(2) 0.001(2) C(2) 0.031(3) 0.017(2) 0.038(3) 0.001(2) 0.008(2) 0.008(2) C(3) 0.035(3) 0.016(2) 0.039(3) -0.004(2) 0.011(2) -0.001(2) C(4) 0.026(3) 0.028(2) 0.036(3) -0.006(2) 0.003(2) 0.001(2) C(5) 0.019(2) 0.027(2) 0.037(3) 0.001(2) 0.010(2) 0.005(2) C(6) 0.026(2) 0.019(2) 0.030(3) -0.002(2) 0.013(2) -0.002(2) C(7) 0.028(3) 0.035(3) 0.031(3) 0.000(2) 0.008(2) 0.011(2) C(8) 0.038(3) 0.048(3) 0.041(4) -0.003(3) 0.005(3) 0.012(3) C(9) 0.052(4) 0.042(3) 0.042(4) -0.008(3) 0.008(3) -0.003(3) C(10) 0.042(4) 0.043(3) 0.039(4) -0.012(3) -0.002(3) -0.001(3) C(11) 0.023(2) 0.017(2) 0.030(3) -0.006(2) 0.008(2) 0.004(2) C(12) 0.026(3) 0.029(2) 0.021(3) -0.002(2) 0.004(2) 0.007(2) C(13) 0.033(3) 0.027(2) 0.024(3) -0.004(2) 0.013(2) 0.005(2) C(14) 0.023(3) 0.029(2) 0.049(4) -0.001(2) 0.015(2) 0.002(2) C(15) 0.023(3) 0.035(3) 0.028(3) -0.004(2) 0.003(2) 0.011(2) C(16) 0.025(2) 0.023(2) 0.029(3) -0.008(2) -0.000(2) -0.002(2) C(17) 0.036(3) 0.021(2) 0.041(3) 0.004(2) 0.014(2) -0.007(2) C(18) 0.074(5) 0.022(3) 0.108(7) -0.002(3) 0.048(5) 0.005(3) C(19) 0.064(5) 0.049(3) 0.044(4) -0.003(3) 0.023(4) -0.012(3) C(20) 0.035(3) 0.050(3) 0.060(4) 0.011(3) 0.028(3) 0.005(3) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Ru(1) Cl(1) 2.4091(14) yes . . Ru(1) N(1) 2.124(5) yes . . Ru(1) N(4) 2.092(3) yes . . Ru(1) C(1) 2.173(5) yes . . Ru(1) C(2) 2.173(5) yes . . Ru(1) C(3) 2.209(5) yes . . Ru(1) C(4) 2.182(5) yes . . Ru(1) C(5) 2.160(5) yes . . Ru(1) C(6) 2.145(6) yes . . Ru(2) Cl(2) 2.4238(15) yes . . Ru(2) N(1) 2.127(4) yes . . Ru(2) N(4) 2.086(4) yes . . Ru(2) C(11) 2.181(4) yes . . Ru(2) C(12) 2.168(5) yes . . Ru(2) C(13) 2.205(6) yes . . Ru(2) C(14) 2.174(6) yes . . Ru(2) C(15) 2.156(5) yes . . Ru(2) C(16) 2.157(5) yes . . N(1) N(2) 1.187(7) yes . . N(2) N(3) 1.153(9) yes . . C(1) C(2) 1.437(8) yes . . C(1) C(6) 1.389(7) yes . . C(1) C(7) 1.527(7) yes . . C(2) C(3) 1.390(8) yes . . C(3) C(4) 1.436(7) yes . . C(4) C(5) 1.414(8) yes . . C(4) C(10) 1.487(8) yes . . C(5) C(6) 1.419(7) yes . . C(7) C(8) 1.530(9) yes . . C(7) C(9) 1.515(8) yes . . C(11) C(12) 1.415(8) yes . . C(11) C(16) 1.427(7) yes . . C(11) C(17) 1.516(8) yes . . C(12) C(13) 1.411(8) yes . . C(13) C(14) 1.427(7) yes . . C(14) C(15) 1.398(9) yes . . C(14) C(20) 1.505(8) yes . . C(15) C(16) 1.412(8) yes . . C(17) C(18) 1.522(8) yes . . C(17) C(19) 1.520(10) yes . . N(4) H(1) 0.950 no . . N(4) H(2) 0.950 no . . C(2) H(3) 0.950 no . . C(3) H(4) 0.950 no . . C(5) H(5) 0.950 no . . C(6) H(6) 0.950 no . . C(7) H(7) 0.950 no . . C(8) H(8) 0.950 no . . C(8) H(9) 0.950 no . . C(8) H(10) 0.950 no . . C(9) H(11) 0.950 no . . C(9) H(12) 0.950 no . . C(9) H(13) 0.950 no . . C(10) H(14) 0.950 no . . C(10) H(15) 0.950 no . . C(10) H(16) 0.950 no . . C(12) H(17) 0.950 no . . C(13) H(18) 0.950 no . . C(15) H(19) 0.950 no . . C(16) H(20) 0.950 no . . C(17) H(21) 0.950 no . . C(18) H(22) 0.950 no . . C(18) H(23) 0.950 no . . C(18) H(24) 0.950 no . . C(19) H(25) 0.950 no . . C(19) H(26) 0.950 no . . C(19) H(27) 0.950 no . . C(20) H(28) 0.950 no . . C(20) H(29) 0.950 no . . C(20) H(30) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Cl(1) Ru(1) N(1) 85.03(13) yes . . . Cl(1) Ru(1) N(4) 85.14(13) yes . . . Cl(1) Ru(1) C(1) 95.66(14) yes . . . Cl(1) Ru(1) C(2) 89.85(15) yes . . . Cl(1) Ru(1) C(3) 110.94(15) yes . . . Cl(1) Ru(1) C(4) 147.42(15) yes . . . Cl(1) Ru(1) C(5) 164.19(16) yes . . . Cl(1) Ru(1) C(6) 126.00(14) yes . . . N(1) Ru(1) N(4) 75.18(17) yes . . . N(1) Ru(1) C(1) 169.83(17) yes . . . N(1) Ru(1) C(2) 131.3(2) yes . . . N(1) Ru(1) C(3) 101.5(2) yes . . . N(1) Ru(1) C(4) 91.6(2) yes . . . N(1) Ru(1) C(5) 110.7(2) yes . . . N(1) Ru(1) C(6) 146.45(18) yes . . . N(4) Ru(1) C(1) 114.99(19) yes . . . N(4) Ru(1) C(2) 152.5(2) yes . . . N(4) Ru(1) C(3) 163.46(19) yes . . . N(4) Ru(1) C(4) 125.28(18) yes . . . N(4) Ru(1) C(5) 97.50(19) yes . . . N(4) Ru(1) C(6) 93.36(19) yes . . . C(1) Ru(1) C(2) 38.6(2) yes . . . C(1) Ru(1) C(3) 68.7(2) yes . . . C(1) Ru(1) C(4) 82.4(2) yes . . . C(1) Ru(1) C(5) 69.0(2) yes . . . C(1) Ru(1) C(6) 37.53(19) yes . . . C(2) Ru(1) C(3) 37.0(2) yes . . . C(2) Ru(1) C(4) 68.4(2) yes . . . C(2) Ru(1) C(5) 80.6(2) yes . . . C(2) Ru(1) C(6) 68.0(2) yes . . . C(3) Ru(1) C(4) 38.2(2) yes . . . C(3) Ru(1) C(5) 68.2(2) yes . . . C(3) Ru(1) C(6) 80.5(2) yes . . . C(4) Ru(1) C(5) 38.0(2) yes . . . C(4) Ru(1) C(6) 69.2(2) yes . . . C(5) Ru(1) C(6) 38.5(2) yes . . . Cl(2) Ru(2) N(1) 85.53(13) yes . . . Cl(2) Ru(2) N(4) 84.70(13) yes . . . Cl(2) Ru(2) C(11) 96.13(14) yes . . . Cl(2) Ru(2) C(12) 89.93(15) yes . . . Cl(2) Ru(2) C(13) 110.82(14) yes . . . Cl(2) Ru(2) C(14) 146.98(17) yes . . . Cl(2) Ru(2) C(15) 165.07(15) yes . . . Cl(2) Ru(2) C(16) 127.30(15) yes . . . N(1) Ru(2) N(4) 75.23(17) yes . . . N(1) Ru(2) C(11) 171.8(2) yes . . . N(1) Ru(2) C(12) 134.2(2) yes . . . N(1) Ru(2) C(13) 103.1(2) yes . . . N(1) Ru(2) C(14) 91.78(19) yes . . . N(1) Ru(2) C(15) 109.36(19) yes . . . N(1) Ru(2) C(16) 143.86(18) yes . . . N(4) Ru(2) C(11) 112.93(19) yes . . . N(4) Ru(2) C(12) 149.67(19) yes . . . N(4) Ru(2) C(13) 164.34(18) yes . . . N(4) Ru(2) C(14) 126.4(2) yes . . . N(4) Ru(2) C(15) 97.8(2) yes . . . N(4) Ru(2) C(16) 91.6(2) yes . . . C(11) Ru(2) C(12) 38.0(2) yes . . . C(11) Ru(2) C(13) 68.8(2) yes . . . C(11) Ru(2) C(14) 82.4(2) yes . . . C(11) Ru(2) C(15) 69.3(2) yes . . . C(11) Ru(2) C(16) 38.40(19) yes . . . C(12) Ru(2) C(13) 37.6(2) yes . . . C(12) Ru(2) C(14) 68.7(2) yes . . . C(12) Ru(2) C(15) 80.5(2) yes . . . C(12) Ru(2) C(16) 68.2(2) yes . . . C(13) Ru(2) C(14) 38.0(2) yes . . . C(13) Ru(2) C(15) 67.8(2) yes . . . C(13) Ru(2) C(16) 80.7(2) yes . . . C(14) Ru(2) C(15) 37.7(2) yes . . . C(14) Ru(2) C(16) 69.0(2) yes . . . C(15) Ru(2) C(16) 38.2(2) yes . . . Ru(1) N(1) Ru(2) 103.5(2) yes . . . Ru(1) N(1) N(2) 127.2(3) yes . . . Ru(2) N(1) N(2) 129.2(4) yes . . . N(1) N(2) N(3) 178.2(6) yes . . . Ru(1) N(4) Ru(2) 106.0(2) yes . . . Ru(1) C(1) C(2) 70.7(3) yes . . . Ru(1) C(1) C(6) 70.2(3) yes . . . Ru(1) C(1) C(7) 130.3(3) yes . . . C(2) C(1) C(6) 117.4(4) yes . . . C(2) C(1) C(7) 120.4(4) yes . . . C(6) C(1) C(7) 122.2(5) yes . . . Ru(1) C(2) C(1) 70.7(2) yes . . . Ru(1) C(2) C(3) 72.9(3) yes . . . C(1) C(2) C(3) 122.0(4) yes . . . Ru(1) C(3) C(2) 70.1(2) yes . . . Ru(1) C(3) C(4) 69.9(2) yes . . . C(2) C(3) C(4) 119.9(5) yes . . . Ru(1) C(4) C(3) 71.9(3) yes . . . Ru(1) C(4) C(5) 70.1(3) yes . . . Ru(1) C(4) C(10) 128.0(4) yes . . . C(3) C(4) C(5) 118.4(5) yes . . . C(3) C(4) C(10) 121.2(5) yes . . . C(5) C(4) C(10) 120.5(5) yes . . . Ru(1) C(5) C(4) 71.8(3) yes . . . Ru(1) C(5) C(6) 70.2(3) yes . . . C(4) C(5) C(6) 120.3(4) yes . . . Ru(1) C(6) C(1) 72.3(3) yes . . . Ru(1) C(6) C(5) 71.3(3) yes . . . C(1) C(6) C(5) 122.0(5) yes . . . C(1) C(7) C(8) 108.8(4) yes . . . C(1) C(7) C(9) 113.6(4) yes . . . C(8) C(7) C(9) 111.6(5) yes . . . Ru(2) C(11) C(12) 70.5(2) yes . . . Ru(2) C(11) C(16) 69.9(2) yes . . . Ru(2) C(11) C(17) 128.8(4) yes . . . C(12) C(11) C(16) 117.2(4) yes . . . C(12) C(11) C(17) 120.1(4) yes . . . C(16) C(11) C(17) 122.7(5) yes . . . Ru(2) C(12) C(11) 71.5(3) yes . . . Ru(2) C(12) C(13) 72.6(3) yes . . . C(11) C(12) C(13) 122.5(4) yes . . . Ru(2) C(13) C(12) 69.7(3) yes . . . Ru(2) C(13) C(14) 69.8(3) yes . . . C(12) C(13) C(14) 119.3(5) yes . . . Ru(2) C(14) C(13) 72.2(3) yes . . . Ru(2) C(14) C(15) 70.5(3) yes . . . Ru(2) C(14) C(20) 128.2(4) yes . . . C(13) C(14) C(15) 118.8(5) yes . . . C(13) C(14) C(20) 120.3(5) yes . . . C(15) C(14) C(20) 120.8(5) yes . . . Ru(2) C(15) C(14) 71.9(3) yes . . . Ru(2) C(15) C(16) 70.9(3) yes . . . C(14) C(15) C(16) 121.5(4) yes . . . Ru(2) C(16) C(11) 71.7(2) yes . . . Ru(2) C(16) C(15) 70.9(3) yes . . . C(11) C(16) C(15) 120.6(5) yes . . . C(11) C(17) C(18) 109.7(5) yes . . . C(11) C(17) C(19) 112.4(4) yes . . . C(18) C(17) C(19) 111.4(5) yes . . . Ru(1) N(4) H(1) 110.3 no . . . Ru(1) N(4) H(2) 110.4 no . . . Ru(2) N(4) H(1) 110.3 no . . . Ru(2) N(4) H(2) 110.3 no . . . H(1) N(4) H(2) 109.5 no . . . Ru(1) C(2) H(3) 130.3 no . . . C(1) C(2) H(3) 119.1 no . . . C(3) C(2) H(3) 118.9 no . . . Ru(1) C(3) H(4) 133.0 no . . . C(2) C(3) H(4) 120.1 no . . . C(4) C(3) H(4) 120.0 no . . . Ru(1) C(5) H(5) 130.9 no . . . C(4) C(5) H(5) 119.8 no . . . C(6) C(5) H(5) 119.9 no . . . Ru(1) C(6) H(6) 130.0 no . . . C(1) C(6) H(6) 119.1 no . . . C(5) C(6) H(6) 118.9 no . . . C(1) C(7) H(7) 107.6 no . . . C(8) C(7) H(7) 107.6 no . . . C(9) C(7) H(7) 107.5 no . . . C(7) C(8) H(8) 109.6 no . . . C(7) C(8) H(9) 109.4 no . . . C(7) C(8) H(10) 109.3 no . . . H(8) C(8) H(9) 109.5 no . . . H(8) C(8) H(10) 109.5 no . . . H(9) C(8) H(10) 109.5 no . . . C(7) C(9) H(11) 109.3 no . . . C(7) C(9) H(12) 109.5 no . . . C(7) C(9) H(13) 109.6 no . . . H(11) C(9) H(12) 109.5 no . . . H(11) C(9) H(13) 109.5 no . . . H(12) C(9) H(13) 109.5 no . . . C(4) C(10) H(14) 109.5 no . . . C(4) C(10) H(15) 109.5 no . . . C(4) C(10) H(16) 109.4 no . . . H(14) C(10) H(15) 109.5 no . . . H(14) C(10) H(16) 109.5 no . . . H(15) C(10) H(16) 109.5 no . . . Ru(2) C(12) H(17) 129.8 no . . . C(11) C(12) H(17) 118.7 no . . . C(13) C(12) H(17) 118.9 no . . . Ru(2) C(13) H(18) 133.1 no . . . C(12) C(13) H(18) 120.4 no . . . C(14) C(13) H(18) 120.3 no . . . Ru(2) C(15) H(19) 131.0 no . . . C(14) C(15) H(19) 119.3 no . . . C(16) C(15) H(19) 119.2 no . . . Ru(2) C(16) H(20) 130.2 no . . . C(11) C(16) H(20) 119.7 no . . . C(15) C(16) H(20) 119.7 no . . . C(11) C(17) H(21) 107.7 no . . . C(18) C(17) H(21) 108.0 no . . . C(19) C(17) H(21) 107.4 no . . . C(17) C(18) H(22) 109.1 no . . . C(17) C(18) H(23) 109.8 no . . . C(17) C(18) H(24) 109.5 no . . . H(22) C(18) H(23) 109.5 no . . . H(22) C(18) H(24) 109.5 no . . . H(23) C(18) H(24) 109.5 no . . . C(17) C(19) H(25) 109.1 no . . . C(17) C(19) H(26) 109.7 no . . . C(17) C(19) H(27) 109.6 no . . . H(25) C(19) H(26) 109.5 no . . . H(25) C(19) H(27) 109.5 no . . . H(26) C(19) H(27) 109.5 no . . . C(14) C(20) H(28) 109.5 no . . . C(14) C(20) H(29) 109.5 no . . . C(14) C(20) H(30) 109.5 no . . . H(28) C(20) H(29) 109.5 no . . . H(28) C(20) H(30) 109.5 no . . . H(29) C(20) H(30) 109.5 no . . . #===END data___2a _database_code_depnum_ccdc_archive 'CCDC 713188' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C20 H31 Cl2 N Ru2 ' _chemical_formula_moiety 'C20 H31 Cl2 N Ru2 ' _chemical_formula_weight 558.52 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z #------------------------------------------------------------------------------ _cell_length_a 9.245(4) _cell_length_b 10.429(4) _cell_length_c 12.464(6) _cell_angle_alpha 70.900(14) _cell_angle_beta 84.302(17) _cell_angle_gamma 70.759(16) _cell_volume 1072.0(8) _cell_formula_units_Z 2 _cell_measurement_reflns_used 3858 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 31.5 _cell_measurement_temperature 193.1 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.730 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 560.00 _exptl_absorpt_coefficient_mu 1.662 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.564 _exptl_absorpt_correction_T_max 0.717 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 9582 _diffrn_reflns_av_R_equivalents 0.043 _diffrn_reflns_theta_max 31.40 _diffrn_measured_fraction_theta_max 0.790 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.932 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 4592 _reflns_number_gt 3306 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.1206 _refine_ls_hydrogen_treatment mixed _refine_ls_number_reflns 4591 _refine_ls_number_parameters 259 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0008Fo^2^ + 0.9000\s(Fo^2^)]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 1.08 _refine_diff_density_min -0.97 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ru Ru -1.259 0.836 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Ru(1) Ru 0.12656(5) 0.55649(5) 0.15235(4) 0.02094(12) Uani 1.00 1 d . . . Ru(2) Ru -0.07735(5) 0.44448(5) 0.31714(4) 0.02055(12) Uani 1.00 1 d . . . Cl(1) Cl -0.09681(17) 0.73390(16) 0.04666(13) 0.0314(3) Uani 1.00 1 d . . . Cl(2) Cl 0.14045(17) 0.23741(15) 0.39892(13) 0.0312(3) Uani 1.00 1 d . . . N(1) N 0.0073(5) 0.4156(5) 0.1644(3) 0.0261(12) Uani 1.00 1 d . . . C(1) C 0.2664(6) 0.7047(6) 0.1132(5) 0.0278(15) Uani 1.00 1 d . . . C(2) C 0.3058(6) 0.6056(5) 0.2207(4) 0.0212(14) Uani 1.00 1 d . . . C(3) C 0.3477(6) 0.4559(6) 0.2393(5) 0.0264(15) Uani 1.00 1 d . . . C(4) C 0.3531(6) 0.4024(6) 0.1474(5) 0.0278(15) Uani 1.00 1 d . . . C(5) C 0.3168(6) 0.5023(6) 0.0374(5) 0.0306(16) Uani 1.00 1 d . . . C(6) C 0.2717(7) 0.6506(6) 0.0221(5) 0.0308(16) Uani 1.00 1 d . . . C(7) C 0.2196(7) 0.8651(6) 0.0936(5) 0.0316(16) Uani 1.00 1 d . . . C(8) C 0.1137(9) 0.9131(7) 0.1831(6) 0.051(2) Uani 1.00 1 d . . . C(9) C 0.3608(8) 0.9096(7) 0.0809(7) 0.051(2) Uani 1.00 1 d . . . C(10) C 0.3948(7) 0.2454(6) 0.1654(6) 0.040(2) Uani 1.00 1 d . . . C(11) C -0.2433(6) 0.3370(5) 0.4093(5) 0.0248(14) Uani 1.00 1 d . . . C(12) C -0.1912(7) 0.3942(6) 0.4809(5) 0.0313(16) Uani 1.00 1 d . . . C(13) C -0.2019(7) 0.5403(6) 0.4482(5) 0.0312(16) Uani 1.00 1 d . . . C(14) C -0.2603(6) 0.6341(6) 0.3381(5) 0.0290(16) Uani 1.00 1 d . . . C(15) C -0.3130(6) 0.5755(5) 0.2664(5) 0.0258(14) Uani 1.00 1 d . . . C(16) C -0.3025(6) 0.4292(6) 0.3016(4) 0.0247(14) Uani 1.00 1 d . . . C(17) C -0.2267(7) 0.1791(6) 0.4495(5) 0.0307(16) Uani 1.00 1 d . . . C(18) C -0.1988(10) 0.1124(6) 0.3541(6) 0.051(2) Uani 1.00 1 d . . . C(19) C -0.3685(8) 0.1568(7) 0.5193(7) 0.053(2) Uani 1.00 1 d . . . C(20) C -0.2682(7) 0.7862(6) 0.3027(6) 0.0384(19) Uani 1.00 1 d . . . H(1) H -0.0683 0.4478 0.1069 0.030 Uiso 1.00 1 c R . . H(2) H 0.0700 0.3210 0.1697 0.030 Uiso 1.00 1 c R . . H(3) H 0.028(7) 0.559(6) 0.274(5) 0.0380 Uiso 1.00 1 c . . . H(4) H 0.3037 0.6387 0.2834 0.029 Uiso 1.00 1 c R . . H(5) H 0.3727 0.3901 0.3135 0.031 Uiso 1.00 1 c R . . H(6) H 0.3261 0.4693 -0.0262 0.038 Uiso 1.00 1 c R . . H(7) H 0.2417 0.7162 -0.0515 0.038 Uiso 1.00 1 c R . . H(8) H 0.1655 0.9111 0.0233 0.035 Uiso 1.00 1 c R . . H(9) H 0.0101 0.9355 0.1621 0.059 Uiso 1.00 1 c R . . H(10) H 0.1289 0.9954 0.1906 0.059 Uiso 1.00 1 c R . . H(11) H 0.1354 0.8390 0.2538 0.059 Uiso 1.00 1 c R . . H(12) H 0.3890 0.9040 0.1538 0.062 Uiso 1.00 1 c R . . H(13) H 0.3401 1.0046 0.0309 0.062 Uiso 1.00 1 c R . . H(14) H 0.4422 0.8476 0.0511 0.062 Uiso 1.00 1 c R . . H(15) H 0.5025 0.2063 0.1588 0.051 Uiso 1.00 1 c R . . H(16) H 0.3444 0.2305 0.1100 0.051 Uiso 1.00 1 c R . . H(17) H 0.3636 0.1995 0.2389 0.051 Uiso 1.00 1 c R . . H(18) H -0.1484 0.3330 0.5530 0.035 Uiso 1.00 1 c R . . H(19) H -0.1703 0.5770 0.4990 0.041 Uiso 1.00 1 c R . . H(20) H -0.3544 0.6364 0.1938 0.029 Uiso 1.00 1 c R . . H(21) H -0.3376 0.3930 0.2522 0.030 Uiso 1.00 1 c R . . H(22) H -0.1415 0.1312 0.5001 0.037 Uiso 1.00 1 c R . . H(23) H -0.2934 0.1206 0.3246 0.064 Uiso 1.00 1 c R . . H(24) H -0.1397 0.0145 0.3827 0.064 Uiso 1.00 1 c R . . H(25) H -0.1436 0.1607 0.2955 0.063 Uiso 1.00 1 c R . . H(26) H -0.3522 0.1416 0.5971 0.059 Uiso 1.00 1 c R . . H(27) H -0.3864 0.0758 0.5114 0.059 Uiso 1.00 1 c R . . H(28) H -0.4554 0.2386 0.4917 0.059 Uiso 1.00 1 c R . . H(29) H -0.3637 0.8420 0.3238 0.047 Uiso 1.00 1 c R . . H(30) H -0.2579 0.8188 0.2226 0.047 Uiso 1.00 1 c R . . H(31) H -0.1873 0.7946 0.3384 0.047 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru(1) 0.0175(2) 0.0248(2) 0.0205(2) -0.00703(19) 0.00051(18) -0.00679(18) Ru(2) 0.0183(2) 0.0234(2) 0.0207(2) -0.00698(19) 0.00006(18) -0.00746(18) Cl(1) 0.0258(7) 0.0315(7) 0.0285(7) -0.0038(6) -0.0049(6) -0.0022(5) Cl(2) 0.0274(7) 0.0264(7) 0.0339(7) -0.0058(6) -0.0022(6) -0.0038(5) N(1) 0.017(2) 0.039(2) 0.019(2) -0.005(2) 0.0005(19) -0.010(2) C(1) 0.017(2) 0.041(3) 0.025(2) -0.014(2) 0.004(2) -0.006(2) C(2) 0.021(2) 0.023(2) 0.030(2) -0.017(2) 0.002(2) -0.011(2) C(3) 0.015(2) 0.032(3) 0.030(3) -0.010(2) -0.000(2) -0.003(2) C(4) 0.014(2) 0.032(3) 0.038(3) -0.008(2) 0.004(2) -0.012(2) C(5) 0.020(2) 0.045(3) 0.030(3) -0.008(2) 0.007(2) -0.020(2) C(6) 0.034(3) 0.032(3) 0.028(3) -0.015(2) 0.001(2) -0.007(2) C(7) 0.026(3) 0.028(3) 0.034(3) -0.008(2) 0.003(2) -0.002(2) C(8) 0.055(4) 0.039(4) 0.053(4) -0.013(3) 0.014(4) -0.014(3) C(9) 0.033(3) 0.029(3) 0.092(6) -0.014(3) 0.008(4) -0.020(3) C(10) 0.024(3) 0.044(3) 0.059(4) -0.005(3) 0.004(3) -0.033(3) C(11) 0.022(2) 0.025(2) 0.029(3) -0.012(2) 0.009(2) -0.007(2) C(12) 0.024(3) 0.040(3) 0.023(2) -0.008(2) 0.002(2) -0.004(2) C(13) 0.026(3) 0.042(3) 0.034(3) -0.017(2) 0.009(2) -0.021(2) C(14) 0.018(2) 0.037(3) 0.037(3) -0.012(2) 0.006(2) -0.017(2) C(15) 0.015(2) 0.023(2) 0.033(3) 0.001(2) -0.001(2) -0.008(2) C(16) 0.013(2) 0.034(3) 0.028(3) -0.012(2) 0.004(2) -0.007(2) C(17) 0.032(3) 0.027(3) 0.033(3) -0.014(2) 0.000(2) -0.004(2) C(18) 0.087(6) 0.023(3) 0.048(4) -0.024(3) -0.002(4) -0.012(3) C(19) 0.042(4) 0.044(4) 0.060(5) -0.020(3) 0.005(3) 0.005(3) C(20) 0.039(3) 0.032(3) 0.046(4) -0.013(3) 0.011(3) -0.016(2) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Ru(1) Ru(2) 2.8721(6) yes . . Ru(1) Cl(1) 2.4186(13) yes . . Ru(1) N(1) 2.071(6) yes . . Ru(1) C(1) 2.236(7) yes . . Ru(1) C(2) 2.204(6) yes . . Ru(1) C(3) 2.177(5) yes . . Ru(1) C(4) 2.190(5) yes . . Ru(1) C(5) 2.199(6) yes . . Ru(1) C(6) 2.189(6) yes . . Ru(2) Cl(2) 2.4203(12) yes . . Ru(2) N(1) 2.062(5) yes . . Ru(2) C(11) 2.207(6) yes . . Ru(2) C(12) 2.188(6) yes . . Ru(2) C(13) 2.221(6) yes . . Ru(2) C(14) 2.210(5) yes . . Ru(2) C(15) 2.182(5) yes . . Ru(2) C(16) 2.171(6) yes . . C(1) C(2) 1.392(7) yes . . C(1) C(6) 1.414(10) yes . . C(1) C(7) 1.523(9) yes . . C(2) C(3) 1.423(8) yes . . C(3) C(4) 1.420(10) yes . . C(4) C(5) 1.415(7) yes . . C(4) C(10) 1.497(9) yes . . C(5) C(6) 1.414(9) yes . . C(7) C(8) 1.510(10) yes . . C(7) C(9) 1.502(11) yes . . C(11) C(12) 1.417(11) yes . . C(11) C(16) 1.406(7) yes . . C(11) C(17) 1.515(8) yes . . C(12) C(13) 1.414(9) yes . . C(13) C(14) 1.433(8) yes . . C(14) C(15) 1.432(11) yes . . C(14) C(20) 1.479(9) yes . . C(15) C(16) 1.415(8) yes . . C(17) C(18) 1.525(11) yes . . C(17) C(19) 1.540(10) yes . . Ru(1) H(3) 1.70(6) no . . Ru(2) H(3) 1.71(7) no . . N(1) H(1) 0.949 no . . N(1) H(2) 0.950 no . . C(2) H(4) 0.949 no . . C(3) H(5) 0.949 no . . C(5) H(6) 0.950 no . . C(6) H(7) 0.949 no . . C(7) H(8) 0.949 no . . C(8) H(9) 0.950 no . . C(8) H(10) 0.949 no . . C(8) H(11) 0.949 no . . C(9) H(12) 0.949 no . . C(9) H(13) 0.949 no . . C(9) H(14) 0.950 no . . C(10) H(15) 0.950 no . . C(10) H(16) 0.949 no . . C(10) H(17) 0.950 no . . C(12) H(18) 0.949 no . . C(13) H(19) 0.949 no . . C(15) H(20) 0.949 no . . C(16) H(21) 0.949 no . . C(17) H(22) 0.949 no . . C(18) H(23) 0.949 no . . C(18) H(24) 0.949 no . . C(18) H(25) 0.950 no . . C(19) H(26) 0.949 no . . C(19) H(27) 0.950 no . . C(19) H(28) 0.949 no . . C(20) H(29) 0.950 no . . C(20) H(30) 0.950 no . . C(20) H(31) 0.949 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Ru(2) Ru(1) Cl(1) 87.99(3) yes . . . Ru(2) Ru(1) N(1) 45.86(13) yes . . . Ru(2) Ru(1) C(1) 142.93(17) yes . . . Ru(2) Ru(1) C(2) 115.57(14) yes . . . Ru(2) Ru(1) C(3) 103.34(15) yes . . . Ru(2) Ru(1) C(4) 114.66(15) yes . . . Ru(2) Ru(1) C(5) 144.27(18) yes . . . Ru(2) Ru(1) C(6) 177.06(14) yes . . . Cl(1) Ru(1) N(1) 83.96(12) yes . . . Cl(1) Ru(1) C(1) 94.89(13) yes . . . Cl(1) Ru(1) C(2) 124.65(13) yes . . . Cl(1) Ru(1) C(3) 162.17(18) yes . . . Cl(1) Ru(1) C(4) 147.22(17) yes . . . Cl(1) Ru(1) C(5) 110.86(14) yes . . . Cl(1) Ru(1) C(6) 89.08(15) yes . . . N(1) Ru(1) C(1) 171.2(2) yes . . . N(1) Ru(1) C(2) 148.55(16) yes . . . N(1) Ru(1) C(3) 113.8(2) yes . . . N(1) Ru(1) C(4) 95.0(2) yes . . . N(1) Ru(1) C(5) 104.3(2) yes . . . N(1) Ru(1) C(6) 133.9(2) yes . . . C(1) Ru(1) C(2) 36.54(19) yes . . . C(1) Ru(1) C(3) 67.8(2) yes . . . C(1) Ru(1) C(4) 81.2(2) yes . . . C(1) Ru(1) C(5) 67.9(2) yes . . . C(1) Ru(1) C(6) 37.3(2) yes . . . C(2) Ru(1) C(3) 37.9(2) yes . . . C(2) Ru(1) C(4) 68.4(2) yes . . . C(2) Ru(1) C(5) 79.2(2) yes . . . C(2) Ru(1) C(6) 66.1(2) yes . . . C(3) Ru(1) C(4) 38.0(2) yes . . . C(3) Ru(1) C(5) 67.4(2) yes . . . C(3) Ru(1) C(6) 79.5(2) yes . . . C(4) Ru(1) C(5) 37.6(2) yes . . . C(4) Ru(1) C(6) 68.1(2) yes . . . C(5) Ru(1) C(6) 37.6(2) yes . . . Ru(1) Ru(2) Cl(2) 88.07(3) yes . . . Ru(1) Ru(2) N(1) 46.10(17) yes . . . Ru(1) Ru(2) C(11) 165.16(18) yes . . . Ru(1) Ru(2) C(12) 157.2(2) yes . . . Ru(1) Ru(2) C(13) 125.33(19) yes . . . Ru(1) Ru(2) C(14) 105.28(16) yes . . . Ru(1) Ru(2) C(15) 108.97(15) yes . . . Ru(1) Ru(2) C(16) 132.24(14) yes . . . Cl(2) Ru(2) N(1) 84.58(12) yes . . . Cl(2) Ru(2) C(11) 92.81(13) yes . . . Cl(2) Ru(2) C(12) 88.07(14) yes . . . Cl(2) Ru(2) C(13) 111.16(14) yes . . . Cl(2) Ru(2) C(14) 148.04(18) yes . . . Cl(2) Ru(2) C(15) 160.23(17) yes . . . Cl(2) Ru(2) C(16) 122.64(15) yes . . . N(1) Ru(2) C(11) 119.2(2) yes . . . N(1) Ru(2) C(12) 155.3(2) yes . . . N(1) Ru(2) C(13) 163.04(18) yes . . . N(1) Ru(2) C(14) 125.63(19) yes . . . N(1) Ru(2) C(15) 99.8(2) yes . . . N(1) Ru(2) C(16) 97.1(2) yes . . . C(11) Ru(2) C(12) 37.6(2) yes . . . C(11) Ru(2) C(13) 68.0(2) yes . . . C(11) Ru(2) C(14) 81.5(2) yes . . . C(11) Ru(2) C(15) 68.13(19) yes . . . C(11) Ru(2) C(16) 37.5(2) yes . . . C(12) Ru(2) C(13) 37.4(2) yes . . . C(12) Ru(2) C(14) 68.3(2) yes . . . C(12) Ru(2) C(15) 79.9(2) yes . . . C(12) Ru(2) C(16) 67.5(2) yes . . . C(13) Ru(2) C(14) 37.7(2) yes . . . C(13) Ru(2) C(15) 67.6(2) yes . . . C(13) Ru(2) C(16) 80.1(2) yes . . . C(14) Ru(2) C(15) 38.0(2) yes . . . C(14) Ru(2) C(16) 68.9(2) yes . . . C(15) Ru(2) C(16) 37.9(2) yes . . . Ru(1) N(1) Ru(2) 88.0(2) yes . . . Ru(1) C(1) C(2) 70.5(3) yes . . . Ru(1) C(1) C(6) 69.6(4) yes . . . Ru(1) C(1) C(7) 131.0(4) yes . . . C(2) C(1) C(6) 117.3(5) yes . . . C(2) C(1) C(7) 121.8(6) yes . . . C(6) C(1) C(7) 121.0(4) yes . . . Ru(1) C(2) C(1) 73.0(4) yes . . . Ru(1) C(2) C(3) 70.0(3) yes . . . C(1) C(2) C(3) 121.8(6) yes . . . Ru(1) C(3) C(2) 72.1(3) yes . . . Ru(1) C(3) C(4) 71.5(3) yes . . . C(2) C(3) C(4) 120.6(4) yes . . . Ru(1) C(4) C(3) 70.5(3) yes . . . Ru(1) C(4) C(5) 71.6(3) yes . . . Ru(1) C(4) C(10) 128.7(4) yes . . . C(3) C(4) C(5) 118.0(5) yes . . . C(3) C(4) C(10) 121.4(5) yes . . . C(5) C(4) C(10) 120.6(6) yes . . . Ru(1) C(5) C(4) 70.8(3) yes . . . Ru(1) C(5) C(6) 70.8(3) yes . . . C(4) C(5) C(6) 120.1(6) yes . . . Ru(1) C(6) C(1) 73.2(3) yes . . . Ru(1) C(6) C(5) 71.6(3) yes . . . C(1) C(6) C(5) 122.2(5) yes . . . C(1) C(7) C(8) 113.7(5) yes . . . C(1) C(7) C(9) 109.2(4) yes . . . C(8) C(7) C(9) 112.1(7) yes . . . Ru(2) C(11) C(12) 70.5(3) yes . . . Ru(2) C(11) C(16) 69.9(3) yes . . . Ru(2) C(11) C(17) 128.9(4) yes . . . C(12) C(11) C(16) 118.0(5) yes . . . C(12) C(11) C(17) 118.9(5) yes . . . C(16) C(11) C(17) 123.0(6) yes . . . Ru(2) C(12) C(11) 71.9(3) yes . . . Ru(2) C(12) C(13) 72.6(3) yes . . . C(11) C(12) C(13) 121.8(5) yes . . . Ru(2) C(13) C(12) 70.0(3) yes . . . Ru(2) C(13) C(14) 70.7(3) yes . . . C(12) C(13) C(14) 120.2(7) yes . . . Ru(2) C(14) C(13) 71.5(3) yes . . . Ru(2) C(14) C(15) 69.9(3) yes . . . Ru(2) C(14) C(20) 130.8(4) yes . . . C(13) C(14) C(15) 117.5(6) yes . . . C(13) C(14) C(20) 120.3(7) yes . . . C(15) C(14) C(20) 122.2(5) yes . . . Ru(2) C(15) C(14) 72.1(3) yes . . . Ru(2) C(15) C(16) 70.6(2) yes . . . C(14) C(15) C(16) 121.1(5) yes . . . Ru(2) C(16) C(11) 72.6(3) yes . . . Ru(2) C(16) C(15) 71.4(3) yes . . . C(11) C(16) C(15) 121.2(6) yes . . . C(11) C(17) C(18) 113.9(5) yes . . . C(11) C(17) C(19) 109.0(5) yes . . . C(18) C(17) C(19) 111.5(7) yes . . . Ru(2) Ru(1) H(3) 33(2) no . . . Cl(1) Ru(1) H(3) 89.0(19) no . . . N(1) Ru(1) H(3) 78(2) no . . . C(1) Ru(1) H(3) 110(2) no . . . C(2) Ru(1) H(3) 88(2) no . . . C(3) Ru(1) H(3) 93(2) no . . . C(4) Ru(1) H(3) 123.0(18) no . . . C(5) Ru(1) H(3) 160.1(19) no . . . C(6) Ru(1) H(3) 147(2) no . . . Ru(1) Ru(2) H(3) 32(2) no . . . Cl(2) Ru(2) H(3) 94.1(17) no . . . N(1) Ru(2) H(3) 78(2) no . . . C(11) Ru(2) H(3) 162(2) no . . . C(12) Ru(2) H(3) 126(2) no . . . C(13) Ru(2) H(3) 94(2) no . . . C(14) Ru(2) H(3) 83.6(19) no . . . C(15) Ru(2) H(3) 105.6(17) no . . . C(16) Ru(2) H(3) 142.6(17) no . . . Ru(1) N(1) H(1) 114.5 no . . . Ru(1) N(1) H(2) 114.6 no . . . Ru(2) N(1) H(1) 114.4 no . . . Ru(2) N(1) H(2) 114.6 no . . . H(1) N(1) H(2) 109.5 no . . . Ru(1) C(2) H(4) 130.2 no . . . C(1) C(2) H(4) 119.2 no . . . C(3) C(2) H(4) 119.0 no . . . Ru(1) C(3) H(5) 129.1 no . . . C(2) C(3) H(5) 120.5 no . . . C(4) C(3) H(5) 118.9 no . . . Ru(1) C(5) H(6) 133.0 no . . . C(4) C(5) H(6) 119.7 no . . . C(6) C(5) H(6) 120.1 no . . . Ru(1) C(6) H(7) 127.5 no . . . C(1) C(6) H(7) 118.7 no . . . C(5) C(6) H(7) 119.0 no . . . C(1) C(7) H(8) 106.9 no . . . C(8) C(7) H(8) 107.2 no . . . C(9) C(7) H(8) 107.3 no . . . C(7) C(8) H(9) 110.1 no . . . C(7) C(8) H(10) 109.4 no . . . C(7) C(8) H(11) 109.7 no . . . H(9) C(8) H(10) 109.3 no . . . H(9) C(8) H(11) 109.4 no . . . H(10) C(8) H(11) 108.9 no . . . C(7) C(9) H(12) 107.9 no . . . C(7) C(9) H(13) 109.7 no . . . C(7) C(9) H(14) 110.3 no . . . H(12) C(9) H(13) 110.3 no . . . H(12) C(9) H(14) 109.5 no . . . H(13) C(9) H(14) 109.1 no . . . C(4) C(10) H(15) 109.6 no . . . C(4) C(10) H(16) 109.5 no . . . C(4) C(10) H(17) 109.6 no . . . H(15) C(10) H(16) 109.4 no . . . H(15) C(10) H(17) 109.5 no . . . H(16) C(10) H(17) 109.2 no . . . Ru(2) C(12) H(18) 129.2 no . . . C(11) C(12) H(18) 119.2 no . . . C(13) C(12) H(18) 119.0 no . . . Ru(2) C(13) H(19) 132.3 no . . . C(12) C(13) H(19) 120.3 no . . . C(14) C(13) H(19) 119.5 no . . . Ru(2) C(15) H(20) 129.9 no . . . C(14) C(15) H(20) 118.8 no . . . C(16) C(15) H(20) 120.1 no . . . Ru(2) C(16) H(21) 129.8 no . . . C(11) C(16) H(21) 119.4 no . . . C(15) C(16) H(21) 119.3 no . . . C(11) C(17) H(22) 107.6 no . . . C(18) C(17) H(22) 108.0 no . . . C(19) C(17) H(22) 106.5 no . . . C(17) C(18) H(23) 110.4 no . . . C(17) C(18) H(24) 109.2 no . . . C(17) C(18) H(25) 108.8 no . . . H(23) C(18) H(24) 109.7 no . . . H(23) C(18) H(25) 109.5 no . . . H(24) C(18) H(25) 109.1 no . . . C(17) C(19) H(26) 110.3 no . . . C(17) C(19) H(27) 108.8 no . . . C(17) C(19) H(28) 109.7 no . . . H(26) C(19) H(27) 109.4 no . . . H(26) C(19) H(28) 109.4 no . . . H(27) C(19) H(28) 109.1 no . . . C(14) C(20) H(29) 110.2 no . . . C(14) C(20) H(30) 108.7 no . . . C(14) C(20) H(31) 109.1 no . . . H(29) C(20) H(30) 109.4 no . . . H(29) C(20) H(31) 109.5 no . . . H(30) C(20) H(31) 109.8 no . . . Ru(1) H(3) Ru(2) 115(4) no . . . #===END data___2b _database_code_depnum_ccdc_archive 'CCDC 713189' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C20 H33 Cl2 Ir2 N ' _chemical_formula_moiety 'C20 H33 Cl2 Ir2 N ' _chemical_formula_weight 742.83 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,+Y,1/2-Z 3 -X,-Y,-Z 4 +X,-Y,1/2+Z 5 1/2+X,1/2+Y,+Z 6 1/2-X,1/2+Y,1/2-Z 7 1/2-X,1/2-Y,-Z 8 1/2+X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 19.250(9) _cell_length_b 13.076(6) _cell_length_c 9.060(4) _cell_angle_alpha 90.0000 _cell_angle_beta 92.449(8) _cell_angle_gamma 90.0000 _cell_volume 2278.6(19) _cell_formula_units_Z 4 _cell_measurement_reflns_used 3829 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 31.5 _cell_measurement_temperature 293.1 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 2.165 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392.00 _exptl_absorpt_coefficient_mu 11.939 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.070 _exptl_absorpt_correction_T_max 0.303 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 9859 _diffrn_reflns_av_R_equivalents 0.051 _diffrn_reflns_theta_max 31.33 _diffrn_measured_fraction_theta_max 0.880 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.967 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 2529 _reflns_number_gt 1991 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0289 _refine_ls_wR_factor_ref 0.0980 _refine_ls_hydrogen_treatment mixed _refine_ls_number_reflns 2528 _refine_ls_number_parameters 134 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0009Fo^2^ + 0.5000\s(Fo^2^)]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 1.04 _refine_diff_density_min -1.10 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ir Ir -1.444 7.990 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Ir(1) Ir 0.426600(10) 0.28135(2) 0.71961(2) 0.03215(8) Uani 1.00 1 d . . . Cl(1) Cl 0.40876(12) 0.3088(2) 0.9782(2) 0.0646(6) Uani 1.00 1 d . . . N(1) N 0.500000(10) 0.3958(6) 0.750000(10) 0.040(2) Uani 1.00 2 d S . . C(1) C 0.3624(3) 0.1602(6) 0.6220(8) 0.0464(19) Uani 1.00 1 d . . . C(2) C 0.3183(4) 0.2348(9) 0.6778(9) 0.060(2) Uani 1.00 1 d . . . C(3) C 0.3322(4) 0.3318(7) 0.6015(9) 0.053(2) Uani 1.00 1 d . . . C(4) C 0.3849(4) 0.3107(6) 0.4985(7) 0.0454(19) Uani 1.00 1 d . . . C(5) C 0.4027(4) 0.2050(5) 0.5111(7) 0.0411(18) Uani 1.00 1 d . . . C(6) C 0.3631(7) 0.0472(8) 0.6659(14) 0.107(4) Uani 1.00 1 d . . . C(7) C 0.2652(6) 0.2240(14) 0.7900(13) 0.119(5) Uani 1.00 1 d . . . C(8) C 0.2958(5) 0.4305(10) 0.6235(14) 0.105(4) Uani 1.00 1 d . . . C(9) C 0.4144(5) 0.3831(7) 0.3907(10) 0.067(2) Uani 1.00 1 d . . . C(10) C 0.4508(5) 0.1502(8) 0.4190(11) 0.078(3) Uani 1.00 1 d . . . H(1) H 0.4939 0.4377 0.8341 0.047 Uiso 1.00 1 c R . . H(2) H 0.5000 0.212(7) 0.7500 0.04(3) Uiso 1.00 2 d S . . H(3) H 0.3309 0.0361 0.7408 0.126 Uiso 1.00 1 c R . . H(4) H 0.3507 0.0059 0.5825 0.126 Uiso 1.00 1 c R . . H(5) H 0.4086 0.0296 0.7023 0.126 Uiso 1.00 1 c R . . H(6) H 0.2422 0.2873 0.8040 0.143 Uiso 1.00 1 c R . . H(7) H 0.2323 0.1737 0.7584 0.143 Uiso 1.00 1 c R . . H(8) H 0.2881 0.2034 0.8801 0.143 Uiso 1.00 1 c R . . H(9) H 0.3134 0.4796 0.5575 0.124 Uiso 1.00 1 c R . . H(10) H 0.2473 0.4213 0.6035 0.124 Uiso 1.00 1 c R . . H(11) H 0.3034 0.4536 0.7223 0.124 Uiso 1.00 1 c R . . H(12) H 0.4474 0.3489 0.3332 0.080 Uiso 1.00 1 c R . . H(13) H 0.3777 0.4086 0.3276 0.080 Uiso 1.00 1 c R . . H(14) H 0.4363 0.4385 0.4419 0.080 Uiso 1.00 1 c R . . H(15) H 0.4525 0.0803 0.4474 0.094 Uiso 1.00 1 c R . . H(16) H 0.4353 0.1550 0.3183 0.094 Uiso 1.00 1 c R . . H(17) H 0.4958 0.1795 0.4324 0.094 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ir(1) 0.02667(17) 0.04366(19) 0.02620(16) -0.00058(10) 0.00209(10) 0.00155(10) Cl(1) 0.0486(11) 0.1128(18) 0.0328(8) 0.0055(11) 0.0073(8) -0.0076(10) N(1) 0.036(4) 0.036(4) 0.047(4) 0.0000 -0.005(3) 0.0000 C(1) 0.044(4) 0.048(4) 0.047(3) -0.018(3) -0.010(3) 0.012(3) C(2) 0.032(3) 0.114(7) 0.035(3) -0.017(4) -0.003(3) -0.000(4) C(3) 0.039(3) 0.065(5) 0.054(4) 0.001(3) -0.013(3) -0.016(4) C(4) 0.054(4) 0.052(4) 0.029(3) -0.010(3) -0.009(3) 0.007(3) C(5) 0.041(3) 0.046(3) 0.035(3) -0.011(2) -0.010(2) -0.002(2) C(6) 0.121(10) 0.066(6) 0.129(10) -0.048(6) -0.054(8) 0.055(6) C(7) 0.051(6) 0.24(2) 0.068(7) -0.049(8) 0.003(5) -0.008(8) C(8) 0.073(7) 0.114(9) 0.124(10) 0.044(7) -0.049(6) -0.049(8) C(9) 0.070(6) 0.069(5) 0.060(5) -0.021(4) -0.014(4) 0.031(4) C(10) 0.083(7) 0.078(6) 0.073(6) -0.010(5) 0.012(5) -0.037(5) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR2002 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Ir(1) Ir(1) 2.856(1) yes . 2_656 Ir(1) Cl(1) 2.4097(19) yes . . Ir(1) N(1) 2.069(6) yes . . Ir(1) C(1) 2.175(7) yes . . Ir(1) C(2) 2.189(8) yes . . Ir(1) C(3) 2.173(7) yes . . Ir(1) C(4) 2.160(6) yes . . Ir(1) C(5) 2.169(7) yes . . C(1) C(2) 1.402(13) yes . . C(1) C(5) 1.422(10) yes . . C(1) C(6) 1.530(13) yes . . C(2) C(3) 1.475(14) yes . . C(2) C(7) 1.478(15) yes . . C(3) C(4) 1.435(11) yes . . C(3) C(8) 1.486(15) yes . . C(4) C(5) 1.427(11) yes . . C(4) C(9) 1.490(12) yes . . C(5) C(10) 1.460(13) yes . . Ir(1) H(2) 1.69(5) no . . N(1) H(1) 0.950 no . . N(1) H(1) 0.950 no . 2_656 C(6) H(3) 0.950 no . . C(6) H(4) 0.950 no . . C(6) H(5) 0.950 no . . C(7) H(6) 0.950 no . . C(7) H(7) 0.950 no . . C(7) H(8) 0.950 no . . C(8) H(9) 0.950 no . . C(8) H(10) 0.950 no . . C(8) H(11) 0.950 no . . C(9) H(12) 0.950 no . . C(9) H(13) 0.950 no . . C(9) H(14) 0.950 no . . C(10) H(15) 0.950 no . . C(10) H(16) 0.950 no . . C(10) H(17) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Ir(1) Ir(1) Cl(1) 89.63(5) yes 2_656 . . Ir(1) Ir(1) N(1) 46.34(15) yes 2_656 . . Ir(1) Ir(1) C(1) 128.3(2) yes 2_656 . . Ir(1) Ir(1) C(2) 163.8(3) yes 2_656 . . Ir(1) Ir(1) C(3) 153.5(2) yes 2_656 . . Ir(1) Ir(1) C(4) 120.3(2) yes 2_656 . . Ir(1) Ir(1) C(5) 109.8(2) yes 2_656 . . Cl(1) Ir(1) N(1) 83.55(6) yes . . . Cl(1) Ir(1) C(1) 113.7(2) yes . . . Cl(1) Ir(1) C(2) 92.0(2) yes . . . Cl(1) Ir(1) C(3) 106.4(2) yes . . . Cl(1) Ir(1) C(4) 144.4(2) yes . . . Cl(1) Ir(1) C(5) 151.9(2) yes . . . N(1) Ir(1) C(1) 162.7(2) yes . . . N(1) Ir(1) C(2) 149.8(3) yes . . . N(1) Ir(1) C(3) 113.5(2) yes . . . N(1) Ir(1) C(4) 102.7(2) yes . . . N(1) Ir(1) C(5) 124.6(2) yes . . . C(1) Ir(1) C(2) 37.5(3) yes . . . C(1) Ir(1) C(3) 64.6(3) yes . . . C(1) Ir(1) C(4) 64.5(2) yes . . . C(1) Ir(1) C(5) 38.2(2) yes . . . C(2) Ir(1) C(3) 39.5(3) yes . . . C(2) Ir(1) C(4) 64.9(3) yes . . . C(2) Ir(1) C(5) 63.7(3) yes . . . C(3) Ir(1) C(4) 38.7(3) yes . . . C(3) Ir(1) C(5) 64.5(3) yes . . . C(4) Ir(1) C(5) 38.5(2) yes . . . Ir(1) N(1) Ir(1) 87.3(3) yes . . 2_656 Ir(1) C(1) C(2) 71.8(5) yes . . . Ir(1) C(1) C(5) 70.7(4) yes . . . Ir(1) C(1) C(6) 126.8(6) yes . . . C(2) C(1) C(5) 109.0(7) yes . . . C(2) C(1) C(6) 125.3(8) yes . . . C(5) C(1) C(6) 125.6(7) yes . . . Ir(1) C(2) C(1) 70.7(4) yes . . . Ir(1) C(2) C(3) 69.7(4) yes . . . Ir(1) C(2) C(7) 126.1(6) yes . . . C(1) C(2) C(3) 107.8(7) yes . . . C(1) C(2) C(7) 128.9(11) yes . . . C(3) C(2) C(7) 123.3(10) yes . . . Ir(1) C(3) C(2) 70.8(4) yes . . . Ir(1) C(3) C(4) 70.2(4) yes . . . Ir(1) C(3) C(8) 126.0(6) yes . . . C(2) C(3) C(4) 106.6(7) yes . . . C(2) C(3) C(8) 126.0(8) yes . . . C(4) C(3) C(8) 127.3(8) yes . . . Ir(1) C(4) C(3) 71.1(4) yes . . . Ir(1) C(4) C(5) 71.1(4) yes . . . Ir(1) C(4) C(9) 125.8(5) yes . . . C(3) C(4) C(5) 108.0(6) yes . . . C(3) C(4) C(9) 127.1(7) yes . . . C(5) C(4) C(9) 124.8(7) yes . . . Ir(1) C(5) C(1) 71.1(4) yes . . . Ir(1) C(5) C(4) 70.4(3) yes . . . Ir(1) C(5) C(10) 127.4(6) yes . . . C(1) C(5) C(4) 108.6(6) yes . . . C(1) C(5) C(10) 125.5(7) yes . . . C(4) C(5) C(10) 125.8(7) yes . . . Ir(1) Ir(1) H(2) 32(2) no 2_656 . . Cl(1) Ir(1) H(2) 94.3(3) no . . . N(1) Ir(1) H(2) 79(2) no . . . C(1) Ir(1) H(2) 98(2) no . . . C(2) Ir(1) H(2) 131(2) no . . . C(3) Ir(1) H(2) 156.7(15) no . . . C(4) Ir(1) H(2) 121.4(4) no . . . C(5) Ir(1) H(2) 92.2(16) no . . . Ir(1) N(1) H(1) 114.7 no . . . Ir(1) N(1) H(1) 114.7 no . . 2_656 Ir(1) N(1) H(1) 114.7 no 2_656 . . Ir(1) N(1) H(1) 114.7 no 2_656 . 2_656 H(1) N(1) H(1) 109.5 no . . 2_656 C(1) C(6) H(3) 109.5 no . . . C(1) C(6) H(4) 110.0 no . . . C(1) C(6) H(5) 108.8 no . . . H(3) C(6) H(4) 109.4 no . . . H(3) C(6) H(5) 109.5 no . . . H(4) C(6) H(5) 109.6 no . . . C(2) C(7) H(6) 110.4 no . . . C(2) C(7) H(7) 109.4 no . . . C(2) C(7) H(8) 108.1 no . . . H(6) C(7) H(7) 109.5 no . . . H(6) C(7) H(8) 109.5 no . . . H(7) C(7) H(8) 110.0 no . . . C(3) C(8) H(9) 108.6 no . . . C(3) C(8) H(10) 109.1 no . . . C(3) C(8) H(11) 110.3 no . . . H(9) C(8) H(10) 110.0 no . . . H(9) C(8) H(11) 109.5 no . . . H(10) C(8) H(11) 109.3 no . . . C(4) C(9) H(12) 110.0 no . . . C(4) C(9) H(13) 108.9 no . . . C(4) C(9) H(14) 109.8 no . . . H(12) C(9) H(13) 109.5 no . . . H(12) C(9) H(14) 109.5 no . . . H(13) C(9) H(14) 109.2 no . . . C(5) C(10) H(15) 109.5 no . . . C(5) C(10) H(16) 109.6 no . . . C(5) C(10) H(17) 109.0 no . . . H(15) C(10) H(16) 109.3 no . . . H(15) C(10) H(17) 109.5 no . . . H(16) C(10) H(17) 110.0 no . . . Ir(1) H(2) Ir(1) 115(5) no . . 2_656 #===END