# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1052c #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C35 H50 B3 Cl F4 N16 O4 Ru2' _chemical_formula_moiety 'C35 H50 B3 Cl F4 N16 O4 Ru2' _chemical_formula_weight 1104.90 _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 11.597(5) _cell_length_b 11.793(5) _cell_length_c 17.685(6) _cell_angle_alpha 77.253(16) _cell_angle_beta 75.450(17) _cell_angle_gamma 84.730(16) _cell_volume 2281.8(16) _cell_formula_units_Z 2 _cell_measurement_reflns_used 6381 _cell_measurement_theta_min 3.10 _cell_measurement_theta_max 27.48 _cell_measurement_temperature 93 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour darkGreen _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.050 _exptl_crystal_density_diffrn 1.608 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120.00 _exptl_absorpt_coefficient_mu 0.794 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_correction_T_min 0.798 _exptl_absorpt_correction_T_max 0.961 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 93 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku Saturn724+' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.111 _diffrn_reflns_number 18577 _diffrn_reflns_av_R_equivalents 0.0545 _diffrn_reflns_theta_max 27.42 _diffrn_reflns_theta_full 27.42 _diffrn_measured_fraction_theta_max 0.978 _diffrn_measured_fraction_theta_full 0.978 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # 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 10180 _reflns_number_gt 6595 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0980 _refine_ls_wR_factor_ref 0.2782 _refine_ls_number_restraints 84 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 10180 _refine_ls_number_parameters 494 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.1319P)^2^+10.7511P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.001 _refine_diff_density_max 2.280 _refine_diff_density_min -1.400 _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 0.0033 0.0016 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; B B 0.0013 0.0007 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.1484 0.1585 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; F F 0.0171 0.0103 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.0061 0.0033 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.0106 0.0060 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ru Ru -1.2594 0.8363 ; 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 Ru1 Ru 1.01398(6) 0.53501(7) 0.22996(5) 0.0316(3) Uani 1.0 2 d . . . Ru2 Ru 0.79704(6) 0.32342(6) 0.22626(4) 0.0299(3) Uani 1.0 2 d . . . Cl1 Cl 0.99503(18) 0.38963(19) 0.15990(13) 0.0308(5) Uani 1.0 2 d . . . F1 F 1.0471(5) 1.0398(6) 0.3790(4) 0.076(3) Uiso 1.0 2 d . . . F2A F 1.2466(6) 1.0132(7) 0.3308(8) 0.061(4) Uiso 0.5000 2 d . . . F2B F 1.2464(6) 1.0110(7) 0.3654(8) 0.049(4) Uiso 0.5000 2 d . . . F3A F 1.1511(9) 1.1834(9) 0.2875(6) 0.074(5) Uiso 0.5000 2 d . . . F3B F 1.1751(10) 1.1404(12) 0.2711(5) 0.117(8) Uiso 0.5000 2 d . . . F4A F 1.1769(10) 1.1392(12) 0.4137(6) 0.103(7) Uiso 0.5000 2 d . . . F4B F 1.1564(9) 1.1812(10) 0.3933(9) 0.132(9) Uiso 0.5000 2 d . . . O1 O 1.0218(8) 0.3798(9) 0.3835(5) 0.066(3) Uani 1.0 2 d . . . O2 O 0.8045(12) 0.4749(12) 0.4687(8) 0.113(4) Uiso 1.0 2 d . . . O3 O 1.3169(13) 1.0366(13) 0.0147(9) 0.129(5) Uiso 1.0 2 d . . . O4 O 0.316(3) 0.186(3) 0.5647(16) 0.244(11) Uiso 1.0 2 d . . . N1 N 1.0053(7) 0.4347(8) 0.3248(5) 0.0369(18) Uani 1.0 2 d . . . N2 N 0.8335(8) 0.2642(8) 0.3340(6) 0.046(3) Uani 1.0 2 d . . . N3 N 1.0292(7) 0.6688(7) 0.2840(5) 0.0359(18) Uani 1.0 2 d . . . N4 N 1.1199(8) 0.7438(8) 0.2527(6) 0.044(3) Uani 1.0 2 d . . . N5 N 1.0433(7) 0.6612(7) 0.1254(5) 0.0342(18) Uani 1.0 2 d . . . N6 N 1.1280(7) 0.7407(7) 0.1109(5) 0.0383(19) Uani 1.0 2 d . . . N7 N 1.1985(7) 0.5134(6) 0.2060(4) 0.0268(15) Uani 1.0 2 d . . . N8 N 1.2663(7) 0.6085(7) 0.1817(5) 0.0359(18) Uani 1.0 2 d . . . N9 N 0.6270(7) 0.2710(7) 0.2782(5) 0.0345(18) Uani 1.0 2 d . . . N10 N 0.5753(8) 0.2031(7) 0.2421(5) 0.043(2) Uani 1.0 2 d . . . N11 N 0.7427(6) 0.3694(6) 0.1209(4) 0.0253(15) Uani 1.0 2 d . . . N12 N 0.6753(7) 0.2941(7) 0.1024(5) 0.0326(17) Uani 1.0 2 d . . . N13 N 0.8383(7) 0.1594(6) 0.2014(5) 0.0266(15) Uani 1.0 2 d . . . N14 N 0.7631(7) 0.1111(7) 0.1710(5) 0.0358(18) Uani 1.0 2 d . . . N15 N 0.8351(7) 0.5698(7) 0.2424(5) 0.0306(16) Uani 1.0 2 d . . . N16 N 0.7531(7) 0.4925(7) 0.2442(4) 0.0283(16) Uani 1.0 2 d . . . C1 C 0.8375(9) 0.2170(10) 0.3961(7) 0.041(3) Uani 1.0 2 d . . . C2 C 0.8433(18) 0.1594(18) 0.4788(11) 0.112(7) Uani 1.0 2 d . . . C3 C 0.9645(10) 0.6993(11) 0.3524(7) 0.049(3) Uani 1.0 2 d . . . C4 C 1.0152(11) 0.7952(11) 0.3624(8) 0.055(4) Uani 1.0 2 d . . . C5 C 1.1102(11) 0.8191(10) 0.3022(8) 0.054(4) Uani 1.0 2 d . . . C6 C 0.9955(9) 0.6859(10) 0.0624(7) 0.045(3) Uani 1.0 2 d . . . C7 C 1.0457(10) 0.7847(10) 0.0085(7) 0.046(3) Uani 1.0 2 d . . . C8 C 1.1282(9) 0.8148(9) 0.0424(6) 0.040(3) Uani 1.0 2 d . . . C9 C 1.2730(8) 0.4195(8) 0.2087(5) 0.0280(18) Uani 1.0 2 d . . . C10 C 1.3896(8) 0.4546(8) 0.1865(6) 0.034(2) Uani 1.0 2 d . . . C11 C 1.3823(8) 0.5734(8) 0.1698(6) 0.034(2) Uani 1.0 2 d . . . C12 C 0.5476(10) 0.2823(11) 0.3452(7) 0.053(3) Uani 1.0 2 d . . . C13 C 0.4448(9) 0.2262(10) 0.3526(7) 0.053(3) Uani 1.0 2 d . . . C14 C 0.4651(9) 0.1785(9) 0.2864(7) 0.044(3) Uani 1.0 2 d . . . C15 C 0.7491(9) 0.4648(8) 0.0633(6) 0.034(2) Uani 1.0 2 d . . . C16 C 0.6886(9) 0.4539(9) 0.0077(6) 0.038(3) Uani 1.0 2 d . . . C17 C 0.6416(9) 0.3420(8) 0.0352(6) 0.038(3) Uani 1.0 2 d . . . C18 C 0.9287(8) 0.0807(8) 0.2075(6) 0.036(2) Uani 1.0 2 d . . . C19 C 0.9151(9) -0.0151(9) 0.1798(7) 0.042(3) Uani 1.0 2 d . . . C20 C 0.8074(10) 0.0035(8) 0.1587(7) 0.044(3) Uani 1.0 2 d . . . C21 C 0.7774(9) 0.6740(9) 0.2448(6) 0.038(3) Uani 1.0 2 d . . . C22 C 0.6560(9) 0.6661(9) 0.2485(6) 0.039(3) Uani 1.0 2 d . . . C23 C 0.6463(9) 0.5482(9) 0.2477(6) 0.037(3) Uani 1.0 2 d . . . C24 C 0.6813(14) 0.4721(15) 0.4734(10) 0.087(5) Uiso 1.0 2 d . . . C25 C 0.62(4) 0.49(4) 0.55(3) 0.13(15) Uiso 1.0 2 d . . . C26 C 0.7104(16) 0.4502(17) 0.6037(11) 0.100(6) Uiso 1.0 2 d . . . C27 C 0.8163(19) 0.503(2) 0.5402(12) 0.131(8) Uiso 1.0 2 d . . . C28 C 1.4042(15) 1.1132(15) -0.0388(11) 0.106(6) Uiso 1.0 2 d . . . C29 C 1.356(2) 1.2327(17) -0.0203(11) 0.145(9) Uiso 1.0 2 d . . . C30 C 1.2945(17) 1.2050(15) 0.0692(10) 0.099(6) Uiso 1.0 2 d . . . C31 C 1.2672(18) 1.0751(14) 0.0878(10) 0.113(7) Uiso 1.0 2 d . . . C32 C 0.435(3) 0.188(3) 0.572(2) 0.188(13) Uiso 1.0 2 d . . . C33 C 0.404(4) 0.089(4) 0.646(2) 0.249(18) Uiso 1.0 2 d . . . C34 C 0.365(4) 0.011(4) 0.597(3) 0.228(16) Uiso 1.0 2 d . . . C35 C 0.266(4) 0.081(3) 0.560(3) 0.251(19) Uiso 1.0 2 d . . . B1 B 1.2060(10) 0.7326(10) 0.1719(8) 0.037(3) Uani 1.0 2 d . . . B2 B 0.6451(9) 0.1761(9) 0.1607(7) 0.034(3) Uani 1.0 2 d . . . B3 B 1.1559(5) 1.0935(5) 0.3524(4) 0.057(4) Uiso 1.0 2 d . . . H1 H 1.2665 0.7942 0.1538 0.0444 Uiso 1.0 2 calc R . . H2 H 0.5969 0.1292 0.1401 0.0403 Uiso 1.0 2 calc R . . H3 H 0.7704 0.1794 0.5164 0.1341 Uiso 1.0 2 calc R . . H4 H 0.9126 0.1859 0.4914 0.1341 Uiso 1.0 2 calc R . . H5 H 0.8507 0.0748 0.4833 0.1341 Uiso 1.0 2 calc R . . H6 H 0.8962 0.6615 0.3872 0.0586 Uiso 1.0 2 calc R . . H7 H 0.9872 0.8362 0.4045 0.0659 Uiso 1.0 2 calc R . . H8 H 1.1632 0.8795 0.2949 0.0651 Uiso 1.0 2 calc R . . H9 H 0.9356 0.6425 0.0550 0.0542 Uiso 1.0 2 calc R . . H10 H 1.0265 0.8220 -0.0404 0.0558 Uiso 1.0 2 calc R . . H11 H 1.1784 0.8791 0.0204 0.0474 Uiso 1.0 2 calc R . . H12 H 1.2494 0.3410 0.2236 0.0336 Uiso 1.0 2 calc R . . H13 H 1.4600 0.4061 0.1835 0.0405 Uiso 1.0 2 calc R . . H14 H 1.4480 0.6231 0.1527 0.0403 Uiso 1.0 2 calc R . . H15 H 0.5600 0.3234 0.3828 0.0638 Uiso 1.0 2 calc R . . H16 H 0.3748 0.2217 0.3947 0.0632 Uiso 1.0 2 calc R . . H17 H 0.4100 0.1350 0.2739 0.0533 Uiso 1.0 2 calc R . . H18 H 0.7903 0.5319 0.0609 0.0410 Uiso 1.0 2 calc R . . H19 H 0.6804 0.5092 -0.0388 0.0460 Uiso 1.0 2 calc R . . H20 H 0.5944 0.3070 0.0104 0.0453 Uiso 1.0 2 calc R . . H21 H 0.9940 0.0905 0.2285 0.0426 Uiso 1.0 2 calc R . . H22 H 0.9685 -0.0807 0.1759 0.0509 Uiso 1.0 2 calc R . . H23 H 0.7705 -0.0490 0.1392 0.0528 Uiso 1.0 2 calc R . . H24 H 0.8138 0.7433 0.2441 0.0451 Uiso 1.0 2 calc R . . H25 H 0.5951 0.7257 0.2509 0.0470 Uiso 1.0 2 calc R . . H26 H 0.5748 0.5133 0.2493 0.0440 Uiso 1.0 2 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru1 0.0266(4) 0.0336(5) 0.0385(5) 0.0038(3) -0.0142(3) -0.0099(3) Ru2 0.0315(4) 0.0273(4) 0.0297(4) 0.0038(3) -0.0111(3) -0.0011(3) Cl1 0.0274(11) 0.0302(11) 0.0360(12) 0.0010(9) -0.0110(9) -0.0062(9) O1 0.068(6) 0.078(7) 0.052(6) 0.008(5) -0.026(5) -0.004(5) N1 0.037(5) 0.038(5) 0.041(5) 0.007(4) -0.018(4) -0.012(4) N2 0.046(6) 0.050(6) 0.042(5) 0.018(5) -0.017(4) -0.009(4) N3 0.034(5) 0.033(5) 0.046(5) 0.005(4) -0.017(4) -0.012(4) N4 0.057(6) 0.034(5) 0.060(6) 0.009(4) -0.042(5) -0.018(4) N5 0.026(4) 0.032(4) 0.050(5) 0.002(4) -0.021(4) -0.009(4) N6 0.038(5) 0.025(4) 0.055(6) -0.001(4) -0.022(4) -0.003(4) N7 0.032(4) 0.022(4) 0.029(4) 0.001(3) -0.015(3) -0.001(3) N8 0.035(5) 0.026(4) 0.051(5) 0.003(4) -0.020(4) -0.006(4) N9 0.025(4) 0.041(5) 0.030(4) 0.003(4) -0.000(3) -0.001(4) N10 0.048(6) 0.026(5) 0.048(5) -0.004(4) -0.016(4) 0.010(4) N11 0.029(4) 0.022(4) 0.024(4) 0.002(3) -0.009(3) -0.001(3) N12 0.027(4) 0.036(5) 0.039(5) -0.001(4) -0.015(4) -0.008(4) N13 0.030(4) 0.015(4) 0.035(4) 0.006(3) -0.014(3) -0.001(3) N14 0.033(5) 0.031(5) 0.043(5) -0.000(4) -0.014(4) -0.002(4) N15 0.028(4) 0.029(4) 0.036(5) 0.007(3) -0.011(3) -0.008(4) N16 0.028(4) 0.031(4) 0.027(4) 0.003(3) -0.011(3) -0.005(3) C1 0.041(6) 0.044(6) 0.039(6) 0.003(5) -0.018(5) -0.002(5) C2 0.109(15) 0.127(17) 0.097(14) -0.006(13) -0.053(11) 0.015(12) C3 0.049(7) 0.061(8) 0.043(6) 0.016(6) -0.019(5) -0.023(6) C4 0.055(8) 0.058(8) 0.071(8) 0.021(6) -0.032(7) -0.042(7) C5 0.056(8) 0.040(6) 0.089(10) 0.016(6) -0.052(7) -0.029(6) C6 0.036(6) 0.043(6) 0.059(7) -0.011(5) -0.019(5) -0.003(5) C7 0.050(7) 0.050(7) 0.036(6) -0.007(5) -0.015(5) 0.007(5) C8 0.033(6) 0.034(6) 0.051(7) -0.001(4) -0.012(5) -0.005(5) C9 0.035(5) 0.024(5) 0.026(5) 0.004(4) -0.014(4) -0.001(4) C10 0.026(5) 0.033(5) 0.041(6) 0.007(4) -0.011(4) -0.003(4) C11 0.026(5) 0.032(5) 0.047(6) -0.003(4) -0.019(4) -0.004(4) C12 0.044(7) 0.054(7) 0.043(7) 0.013(6) -0.001(5) 0.011(5) C13 0.030(6) 0.050(7) 0.053(7) -0.004(5) 0.010(5) 0.018(6) C14 0.033(6) 0.038(6) 0.049(7) -0.001(5) -0.001(5) 0.009(5) C15 0.039(6) 0.022(5) 0.043(6) -0.002(4) -0.020(4) 0.002(4) C16 0.052(6) 0.032(5) 0.035(6) 0.003(5) -0.023(5) -0.003(4) C17 0.041(6) 0.028(5) 0.048(6) 0.009(4) -0.022(5) -0.007(4) C18 0.031(5) 0.030(5) 0.044(6) 0.003(4) -0.016(4) 0.001(4) C19 0.038(6) 0.023(5) 0.066(7) 0.005(4) -0.018(5) -0.005(5) C20 0.049(6) 0.013(4) 0.075(8) -0.004(4) -0.028(6) -0.004(5) C21 0.035(6) 0.035(5) 0.045(6) 0.003(4) -0.019(5) -0.003(5) C22 0.038(6) 0.037(6) 0.044(6) 0.015(5) -0.014(5) -0.011(5) C23 0.029(5) 0.039(6) 0.052(6) 0.008(4) -0.025(5) -0.017(5) B1 0.033(6) 0.028(6) 0.058(8) -0.001(5) -0.026(5) -0.009(5) B2 0.027(6) 0.026(5) 0.043(7) -0.003(4) -0.012(5) 0.007(5) #============================================================================== _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'DIRDIF99-PATTY (Gould, et al., 1999)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # 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 Ru1 Cl1 2.380(3) yes . . Ru1 N1 1.813(8) yes . . Ru1 N3 2.058(10) yes . . Ru1 N5 2.076(8) yes . . Ru1 N7 2.077(7) yes . . Ru1 N15 2.043(8) yes . . Ru2 Cl1 2.415(3) yes . . Ru2 N2 2.015(10) yes . . Ru2 N9 2.044(8) yes . . Ru2 N11 2.060(8) yes . . Ru2 N13 2.064(7) yes . . Ru2 N16 2.085(8) yes . . F1 B3 1.390(8) yes . . F2A B3 1.388(10) yes . . F2B B3 1.392(9) yes . . F3A B3 1.389(11) yes . . F3B B3 1.392(10) yes . . F4A B3 1.392(15) yes . . F4B B3 1.388(16) yes . . O1 N1 1.145(12) yes . . O2 C24 1.41(2) yes . . O2 C27 1.42(3) yes . . O3 C28 1.43(2) yes . . O3 C31 1.43(3) yes . . O4 C32 1.43(5) yes . . O4 C35 1.43(5) yes . . N2 C1 1.126(14) yes . . N3 N4 1.362(12) yes . . N3 C3 1.357(14) yes . . N4 C5 1.357(18) yes . . N4 B1 1.550(15) yes . . N5 N6 1.358(12) yes . . N5 C6 1.331(15) yes . . N6 C8 1.328(13) yes . . N6 B1 1.556(17) yes . . N7 N8 1.357(11) yes . . N7 C9 1.340(11) yes . . N8 C11 1.349(12) yes . . N8 B1 1.556(13) yes . . N9 N10 1.383(14) yes . . N9 C12 1.330(13) yes . . N10 C14 1.340(13) yes . . N10 B2 1.548(14) yes . . N11 N12 1.374(12) yes . . N11 C15 1.335(11) yes . . N12 C17 1.335(14) yes . . N12 B2 1.548(12) yes . . N13 N14 1.355(13) yes . . N13 C18 1.344(12) yes . . N14 C20 1.366(13) yes . . N14 B2 1.537(13) yes . . N15 N16 1.367(12) yes . . N15 C21 1.348(13) yes . . N16 C23 1.341(12) yes . . C1 C2 1.49(2) yes . . C3 C4 1.39(2) yes . . C4 C5 1.328(16) yes . . C6 C7 1.400(14) yes . . C7 C8 1.358(18) yes . . C9 C10 1.385(13) yes . . C10 C11 1.366(13) yes . . C12 C13 1.380(17) yes . . C13 C14 1.367(18) yes . . C15 C16 1.376(17) yes . . C16 C17 1.411(14) yes . . C18 C19 1.362(16) yes . . C19 C20 1.376(17) yes . . C21 C22 1.403(15) yes . . C22 C23 1.409(15) yes . . C24 C25 1.4(5) yes . . C25 C26 1.6(5) yes . . C26 C27 1.51(3) yes . . C28 C29 1.54(3) yes . . C29 C30 1.54(3) yes . . C30 C31 1.54(3) yes . . C32 C33 1.54(5) yes . . C33 C34 1.54(7) yes . . C34 C35 1.54(6) yes . . 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 Cl1 Ru1 N1 94.8(4) yes . . . Cl1 Ru1 N3 176.3(3) yes . . . Cl1 Ru1 N5 91.5(3) yes . . . Cl1 Ru1 N7 92.9(3) yes . . . Cl1 Ru1 N15 87.2(3) yes . . . N1 Ru1 N3 88.9(4) yes . . . N1 Ru1 N5 171.6(4) yes . . . N1 Ru1 N7 88.9(3) yes . . . N1 Ru1 N15 97.3(4) yes . . . N3 Ru1 N5 84.8(4) yes . . . N3 Ru1 N7 87.7(3) yes . . . N3 Ru1 N15 91.8(4) yes . . . N5 Ru1 N7 85.3(3) yes . . . N5 Ru1 N15 88.4(3) yes . . . N7 Ru1 N15 173.8(3) yes . . . Cl1 Ru2 N2 95.2(3) yes . . . Cl1 Ru2 N9 177.5(3) yes . . . Cl1 Ru2 N11 91.4(2) yes . . . Cl1 Ru2 N13 92.7(2) yes . . . Cl1 Ru2 N16 86.9(2) yes . . . N2 Ru2 N9 87.2(4) yes . . . N2 Ru2 N11 172.8(4) yes . . . N2 Ru2 N13 89.3(4) yes . . . N2 Ru2 N16 94.3(4) yes . . . N9 Ru2 N11 86.2(3) yes . . . N9 Ru2 N13 87.7(3) yes . . . N9 Ru2 N16 92.5(3) yes . . . N11 Ru2 N13 87.4(3) yes . . . N11 Ru2 N16 89.0(3) yes . . . N13 Ru2 N16 176.4(3) yes . . . Ru1 Cl1 Ru2 101.91(9) yes . . . C24 O2 C27 107.4(14) yes . . . C28 O3 C31 112.2(16) yes . . . C32 O4 C35 122(3) yes . . . Ru1 N1 O1 166.1(9) yes . . . Ru2 N2 C1 166.9(10) yes . . . Ru1 N3 N4 120.9(7) yes . . . Ru1 N3 C3 131.7(8) yes . . . N4 N3 C3 107.4(10) yes . . . N3 N4 C5 107.9(9) yes . . . N3 N4 B1 118.7(9) yes . . . C5 N4 B1 133.3(9) yes . . . Ru1 N5 N6 120.3(7) yes . . . Ru1 N5 C6 133.9(7) yes . . . N6 N5 C6 105.8(8) yes . . . N5 N6 C8 109.9(10) yes . . . N5 N6 B1 119.1(8) yes . . . C8 N6 B1 131.0(9) yes . . . Ru1 N7 N8 119.4(6) yes . . . Ru1 N7 C9 133.3(6) yes . . . N8 N7 C9 107.3(7) yes . . . N7 N8 C11 108.9(7) yes . . . N7 N8 B1 120.1(8) yes . . . C11 N8 B1 130.9(8) yes . . . Ru2 N9 N10 119.1(6) yes . . . Ru2 N9 C12 134.8(9) yes . . . N10 N9 C12 106.1(9) yes . . . N9 N10 C14 108.8(9) yes . . . N9 N10 B2 118.8(8) yes . . . C14 N10 B2 132.3(11) yes . . . Ru2 N11 N12 119.1(5) yes . . . Ru2 N11 C15 135.0(8) yes . . . N12 N11 C15 105.7(8) yes . . . N11 N12 C17 110.5(8) yes . . . N11 N12 B2 118.8(8) yes . . . C17 N12 B2 130.6(10) yes . . . Ru2 N13 N14 119.2(6) yes . . . Ru2 N13 C18 135.1(8) yes . . . N14 N13 C18 105.6(8) yes . . . N13 N14 C20 109.7(8) yes . . . N13 N14 B2 119.3(8) yes . . . C20 N14 B2 130.9(10) yes . . . Ru1 N15 N16 125.8(6) yes . . . Ru1 N15 C21 126.7(7) yes . . . N16 N15 C21 107.4(8) yes . . . Ru2 N16 N15 123.8(6) yes . . . Ru2 N16 C23 126.7(7) yes . . . N15 N16 C23 108.9(8) yes . . . N2 C1 C2 177.6(15) yes . . . N3 C3 C4 108.0(10) yes . . . C3 C4 C5 107.2(12) yes . . . N4 C5 C4 109.5(12) yes . . . N5 C6 C7 110.6(11) yes . . . C6 C7 C8 104.0(10) yes . . . N6 C8 C7 109.6(9) yes . . . N7 C9 C10 109.4(8) yes . . . C9 C10 C11 105.7(8) yes . . . N8 C11 C10 108.6(8) yes . . . N9 C12 C13 110.8(12) yes . . . C12 C13 C14 105.3(10) yes . . . N10 C14 C13 109.0(11) yes . . . N11 C15 C16 111.7(9) yes . . . C15 C16 C17 104.5(9) yes . . . N12 C17 C16 107.6(10) yes . . . N13 C18 C19 111.7(10) yes . . . C18 C19 C20 105.4(9) yes . . . N14 C20 C19 107.6(10) yes . . . N15 C21 C22 110.6(10) yes . . . C21 C22 C23 103.2(9) yes . . . N16 C23 C22 109.9(9) yes . . . O2 C24 C25 106(20) yes . . . C24 C25 C26 106(25) yes . . . C25 C26 C27 92(14) yes . . . O2 C27 C26 105.1(19) yes . . . O3 C28 C29 102.4(14) yes . . . C28 C29 C30 103.9(14) yes . . . C29 C30 C31 105.0(15) yes . . . O3 C31 C30 105.1(13) yes . . . O4 C32 C33 87(3) yes . . . C32 C33 C34 92(3) yes . . . C33 C34 C35 107(4) yes . . . O4 C35 C34 89(3) yes . . . N4 B1 N6 106.9(8) yes . . . N4 B1 N8 108.1(8) yes . . . N6 B1 N8 107.0(10) yes . . . N10 B2 N12 107.3(8) yes . . . N10 B2 N14 108.8(9) yes . . . N12 B2 N14 108.0(7) yes . . . F1 B3 F2A 109.9(6) yes . . . F1 B3 F2B 109.0(6) yes . . . F1 B3 F3A 109.1(7) yes . . . F1 B3 F3B 109.4(8) yes . . . F1 B3 F4A 108.9(7) yes . . . F1 B3 F4B 110.2(7) yes . . . F2A B3 F3A 110.1(7) yes . . . F2A B3 F4A 109.6(8) yes . . . F2B B3 F3B 109.0(8) yes . . . F2B B3 F4B 109.6(9) yes . . . F3A B3 F4A 109.2(8) yes . . . F3B B3 F4B 109.6(9) yes . . . #============================================================================== #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== _database_code_depnum_ccdc_archive 'CCDC 939832' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1013a #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C23 H29.67 B2 Cl1.67 N15 O2.33 Ru2' _chemical_formula_moiety 'C23 H29.67 B2 Cl1.67 N15 O2.33 Ru2' _chemical_formula_weight 836.50 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'P 63/m' _symmetry_space_group_name_Hall '-P 6c' _symmetry_Int_Tables_number 176 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 +X-Y,+X,1/2+Z 3 -Y,+X-Y,+Z 4 -X,-Y,1/2+Z 5 -X+Y,-X,+Z 6 +Y,-X+Y,1/2+Z 7 -X,-Y,-Z 8 -X+Y,-X,1/2-Z 9 +Y,-X+Y,-Z 10 +X,+Y,1/2-Z 11 +X-Y,+X,-Z 12 -Y,+X-Y,1/2-Z #------------------------------------------------------------------------------ _cell_length_a 19.3345(5) _cell_length_b 19.3345(5) _cell_length_c 14.6049(4) _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 120.0000 _cell_volume 4728.2(3) _cell_formula_units_Z 6 _cell_measurement_reflns_used 16401 _cell_measurement_theta_min 3.04 _cell_measurement_theta_max 27.49 _cell_measurement_temperature 93 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour darkbrown _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.050 _exptl_crystal_density_diffrn 1.763 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2506.20 _exptl_absorpt_coefficient_mu 1.152 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_correction_T_min 0.837 _exptl_absorpt_correction_T_max 0.944 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 93 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku Saturn724' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.111 _diffrn_reflns_number 30479 _diffrn_reflns_av_R_equivalents 0.0197 _diffrn_reflns_theta_max 27.47 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 11 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # 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 3746 _reflns_number_gt 3504 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0255 _refine_ls_wR_factor_ref 0.0720 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 3746 _refine_ls_number_parameters 228 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0393P)^2^+8.1168P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.001 _refine_diff_density_max 1.470 _refine_diff_density_min -0.680 _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 0.0033 0.0016 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.0061 0.0033 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; B B 0.0013 0.0007 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.1484 0.1585 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.0106 0.0060 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ru Ru -1.2594 0.8363 ; 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 Ru1 Ru 0.324707(9) 0.361296(9) 0.150542(10) 0.00809(7) Uani 1.0 12 d . . . Cl1 Cl 0.31283(4) 0.25294(4) 0.2500 0.01201(14) Uani 1.0 6 d . . . Cl2 Cl -0.03576(8) 0.06214(8) 0.2500 0.0320(3) Uani 0.6700 6 d . . . O1 O 0.24254(14) 0.42869(14) 0.2500 0.0185(5) Uani 1.0 6 d . . . O2 O 0.23353(17) 0.48224(17) -0.2500 0.0345(7) Uani 1.0 6 d . . . O3 O 0.2550(5) 0.5867(5) 0.2500 0.0276(17) Uani 0.3300 6 d . . . N1 N 0.28148(14) 0.39548(15) 0.2500 0.0115(5) Uani 1.0 6 d . . . N2 N 0.33859(10) 0.45425(10) 0.07169(12) 0.0115(4) Uani 1.0 12 d . . . N3 N 0.31523(10) 0.44218(10) -0.01785(12) 0.0122(4) Uani 1.0 12 d . . . N4 N 0.37069(10) 0.33016(10) 0.03706(12) 0.0110(4) Uani 1.0 12 d . . . N5 N 0.34234(10) 0.33092(10) -0.04840(12) 0.0124(4) Uani 1.0 12 d . . . N6 N 0.21336(10) 0.29000(10) 0.08837(12) 0.0115(4) Uani 1.0 12 d . . . N7 N 0.20571(10) 0.30095(10) -0.00285(12) 0.0122(4) Uani 1.0 12 d . . . N8 N 0.43645(10) 0.43170(10) 0.20363(11) 0.0107(4) Uani 1.0 12 d . . . C1 C 0.37044(12) 0.53234(12) 0.08883(15) 0.0143(4) Uani 1.0 12 d . . . C2 C 0.36711(13) 0.57142(12) 0.00984(16) 0.0160(4) Uani 1.0 12 d . . . C3 C 0.33203(12) 0.51223(13) -0.05618(15) 0.0145(4) Uani 1.0 12 d . . . C4 C 0.42239(12) 0.30355(12) 0.02763(14) 0.0133(4) Uani 1.0 12 d . . . C5 C 0.42731(13) 0.28603(13) -0.06459(15) 0.0164(5) Uani 1.0 12 d . . . C6 C 0.37588(13) 0.30417(13) -0.10940(15) 0.0161(4) Uani 1.0 12 d . . . C7 C 0.14113(13) 0.23409(13) 0.11682(15) 0.0173(5) Uani 1.0 12 d . . . C8 C 0.08603(13) 0.20872(14) 0.04526(16) 0.0189(5) Uani 1.0 12 d . . . C9 C 0.12939(12) 0.25270(12) -0.02946(15) 0.0153(4) Uani 1.0 12 d . . . C10 C 0.51056(12) 0.48403(12) 0.17402(15) 0.0146(4) Uani 1.0 12 d . . . C11 C 0.55988(18) 0.51840(19) 0.2500 0.0169(6) Uani 1.0 6 d . . . C12 C 0.0000 0.0000 0.2094(8) 0.042(3) Uani 0.5000 4 d . . . C13 C 0.0000 0.0000 0.109(3) 0.157(14) Uani 0.5000 4 d . . . C14 C 0.2233(3) 0.5520(3) -0.2500 0.0442(13) Uani 1.0 6 d . . . C15 C 0.3333 0.6667 0.2500 0.048(2) Uani 1.0000 2 d . . . B1 B 0.27973(14) 0.35763(13) -0.05986(16) 0.0132(5) Uani 1.0 12 d . . . H1 H 0.2656 0.3574 -0.1258 0.0159 Uiso 1.0 12 calc R . . H2 H 0.3920 0.5574 0.1460 0.0172 Uiso 1.0 12 calc R . . H3 H 0.3851 0.6267 0.0029 0.0192 Uiso 1.0 12 calc R . . H4 H 0.3216 0.5198 -0.1179 0.0174 Uiso 1.0 12 calc R . . H5 H 0.4515 0.2974 0.0763 0.0159 Uiso 1.0 12 calc R . . H6 H 0.4591 0.2661 -0.0903 0.0197 Uiso 1.0 12 calc R . . H7 H 0.3656 0.2987 -0.1734 0.0194 Uiso 1.0 12 calc R . . H8 H 0.1289 0.2142 0.1777 0.0208 Uiso 1.0 12 calc R . . H9 H 0.0309 0.1698 0.0475 0.0227 Uiso 1.0 12 calc R . . H10 H 0.1090 0.2496 -0.0894 0.0184 Uiso 1.0 12 calc R . . H11 H 0.5266 0.4956 0.1118 0.0175 Uiso 1.0 12 calc R . . H12 H 0.6152 0.5570 0.2500 0.0202 Uiso 1.0 6 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru1 0.00795(9) 0.00923(9) 0.00695(10) 0.00420(6) -0.00024(5) -0.00009(5) Cl1 0.0147(3) 0.0115(3) 0.0104(3) 0.0070(3) 0.0000 0.0000 Cl2 0.0233(7) 0.0270(7) 0.0510(9) 0.0165(6) 0.0000 0.0000 O1 0.0250(12) 0.0292(13) 0.0127(10) 0.0222(11) 0.0000 0.0000 O2 0.0359(16) 0.0338(15) 0.0310(15) 0.0152(13) 0.0000 0.0000 O3 0.030(4) 0.024(4) 0.030(4) 0.015(4) 0.0000 0.0000 N1 0.0110(11) 0.0131(12) 0.0100(11) 0.0057(10) 0.0000 0.0000 N2 0.0111(8) 0.0136(8) 0.0101(8) 0.0064(7) -0.0003(7) 0.0000(7) N3 0.0132(8) 0.0135(8) 0.0108(8) 0.0074(7) -0.0009(7) 0.0012(7) N4 0.0119(8) 0.0127(8) 0.0086(8) 0.0063(7) -0.0008(6) -0.0005(7) N5 0.0147(9) 0.0143(8) 0.0078(8) 0.0070(7) -0.0004(7) -0.0005(7) N6 0.0114(8) 0.0127(8) 0.0098(8) 0.0057(7) -0.0014(7) -0.0010(7) N7 0.0133(8) 0.0123(8) 0.0118(8) 0.0069(7) -0.0038(7) -0.0013(7) N8 0.0105(8) 0.0123(8) 0.0093(9) 0.0057(7) 0.0005(7) 0.0006(7) C1 0.0132(10) 0.0130(10) 0.0167(10) 0.0065(8) -0.0002(8) -0.0012(8) C2 0.0142(10) 0.0122(10) 0.0223(11) 0.0071(8) 0.0013(8) 0.0029(8) C3 0.0127(10) 0.0154(10) 0.0167(10) 0.0079(8) 0.0018(8) 0.0053(8) C4 0.0119(9) 0.0129(10) 0.0155(10) 0.0065(8) 0.0007(8) -0.0003(8) C5 0.0177(10) 0.0151(10) 0.0168(11) 0.0085(9) 0.0044(8) -0.0019(8) C6 0.0209(11) 0.0149(10) 0.0109(10) 0.0077(9) 0.0024(8) -0.0013(8) C7 0.0132(10) 0.0187(11) 0.0163(11) 0.0052(9) 0.0013(8) -0.0011(9) C8 0.0110(10) 0.0205(11) 0.0224(11) 0.0057(9) -0.0024(9) -0.0048(9) C9 0.0151(10) 0.0160(10) 0.0176(10) 0.0098(9) -0.0061(8) -0.0050(8) C10 0.0116(10) 0.0154(10) 0.0144(10) 0.0051(8) 0.0016(8) 0.0013(8) C11 0.0113(14) 0.0170(15) 0.0168(15) 0.0030(12) 0.0000 0.0000 C12 0.042(4) 0.042(4) 0.042(6) 0.0208(18) 0.0000 0.0000 C13 0.103(12) 0.103(12) 0.26(5) 0.052(6) 0.0000 0.0000 C14 0.060(3) 0.093(4) 0.0165(17) 0.066(3) 0.0000 0.0000 C15 0.042(3) 0.042(3) 0.059(6) 0.0208(14) 0.0000 0.0000 B1 0.0157(11) 0.0136(11) 0.0105(10) 0.0073(9) -0.0018(9) -0.0003(8) #============================================================================== _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'Il Milione (Burla, et al., 2007)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # 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 Ru1 Ru1 2.9051(3) yes . 10_555 Ru1 Cl1 2.4639(7) yes . . Ru1 N1 1.949(3) yes . . Ru1 N2 2.036(2) yes . . Ru1 N4 2.106(2) yes . . Ru1 N6 2.0957(16) yes . . Ru1 N8 2.0447(16) yes . . Cl2 C12 1.762(5) yes . . Cl2 C12 1.762(5) yes . 8_555 O1 N1 1.209(5) yes . . O2 C14 1.458(8) yes . . O3 C15 1.531(7) yes . . N2 N3 1.365(3) yes . . N2 C1 1.339(3) yes . . N3 C3 1.347(4) yes . . N3 B1 1.549(3) yes . . N4 N5 1.366(3) yes . . N4 C4 1.341(4) yes . . N5 C6 1.348(4) yes . . N5 B1 1.544(4) yes . . N6 N7 1.369(3) yes . . N6 C7 1.335(3) yes . . N7 C9 1.350(3) yes . . N7 B1 1.541(3) yes . . N8 N8 1.354(3) yes . 10_555 N8 C10 1.347(3) yes . . C1 C2 1.398(4) yes . . C2 C3 1.387(3) yes . . C4 C5 1.404(3) yes . . C5 C6 1.374(4) yes . . C7 C8 1.395(4) yes . . C8 C9 1.380(3) yes . . C10 C11 1.396(3) yes . . C12 C12 1.186(17) yes . 8_555 C12 C13 1.47(5) yes . . C1 H2 0.950 no . . C2 H3 0.950 no . . C3 H4 0.950 no . . C4 H5 0.950 no . . C5 H6 0.950 no . . C6 H7 0.950 no . . C7 H8 0.950 no . . C8 H9 0.950 no . . C9 H10 0.950 no . . C10 H11 0.950 no . . C11 H12 0.950 no . . B1 H1 1.000 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 Ru1 Ru1 Cl1 53.875(13) yes 10_555 . . Ru1 Ru1 N1 41.81(8) yes 10_555 . . Ru1 Ru1 N2 124.44(6) yes 10_555 . . Ru1 Ru1 N4 141.91(6) yes 10_555 . . Ru1 Ru1 N6 115.68(5) yes 10_555 . . Ru1 Ru1 N8 67.72(5) yes 10_555 . . Cl1 Ru1 N1 88.60(8) yes . . . Cl1 Ru1 N2 177.53(5) yes . . . Cl1 Ru1 N4 95.40(6) yes . . . Cl1 Ru1 N6 93.89(6) yes . . . Cl1 Ru1 N8 87.75(6) yes . . . N1 Ru1 N2 90.68(10) yes . . . N1 Ru1 N4 175.96(10) yes . . . N1 Ru1 N6 94.15(9) yes . . . N1 Ru1 N8 88.92(9) yes . . . N2 Ru1 N4 85.35(8) yes . . . N2 Ru1 N6 88.52(7) yes . . . N2 Ru1 N8 89.87(7) yes . . . N4 Ru1 N6 84.99(7) yes . . . N4 Ru1 N8 91.84(7) yes . . . N6 Ru1 N8 176.55(7) yes . . . Ru1 Cl1 Ru1 72.25(3) yes . . 10_555 C12 Cl2 C12 39.3(5) yes . . 8_555 Ru1 N1 Ru1 96.38(15) yes . . 10_555 Ru1 N1 O1 131.80(8) yes . . . Ru1 N1 O1 131.80(8) yes 10_555 . . Ru1 N2 N3 120.31(14) yes . . . Ru1 N2 C1 132.31(15) yes . . . N3 N2 C1 107.36(19) yes . . . N2 N3 C3 109.48(17) yes . . . N2 N3 B1 119.62(19) yes . . . C3 N3 B1 130.83(18) yes . . . Ru1 N4 N5 119.14(17) yes . . . Ru1 N4 C4 133.86(15) yes . . . N5 N4 C4 106.88(19) yes . . . N4 N5 C6 109.1(3) yes . . . N4 N5 B1 119.23(19) yes . . . C6 N5 B1 131.65(19) yes . . . Ru1 N6 N7 118.36(11) yes . . . Ru1 N6 C7 135.44(15) yes . . . N7 N6 C7 106.14(16) yes . . . N6 N7 C9 109.80(16) yes . . . N6 N7 B1 120.15(16) yes . . . C9 N7 B1 129.91(18) yes . . . Ru1 N8 N8 112.28(12) yes . . 10_555 Ru1 N8 C10 138.72(15) yes . . . N8 N8 C10 108.73(16) yes 10_555 . . N2 C1 C2 109.62(19) yes . . . C1 C2 C3 105.3(2) yes . . . N3 C3 C2 108.3(2) yes . . . N4 C4 C5 110.2(3) yes . . . C4 C5 C6 104.5(3) yes . . . N5 C6 C5 109.4(2) yes . . . N6 C7 C8 110.94(19) yes . . . C7 C8 C9 104.72(18) yes . . . N7 C9 C8 108.4(2) yes . . . N8 C10 C11 108.62(19) yes . . . C10 C11 C10 105.3(2) yes . . 10_555 Cl2 C12 Cl2 109.3(4) yes . . 3_555 Cl2 C12 Cl2 109.3(4) yes . . 5_555 Cl2 C12 C12 70.3(4) yes . . 8_555 Cl2 C12 C13 109.7(4) yes . . . Cl2 C12 Cl2 109.3(4) yes 3_555 . 5_555 Cl2 C12 C12 70.3(4) yes 3_555 . 8_555 Cl2 C12 C13 109.7(4) yes 3_555 . . Cl2 C12 C12 70.3(4) yes 5_555 . 8_555 Cl2 C12 C13 109.7(4) yes 5_555 . . C12 C12 C13 180.000 yes 8_555 . . O3 C15 O3 120.0(7) yes . . 3_665 O3 C15 O3 120.0(7) yes . . 5_565 O3 C15 O3 120.0(7) yes 3_665 . 5_565 N3 B1 N5 107.59(17) yes . . . N3 B1 N7 107.49(19) yes . . . N5 B1 N7 107.95(19) yes . . . N2 C1 H2 125.194 no . . . C2 C1 H2 125.187 no . . . C1 C2 H3 127.361 no . . . C3 C2 H3 127.366 no . . . N3 C3 H4 125.865 no . . . C2 C3 H4 125.868 no . . . N4 C4 H5 124.909 no . . . C5 C4 H5 124.926 no . . . C4 C5 H6 127.751 no . . . C6 C5 H6 127.750 no . . . N5 C6 H7 125.314 no . . . C5 C6 H7 125.330 no . . . N6 C7 H8 124.520 no . . . C8 C7 H8 124.539 no . . . C7 C8 H9 127.636 no . . . C9 C8 H9 127.649 no . . . N7 C9 H10 125.799 no . . . C8 C9 H10 125.805 no . . . N8 C10 H11 125.692 no . . . C11 C10 H11 125.687 no . . . C10 C11 H12 127.350 no . . . C10 C11 H12 127.350 no 10_555 . . N3 B1 H1 111.211 no . . . N5 B1 H1 111.210 no . . . N7 B1 H1 111.209 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 Ru1 Ru1 Cl1 Ru1 0.0 no 10_555 . . 10_555 Cl1 Ru1 Ru1 Cl1 0.00(2) no . . 10_555 . Cl1 Ru1 Ru1 N1 -140.41(3) no . . 10_555 . Cl1 Ru1 Ru1 N2 177.78(3) no . . 10_555 10_555 Cl1 Ru1 Ru1 N4 42.08(3) no . . 10_555 10_555 Cl1 Ru1 Ru1 N6 -75.06(3) no . . 10_555 10_555 Cl1 Ru1 Ru1 N8 104.28(3) no . . 10_555 10_555 Ru1 Ru1 N1 Ru1 0.0 no 10_555 . . 10_555 Ru1 Ru1 N1 O1 178.3(3) no 10_555 . . . N1 Ru1 Ru1 Cl1 140.41(9) no . . 10_555 . N1 Ru1 Ru1 N1 0.00(9) no . . 10_555 . N1 Ru1 Ru1 N2 -41.82(9) no . . 10_555 10_555 N1 Ru1 Ru1 N4 -177.52(9) no . . 10_555 10_555 N1 Ru1 Ru1 N6 65.34(9) no . . 10_555 10_555 N1 Ru1 Ru1 N8 -115.32(9) no . . 10_555 10_555 Ru1 Ru1 N2 N3 -160.86(10) no 10_555 . . . Ru1 Ru1 N2 C1 21.4(2) no 10_555 . . . N2 Ru1 Ru1 Cl1 -177.78(7) no . . 10_555 . N2 Ru1 Ru1 N1 41.82(7) no . . 10_555 . N2 Ru1 Ru1 N2 0.00(7) no . . 10_555 10_555 N2 Ru1 Ru1 N4 -135.70(7) no . . 10_555 10_555 N2 Ru1 Ru1 N6 107.16(7) no . . 10_555 10_555 N2 Ru1 Ru1 N8 -73.50(7) no . . 10_555 10_555 Ru1 Ru1 N4 N5 169.80(5) no 10_555 . . . Ru1 Ru1 N4 C4 -5.71(17) no 10_555 . . . N4 Ru1 Ru1 Cl1 -42.08(7) no . . 10_555 . N4 Ru1 Ru1 N1 177.52(7) no . . 10_555 . N4 Ru1 Ru1 N2 135.70(7) no . . 10_555 10_555 N4 Ru1 Ru1 N4 0.00(7) no . . 10_555 10_555 N4 Ru1 Ru1 N6 -117.14(7) no . . 10_555 10_555 N4 Ru1 Ru1 N8 62.20(7) no . . 10_555 10_555 Ru1 Ru1 N6 N7 165.45(12) no 10_555 . . . Ru1 Ru1 N6 C7 -11.4(3) no 10_555 . . . N6 Ru1 Ru1 Cl1 75.06(7) no . . 10_555 . N6 Ru1 Ru1 N1 -65.34(7) no . . 10_555 . N6 Ru1 Ru1 N2 -107.16(7) no . . 10_555 10_555 N6 Ru1 Ru1 N4 117.14(7) no . . 10_555 10_555 N6 Ru1 Ru1 N6 0.00(7) no . . 10_555 10_555 N6 Ru1 Ru1 N8 179.34(7) no . . 10_555 10_555 Ru1 Ru1 N8 N8 0.00(11) no 10_555 . . 10_555 Ru1 Ru1 N8 C10 -173.0(3) no 10_555 . . . N8 Ru1 Ru1 Cl1 -104.28(7) no . . 10_555 . N8 Ru1 Ru1 N1 115.32(7) no . . 10_555 . N8 Ru1 Ru1 N2 73.50(7) no . . 10_555 10_555 N8 Ru1 Ru1 N4 -62.20(7) no . . 10_555 10_555 N8 Ru1 Ru1 N6 -179.34(7) no . . 10_555 10_555 N8 Ru1 Ru1 N8 0.00(7) no . . 10_555 10_555 Cl1 Ru1 N1 Ru1 30.99(7) no . . . 10_555 Cl1 Ru1 N1 O1 -150.66(19) no . . . . N1 Ru1 Cl1 Ru1 -25.15(6) no . . . 10_555 Cl1 Ru1 N4 N5 136.87(10) no . . . . Cl1 Ru1 N4 C4 -38.65(13) no . . . . N4 Ru1 Cl1 Ru1 155.46(5) no . . . 10_555 Cl1 Ru1 N6 N7 -143.08(14) no . . . . Cl1 Ru1 N6 C7 40.1(2) no . . . . N6 Ru1 Cl1 Ru1 -119.21(6) no . . . 10_555 Cl1 Ru1 N8 N8 -51.57(13) no . . . 10_555 Cl1 Ru1 N8 C10 135.4(3) no . . . . N8 Ru1 Cl1 Ru1 63.82(6) no . . . 10_555 N1 Ru1 N2 N3 -134.47(15) no . . . . N1 Ru1 N2 C1 47.83(18) no . . . . N2 Ru1 N1 Ru1 -146.64(8) no . . . 10_555 N2 Ru1 N1 O1 31.71(19) no . . . . N1 Ru1 N6 N7 128.05(16) no . . . . N1 Ru1 N6 C7 -48.8(3) no . . . . N6 Ru1 N1 Ru1 124.79(9) no . . . 10_555 N6 Ru1 N1 O1 -56.86(19) no . . . . N1 Ru1 N8 N8 37.06(15) no . . . 10_555 N1 Ru1 N8 C10 -136.0(3) no . . . . N8 Ru1 N1 Ru1 -56.78(9) no . . . 10_555 N8 Ru1 N1 O1 121.56(19) no . . . . N2 Ru1 N4 N5 -45.50(10) no . . . . N2 Ru1 N4 C4 138.99(13) no . . . . N4 Ru1 N2 N3 44.75(14) no . . . . N4 Ru1 N2 C1 -132.95(18) no . . . . N2 Ru1 N6 N7 37.47(16) no . . . . N2 Ru1 N6 C7 -139.3(3) no . . . . N6 Ru1 N2 N3 -40.34(14) no . . . . N6 Ru1 N2 C1 141.96(18) no . . . . N2 Ru1 N8 N8 127.75(15) no . . . 10_555 N2 Ru1 N8 C10 -45.3(3) no . . . . N8 Ru1 N2 N3 136.61(14) no . . . . N8 Ru1 N2 C1 -41.09(18) no . . . . N4 Ru1 N6 N7 -47.99(15) no . . . . N4 Ru1 N6 C7 135.2(3) no . . . . N6 Ru1 N4 N5 43.42(11) no . . . . N6 Ru1 N4 C4 -132.09(14) no . . . . N4 Ru1 N8 N8 -146.91(14) no . . . 10_555 N4 Ru1 N8 C10 40.1(3) no . . . . N8 Ru1 N4 N5 -135.22(11) no . . . . N8 Ru1 N4 C4 49.26(14) no . . . . C12 Cl2 C12 Cl2 59.8(5) no . . 8_555 5_555 C12 Cl2 C12 Cl2 -59.8(5) no . . 8_555 3_555 C12 Cl2 C12 C12 0.0 no . . 8_555 . C12 Cl2 C12 C13 180(28800) no . . 8_555 8_555 C12 Cl2 C12 Cl2 59.8(5) no 8_555 . . 3_555 C12 Cl2 C12 Cl2 -59.8(5) no 8_555 . . 5_555 C12 Cl2 C12 C12 0.0 no 8_555 . . 8_555 C12 Cl2 C12 C13 180(288000) no 8_555 . . . Ru1 N2 N3 C3 -178.53(11) no . . . . Ru1 N2 N3 B1 -1.3(3) no . . . . Ru1 N2 C1 C2 178.47(14) no . . . . N3 N2 C1 C2 0.6(3) no . . . . C1 N2 N3 C3 -0.3(3) no . . . . C1 N2 N3 B1 176.90(17) no . . . . N2 N3 C3 C2 -0.0(3) no . . . . N2 N3 B1 N5 -57.6(3) no . . . . N2 N3 B1 N7 58.4(3) no . . . . C3 N3 B1 N5 118.9(3) no . . . . C3 N3 B1 N7 -125.1(3) no . . . . B1 N3 C3 C2 -176.8(2) no . . . . Ru1 N4 N5 C6 -175.99(8) no . . . . Ru1 N4 N5 B1 2.29(17) no . . . . Ru1 N4 C4 C5 175.33(10) no . . . . N5 N4 C4 C5 -0.58(18) no . . . . C4 N4 N5 C6 0.63(17) no . . . . C4 N4 N5 B1 178.91(12) no . . . . N4 N5 C6 C5 -0.45(19) no . . . . N4 N5 B1 N3 55.87(19) no . . . . N4 N5 B1 N7 -59.86(19) no . . . . C6 N5 B1 N3 -126.30(19) no . . . . C6 N5 B1 N7 118.0(2) no . . . . B1 N5 C6 C5 -178.44(15) no . . . . Ru1 N6 N7 C9 -177.11(13) no . . . . Ru1 N6 N7 B1 6.8(3) no . . . . Ru1 N6 C7 C8 176.61(16) no . . . . N7 N6 C7 C8 -0.5(3) no . . . . C7 N6 N7 C9 0.6(3) no . . . . C7 N6 N7 B1 -175.6(2) no . . . . N6 N7 C9 C8 -0.4(3) no . . . . N6 N7 B1 N3 -61.1(3) no . . . . N6 N7 B1 N5 54.7(3) no . . . . C9 N7 B1 N3 123.6(3) no . . . . C9 N7 B1 N5 -120.6(3) no . . . . B1 N7 C9 C8 175.2(3) no . . . . Ru1 N8 N8 Ru1 0.0(2) no . . 10_555 10_555 Ru1 N8 N8 C10 -175.15(13) no . . 10_555 10_555 Ru1 N8 C10 C11 173.57(18) no . . . . N8 N8 C10 C11 0.4(3) no 10_555 . . . C10 N8 N8 Ru1 175.15(18) no . . 10_555 10_555 C10 N8 N8 C10 0.0(3) no . . 10_555 10_555 N2 C1 C2 C3 -0.6(3) no . . . . C1 C2 C3 N3 0.4(3) no . . . . N4 C4 C5 C6 0.31(19) no . . . . C4 C5 C6 N5 0.1(2) no . . . . N6 C7 C8 C9 0.2(4) no . . . . C7 C8 C9 N7 0.1(3) no . . . . N8 C10 C11 C10 -0.6(4) no . . . 10_555 Cl2 C12 C12 Cl2 -120.00(4) no . . 8_555 5_555 Cl2 C12 C12 Cl2 0.00(4) no . . 8_555 . Cl2 C12 C12 Cl2 120.00(4) no . . 8_555 3_555 Cl2 C12 C12 Cl2 120.00(4) no 3_555 . 8_555 5_555 Cl2 C12 C12 Cl2 -120.00(4) no 3_555 . 8_555 . Cl2 C12 C12 Cl2 0.00(4) no 3_555 . 8_555 3_555 Cl2 C12 C12 Cl2 0.00(4) no 5_555 . 8_555 5_555 Cl2 C12 C12 Cl2 120.00(4) no 5_555 . 8_555 . Cl2 C12 C12 Cl2 -120.00(4) no 5_555 . 8_555 3_555 loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Ru1 B1 3.185(3) no . . Cl1 N4 3.3885(18) no . 10_555 Cl1 N6 3.341(3) no . 10_555 Cl1 N8 3.1394(16) no . 10_555 Cl2 C13 2.64(4) no . 8_555 O1 N2 3.091(3) no . . O1 N2 3.091(3) no . 10_555 O1 N6 3.401(3) no . . O1 N6 3.401(3) no . 10_555 O1 C1 3.274(3) no . . O1 C1 3.274(3) no . 10_555 N1 N2 2.8351(19) no . 10_555 N1 N6 2.963(3) no . 10_555 N1 N8 2.798(4) no . 10_555 N1 C1 3.309(3) no . . N1 C1 3.309(3) no . 10_555 N1 C7 3.524(3) no . . N1 C7 3.524(3) no . 10_555 N2 N5 2.990(3) no . . N2 N7 2.993(2) no . . N2 C10 3.421(3) no . . N3 N4 2.968(4) no . . N3 N6 3.025(3) no . . N4 N7 3.005(3) no . . N4 C10 3.481(3) no . . N5 N6 2.977(3) no . . N8 C1 3.273(4) no . . N8 C4 3.485(3) no . . C1 C10 3.506(4) no . . Cl1 O2 3.317(3) no . 6_555 O1 O3 2.942(11) no . . O1 C5 3.334(3) no . 2_555 O1 C5 3.334(3) no . 11_555 O1 C6 3.577(4) no . 2_555 O1 C6 3.577(4) no . 11_555 O2 Cl1 3.317(3) no . 2_554 O2 C3 3.297(3) no . . O2 C3 3.297(3) no . 10_554 O3 O1 2.942(11) no . . O3 C1 3.310(9) no . 5_565 O3 C1 3.310(9) no . 8_565 N2 C5 3.584(4) no . 11_555 N3 C5 3.446(4) no . 11_555 N4 C9 3.477(4) no . 9_555 N5 C8 3.533(4) no . 9_555 N6 C5 3.579(3) no . 11_555 N7 C4 3.523(3) no . 11_555 N7 C5 3.396(3) no . 11_555 N7 C8 3.531(4) no . 9_555 C1 O3 3.310(9) no . 3_665 C2 C4 3.587(3) no . 7_665 C3 O2 3.297(3) no . . C3 C10 3.466(4) no . 7_665 C4 N7 3.523(3) no . 9_555 C4 C2 3.587(3) no . 7_665 C4 C9 3.388(4) no . 9_555 C5 O1 3.334(3) no . 6_554 C5 N2 3.584(4) no . 9_555 C5 N3 3.446(4) no . 9_555 C5 N6 3.579(3) no . 9_555 C5 N7 3.396(3) no . 9_555 C5 C9 3.544(3) no . 9_555 C6 O1 3.577(4) no . 6_554 C6 C8 3.506(4) no . 9_555 C8 N5 3.533(4) no . 11_555 C8 N7 3.531(4) no . 11_555 C8 C6 3.506(4) no . 11_555 C8 C9 3.547(4) no . 11_555 C9 N4 3.477(4) no . 11_555 C9 C4 3.388(4) no . 11_555 C9 C5 3.544(3) no . 11_555 C9 C8 3.547(4) no . 9_555 C10 C3 3.466(4) no . 7_665 C11 C14 3.594(8) no . 6_555 C13 C13 3.18(7) no . 7_555 C14 C11 3.594(8) no . 2_554 Ru1 H2 3.3375 no . . Ru1 H5 3.4254 no . . Ru1 H8 3.4365 no . . Ru1 H11 3.4877 no . . Cl1 H5 3.4719 no . . Cl1 H5 3.4719 no . 10_555 Cl1 H8 3.4148 no . . Cl1 H8 3.4148 no . 10_555 O1 H2 3.1083 no . . O1 H2 3.1083 no . 10_555 N1 H2 3.1600 no . . N1 H2 3.1600 no . 10_555 N1 H8 3.4293 no . . N1 H8 3.4293 no . 10_555 N2 H1 3.3424 no . . N2 H3 3.1528 no . . N2 H4 3.1292 no . . N2 H11 3.3601 no . . N3 H2 3.0956 no . . N3 H3 3.1348 no . . N4 H1 3.3368 no . . N4 H6 3.1667 no . . N4 H7 3.1247 no . . N4 H11 3.2967 no . . N5 H5 3.0912 no . . N5 H6 3.1410 no . . N6 H1 3.3438 no . . N6 H9 3.1636 no . . N6 H10 3.1383 no . . N7 H8 3.0787 no . . N7 H9 3.1348 no . . N8 H2 3.0727 no . . N8 H5 3.3218 no . . N8 H11 3.1107 no . 10_555 N8 H12 3.1462 no . . C1 H4 3.1356 no . . C1 H11 3.4464 no . . C3 H1 2.7925 no . . C3 H2 3.1322 no . . C4 H7 3.1192 no . . C4 H11 3.4464 no . . C6 H1 2.8039 no . . C6 H5 3.1146 no . . C7 H8 3.0200 no . 10_555 C7 H10 3.1202 no . . C9 H1 2.7707 no . . C9 H8 3.1142 no . . C10 H2 3.2687 no . . C10 H5 3.4978 no . . C10 H11 3.1402 no . 10_555 C11 H11 2.0972 no . 10_555 B1 H4 2.9435 no . . B1 H7 2.9480 no . . B1 H10 2.9243 no . . H1 H4 2.7647 no . . H1 H7 2.7758 no . . H1 H10 2.7348 no . . H2 H2 3.0390 no . 10_555 H2 H3 2.5222 no . . H2 H11 3.3995 no . . H3 H4 2.5200 no . . H5 H6 2.5292 no . . H5 H11 3.3901 no . . H6 H7 2.5054 no . . H8 H8 2.1125 no . 10_555 H8 H9 2.5137 no . . H9 H10 2.5160 no . . H11 H12 2.5265 no . . Cl1 H10 3.0097 no . 6_555 Cl1 H10 3.0097 no . 9_555 Cl2 H8 3.2461 no . . Cl2 H8 3.3637 no . 3_555 Cl2 H8 3.2461 no . 10_555 Cl2 H8 3.3637 no . 12_555 Cl2 H9 3.4725 no . . Cl2 H9 3.4725 no . 10_555 Cl2 H10 3.5016 no . 2_555 Cl2 H10 3.5016 no . 11_555 O1 H6 2.6961 no . 2_555 O1 H6 2.6961 no . 11_555 O1 H7 3.1835 no . 2_555 O1 H7 3.1835 no . 11_555 O2 H1 3.3161 no . . O2 H1 3.3161 no . 10_554 O2 H4 2.4326 no . . O2 H4 2.4326 no . 10_554 O2 H5 2.8698 no . 2_554 O2 H5 2.8698 no . 11_555 O2 H12 3.3684 no . 4_664 O3 H2 3.3389 no . . O3 H2 2.4888 no . 5_565 O3 H2 2.4888 no . 8_565 O3 H2 3.3389 no . 10_555 O3 H6 3.1640 no . 2_555 O3 H6 3.1640 no . 11_555 N1 H6 3.4621 no . 2_555 N1 H6 3.4621 no . 11_555 N2 H6 2.8761 no . 11_555 N2 H11 3.5198 no . 7_665 N3 H5 3.3219 no . 11_555 N3 H6 2.9934 no . 11_555 N3 H11 3.0006 no . 7_665 N4 H10 3.3050 no . 9_555 N5 H9 3.5393 no . 9_555 N5 H11 3.1670 no . 7_665 N5 H12 3.5017 no . 4_664 N6 H6 3.4828 no . 11_555 N6 H9 3.2738 no . 9_555 N6 H10 3.2956 no . 9_555 N7 H6 3.4654 no . 11_555 N7 H9 2.9233 no . 9_555 C1 H6 2.9868 no . 11_555 C2 H3 3.5572 no . 3_665 C2 H3 2.9399 no . 5_565 C2 H5 3.3796 no . 7_665 C2 H6 3.4621 no . 7_665 C2 H6 3.1815 no . 11_555 C2 H11 3.4237 no . 7_665 C3 H3 3.3483 no . 5_565 C3 H5 3.0442 no . 11_555 C3 H6 3.1776 no . 11_555 C3 H11 2.9271 no . 7_665 C3 H12 3.4942 no . 4_664 C4 H3 3.2951 no . 7_665 C4 H10 3.3737 no . 9_555 C5 H2 3.4936 no . 7_665 C5 H3 3.2710 no . 7_665 C6 H7 3.1775 no . 10_554 C6 H11 3.3532 no . 7_665 C6 H12 3.3153 no . 4_664 C7 H7 3.5856 no . 11_555 C7 H9 3.2357 no . 9_555 C7 H10 3.4083 no . 9_555 C8 H9 2.9091 no . 9_555 C9 H9 2.6901 no . 9_555 C10 H4 3.3830 no . 7_665 C11 H1 3.5138 no . 4_665 C11 H1 3.5138 no . 7_665 C11 H4 3.3481 no . 4_665 C11 H4 3.3481 no . 7_665 C11 H7 3.2768 no . 4_665 C11 H7 3.2768 no . 7_665 C13 H9 3.1591 no . . C13 H9 3.1591 no . 3_555 C13 H9 3.1591 no . 5_555 C14 H4 2.9852 no . . C14 H4 3.3343 no . 5_565 C14 H4 3.3343 no . 8_564 C14 H4 2.9852 no . 10_554 C14 H5 3.0663 no . 2_554 C14 H5 3.0663 no . 11_555 C15 H2 3.2338 no . . C15 H2 3.2337 no . 3_665 C15 H2 3.2336 no . 5_565 C15 H2 3.2336 no . 8_565 C15 H2 3.2338 no . 10_555 C15 H2 3.2337 no . 12_665 B1 H11 3.4675 no . 7_665 B1 H12 3.3482 no . 4_664 H1 O2 3.3161 no . . H1 C11 3.5138 no . 4_664 H1 H5 3.5214 no . 11_555 H1 H11 3.5843 no . 7_665 H1 H12 2.7446 no . 4_664 H2 O3 3.3389 no . . H2 O3 2.4888 no . 3_665 H2 C5 3.4936 no . 7_665 H2 C15 3.2338 no . . H2 H6 3.2822 no . 7_665 H2 H6 3.4308 no . 11_555 H3 C2 2.9399 no . 3_665 H3 C2 3.5572 no . 5_565 H3 C3 3.3483 no . 3_665 H3 C4 3.2951 no . 7_665 H3 C5 3.2710 no . 7_665 H3 H3 2.6660 no . 3_665 H3 H3 2.6660 no . 5_565 H3 H4 3.4248 no . 3_665 H3 H5 2.9737 no . 7_665 H3 H6 2.9601 no . 7_665 H4 O2 2.4326 no . . H4 C10 3.3830 no . 7_665 H4 C11 3.3481 no . 4_664 H4 C14 2.9852 no . . H4 C14 3.3343 no . 3_665 H4 H3 3.4248 no . 5_565 H4 H5 2.8867 no . 11_555 H4 H11 3.0951 no . 7_665 H4 H12 3.0384 no . 4_664 H5 O2 2.8698 no . 6_555 H5 N3 3.3219 no . 9_555 H5 C2 3.3796 no . 7_665 H5 C3 3.0442 no . 9_555 H5 C14 3.0663 no . 6_555 H5 H1 3.5214 no . 9_555 H5 H3 2.9737 no . 7_665 H5 H4 2.8867 no . 9_555 H5 H10 3.5548 no . 9_555 H6 O1 2.6961 no . 6_554 H6 O3 3.1640 no . 6_554 H6 N1 3.4621 no . 6_554 H6 N2 2.8761 no . 9_555 H6 N3 2.9934 no . 9_555 H6 N6 3.4828 no . 9_555 H6 N7 3.4654 no . 9_555 H6 C1 2.9868 no . 9_555 H6 C2 3.4621 no . 7_665 H6 C2 3.1815 no . 9_555 H6 C3 3.1776 no . 9_555 H6 H2 3.2822 no . 7_665 H6 H2 3.4308 no . 9_555 H6 H3 2.9601 no . 7_665 H7 O1 3.1835 no . 6_554 H7 C6 3.1775 no . 10_554 H7 C7 3.5856 no . 9_555 H7 C11 3.2768 no . 4_664 H7 H7 2.2386 no . 10_554 H7 H11 3.5608 no . 7_665 H7 H12 2.8530 no . 4_664 H8 Cl2 3.2461 no . . H8 Cl2 3.3637 no . 5_555 H8 H10 3.5293 no . 9_555 H9 Cl2 3.4725 no . . H9 N5 3.5393 no . 11_555 H9 N6 3.2738 no . 11_555 H9 N7 2.9233 no . 11_555 H9 C7 3.2357 no . 11_555 H9 C8 2.9091 no . 11_555 H9 C9 2.6901 no . 11_555 H9 C13 3.1591 no . . H9 H9 3.3311 no . 9_555 H9 H9 3.3311 no . 11_555 H9 H10 2.9743 no . 11_555 H10 Cl1 3.0097 no . 2_554 H10 Cl2 3.5016 no . 6_554 H10 N4 3.3050 no . 11_555 H10 N6 3.2956 no . 11_555 H10 C4 3.3737 no . 11_555 H10 C7 3.4083 no . 11_555 H10 H5 3.5548 no . 11_555 H10 H8 3.5293 no . 11_555 H10 H9 2.9743 no . 9_555 H11 N2 3.5198 no . 7_665 H11 N3 3.0006 no . 7_665 H11 N5 3.1670 no . 7_665 H11 C2 3.4237 no . 7_665 H11 C3 2.9271 no . 7_665 H11 C6 3.3532 no . 7_665 H11 B1 3.4675 no . 7_665 H11 H1 3.5843 no . 7_665 H11 H4 3.0951 no . 7_665 H11 H7 3.5608 no . 7_665 H11 H11 3.4537 no . 7_665 H12 O2 3.3684 no . 4_665 H12 N5 3.5017 no . 4_665 H12 N5 3.5017 no . 7_665 H12 C3 3.4942 no . 4_665 H12 C3 3.4942 no . 7_665 H12 C6 3.3153 no . 4_665 H12 C6 3.3153 no . 7_665 H12 B1 3.3482 no . 4_665 H12 B1 3.3482 no . 7_665 H12 H1 2.7446 no . 4_665 H12 H1 2.7446 no . 7_665 H12 H4 3.0384 no . 4_665 H12 H4 3.0384 no . 7_665 H12 H7 2.8530 no . 4_665 H12 H7 2.8530 no . 7_665 #============================================================================== #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== _database_code_depnum_ccdc_archive 'CCDC 939833' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1051b #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C24 H30 B3 Cl3 F4 N14 O Ru2' _chemical_formula_moiety 'C24 H30 B3 Cl3 F4 N14 O Ru2' _chemical_formula_weight 947.52 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/m 1' _symmetry_space_group_name_Hall '-P 2yb' _symmetry_Int_Tables_number 11 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,-Z 3 -X,-Y,-Z 4 +X,1/2-Y,+Z #------------------------------------------------------------------------------ _cell_length_a 9.2986(15) _cell_length_b 14.618(3) _cell_length_c 13.390(3) _cell_angle_alpha 90.0000 _cell_angle_beta 100.519(3) _cell_angle_gamma 90.0000 _cell_volume 1789.5(5) _cell_formula_units_Z 2 _cell_measurement_reflns_used 5689 _cell_measurement_theta_min 3.19 _cell_measurement_theta_max 27.49 _cell_measurement_temperature 93 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour darkBrown _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.070 _exptl_crystal_size_min 0.040 _exptl_crystal_density_diffrn 1.758 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 940.00 _exptl_absorpt_coefficient_mu 1.133 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_correction_T_min 0.879 _exptl_absorpt_correction_T_max 0.956 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 93 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku Saturn724' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.111 _diffrn_reflns_number 14890 _diffrn_reflns_av_R_equivalents 0.0258 _diffrn_reflns_theta_max 27.47 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measured_fraction_theta_full 0.994 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # 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 4230 _reflns_number_gt 3692 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_ref 0.1125 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 4230 _refine_ls_number_parameters 257 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0617P)^2^+4.5419P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.000 _refine_diff_density_max 2.820 _refine_diff_density_min -1.110 _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 0.0033 0.0016 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.0061 0.0033 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; B B 0.0013 0.0007 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.1484 0.1585 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; F F 0.0171 0.0103 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ru Ru -1.2594 0.8363 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.0106 0.0060 ; 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 Ru1 Ru 0.59849(3) 0.141928(17) 0.78166(2) 0.01677(11) Uani 1.0 4 d . . . Cl1 Cl 0.50084(13) 0.2500 0.89191(9) 0.0204(3) Uani 1.0 2 d . . . Cl2 Cl 0.2181(2) -0.2500 0.84592(14) 0.0490(5) Uani 1.0 2 d . . . Cl3 Cl -0.0421(3) -0.39968(18) 0.85406(17) 0.0422(5) Uani 0.5000 4 d . . . F1 F 1.1556(4) 0.2500 0.4863(3) 0.0390(9) Uani 1.0 2 d . . . F2 F 0.9985(4) 0.2500 0.5986(3) 0.0374(8) Uani 1.0 2 d . . . F3 F 0.9461(4) 0.1710(3) 0.4532(3) 0.0694(11) Uani 1.0 4 d . . . O1 O 0.5599(4) 0.2500 0.6901(3) 0.0194(7) Uani 1.0 2 d . . . N2 N 0.6783(4) 0.0584(2) 0.6846(3) 0.0219(6) Uani 1.0 4 d . . . N3 N 0.6399(4) -0.0316(3) 0.6794(3) 0.0264(7) Uani 1.0 4 d . . . N4 N 0.6411(4) 0.0417(2) 0.8854(2) 0.0199(6) Uani 1.0 4 d . . . N5 N 0.6058(4) -0.0463(2) 0.8592(3) 0.0235(7) Uani 1.0 4 d . . . N6 N 0.3983(3) 0.0798(2) 0.7328(2) 0.0204(6) Uani 1.0 4 d . . . N7 N 0.3929(4) -0.0125(3) 0.7233(3) 0.0239(7) Uani 1.0 4 d . . . N8 N 0.7956(4) 0.20297(19) 0.8301(2) 0.0195(6) Uani 1.0 4 d . . . C1 C 0.7678(4) 0.0737(3) 0.6181(3) 0.0268(8) Uani 1.0 4 d . . . C2 C 0.7875(5) -0.0078(4) 0.5693(3) 0.0339(10) Uani 1.0 4 d . . . C3 C 0.7070(5) -0.0724(3) 0.6096(3) 0.0344(10) Uani 1.0 4 d . . . C4 C 0.6963(4) 0.0416(3) 0.9857(3) 0.0256(8) Uani 1.0 4 d . . . C5 C 0.6963(5) -0.0470(3) 1.0231(3) 0.0336(9) Uani 1.0 4 d . . . C6 C 0.6384(5) -0.0998(3) 0.9414(4) 0.0348(10) Uani 1.0 4 d . . . C7 C 0.2609(4) 0.1103(3) 0.7110(3) 0.0249(8) Uani 1.0 4 d . . . C8 C 0.1654(5) 0.0371(3) 0.6873(3) 0.0313(9) Uani 1.0 4 d . . . C9 C 0.2524(5) -0.0387(3) 0.6958(3) 0.0332(10) Uani 1.0 4 d . . . C10 C 0.9342(4) 0.1748(3) 0.8579(3) 0.0232(7) Uani 1.0 4 d . . . C11 C 1.0261(6) 0.2500 0.8768(4) 0.0266(11) Uani 1.0 2 d . . . C12 C 0.5024(6) 0.2500 0.5851(4) 0.0229(10) Uani 1.0 2 d . . . C13 C 0.0247(16) -0.2231(9) 0.8142(16) 0.095(6) Uani 0.5000 4 d . . . C14 C -0.0618(16) -0.2966(11) 0.7750(12) 0.079(5) Uani 0.5000 4 d . . . B1 B 0.5355(6) -0.0677(3) 0.7473(4) 0.0290(10) Uani 1.0 4 d . . . B2 B 1.0103(7) 0.2500 0.4966(5) 0.0269(13) Uani 1.0 2 d . . . H1 H 0.5168 -0.1347 0.7368 0.0348 Uiso 1.0 4 calc R . . H2 H 0.8105 0.1308 0.6064 0.0322 Uiso 1.0 4 calc R . . H3 H 0.8450 -0.0172 0.5183 0.0406 Uiso 1.0 4 calc R . . H4 H 0.6996 -0.1352 0.5915 0.0413 Uiso 1.0 4 calc R . . H5 H 0.7301 0.0941 1.0248 0.0307 Uiso 1.0 4 calc R . . H6 H 0.7295 -0.0667 1.0910 0.0403 Uiso 1.0 4 calc R . . H7 H 0.6237 -0.1641 0.9427 0.0418 Uiso 1.0 4 calc R . . H8 H 0.2326 0.1727 0.7116 0.0299 Uiso 1.0 4 calc R . . H9 H 0.0618 0.0393 0.6690 0.0376 Uiso 1.0 4 calc R . . H10 H 0.2193 -0.0999 0.6843 0.0398 Uiso 1.0 4 calc R . . H11 H 0.9649 0.1127 0.8637 0.0278 Uiso 1.0 4 calc R . . H12 H 1.1293 0.2500 0.8981 0.0319 Uiso 1.0 2 calc R . . H13 H 0.4914 0.1868 0.5604 0.0275 Uiso 0.5000 4 calc R . . H14 H 0.5691 0.2830 0.5490 0.0275 Uiso 0.5000 4 calc R . . H15 H 0.4067 0.2802 0.5729 0.0275 Uiso 0.5000 4 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru1 0.01827(16) 0.01349(15) 0.01850(15) -0.00074(9) 0.00324(10) 0.00067(10) Cl1 0.0249(6) 0.0174(6) 0.0197(6) 0.0000 0.0057(5) 0.0000 Cl2 0.0504(11) 0.0412(9) 0.0497(10) 0.0000 -0.0064(8) 0.0000 Cl3 0.0334(12) 0.0549(14) 0.0380(11) -0.0126(10) 0.0056(9) 0.0016(10) F1 0.032(2) 0.039(2) 0.049(3) 0.0000 0.0141(16) 0.0000 F2 0.044(3) 0.043(2) 0.0267(17) 0.0000 0.0089(15) 0.0000 F3 0.062(3) 0.082(3) 0.067(2) -0.0400(19) 0.0183(17) -0.043(2) O1 0.0198(18) 0.0173(17) 0.0203(17) 0.0000 0.0012(13) 0.0000 N2 0.0234(16) 0.0226(15) 0.0198(14) 0.0000(12) 0.0039(11) 0.0016(12) N3 0.0347(18) 0.0255(17) 0.0186(15) 0.0032(13) 0.0040(13) -0.0061(12) N4 0.0229(15) 0.0181(14) 0.0187(14) 0.0010(11) 0.0040(11) -0.0006(11) N5 0.0345(18) 0.0140(14) 0.0227(15) -0.0011(12) 0.0072(13) 0.0013(12) N6 0.0248(16) 0.0191(14) 0.0171(13) -0.0041(12) 0.0033(11) -0.0005(12) N7 0.0283(17) 0.0198(15) 0.0229(15) -0.0086(12) 0.0033(12) -0.0043(12) N8 0.0200(15) 0.0158(15) 0.0217(14) 0.0007(11) 0.0015(11) 0.0006(12) C1 0.0266(19) 0.034(2) 0.0206(17) 0.0033(16) 0.0064(14) 0.0012(16) C2 0.031(3) 0.048(3) 0.0229(19) 0.0055(19) 0.0072(16) -0.0067(18) C3 0.040(3) 0.035(3) 0.0264(19) 0.0074(18) 0.0019(17) -0.0137(17) C4 0.028(2) 0.030(2) 0.0192(17) 0.0034(15) 0.0050(14) -0.0012(15) C5 0.044(3) 0.034(3) 0.0248(19) 0.0092(19) 0.0106(17) 0.0111(17) C6 0.050(3) 0.024(2) 0.033(2) 0.0022(18) 0.0136(19) 0.0096(17) C7 0.0221(19) 0.031(2) 0.0200(17) 0.0000(15) 0.0007(14) 0.0012(15) C8 0.025(2) 0.043(3) 0.0247(19) -0.0102(17) 0.0016(15) -0.0007(17) C9 0.039(3) 0.033(3) 0.0264(19) -0.0182(18) 0.0021(17) -0.0038(17) C10 0.0235(19) 0.0209(18) 0.0254(18) 0.0047(14) 0.0049(14) 0.0018(15) C11 0.021(3) 0.030(3) 0.028(3) 0.0000 0.001(2) 0.0000 C12 0.029(3) 0.021(3) 0.019(3) 0.0000 0.005(2) 0.0000 C13 0.045(8) 0.047(9) 0.188(17) 0.003(5) 0.007(9) 0.041(9) C14 0.056(8) 0.079(10) 0.091(10) -0.021(7) -0.015(8) 0.014(8) B1 0.044(3) 0.0150(19) 0.029(2) -0.0045(18) 0.0095(19) -0.0063(16) B2 0.027(4) 0.026(3) 0.027(3) 0.0000 0.004(3) 0.0000 #============================================================================== _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'Il Milione (Burla, et al., 2007)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # 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 Ru1 Ru1 3.1596(6) yes . 4_555 Ru1 Cl1 2.4473(11) yes . . Ru1 O1 1.992(3) yes . . Ru1 N2 2.021(4) yes . . Ru1 N4 2.008(3) yes . . Ru1 N6 2.067(3) yes . . Ru1 N8 2.035(3) yes . . Cl2 C13 1.814(14) yes . . Cl2 C13 1.814(14) yes . 4_545 Cl3 C13 2.004(14) yes . 4_545 Cl3 C14 1.832(16) yes . . F1 B2 1.383(8) yes . . F2 B2 1.390(8) yes . . F3 B2 1.379(5) yes . . O1 C12 1.410(7) yes . . N2 N3 1.362(5) yes . . N2 C1 1.344(6) yes . . N3 C3 1.353(6) yes . . N3 B1 1.540(7) yes . . N4 N5 1.358(5) yes . . N4 C4 1.347(5) yes . . N5 C6 1.339(6) yes . . N5 B1 1.554(6) yes . . N6 N7 1.356(5) yes . . N6 C7 1.333(5) yes . . N7 C9 1.347(6) yes . . N7 B1 1.535(6) yes . . N8 N8 1.375(4) yes . 4_555 N8 C10 1.339(5) yes . . C1 C2 1.387(7) yes . . C2 C3 1.375(7) yes . . C4 C5 1.389(6) yes . . C5 C6 1.367(6) yes . . C7 C8 1.391(6) yes . . C8 C9 1.364(7) yes . . C10 C11 1.387(5) yes . . C13 C13 0.785(18) yes . 4_545 C13 C14 1.39(2) yes . . C13 C14 0.92(2) yes . 4_545 C14 C14 1.36(3) yes . 4_545 C1 H2 0.950 no . . C2 H3 0.950 no . . C3 H4 0.950 no . . C4 H5 0.950 no . . C5 H6 0.950 no . . C6 H7 0.950 no . . C7 H8 0.950 no . . C8 H9 0.950 no . . C9 H10 0.950 no . . C10 H11 0.950 no . . C11 H12 0.950 no . . C12 H13 0.980 no . . C12 H13 0.980 no . 4_555 C12 H14 0.980 no . . C12 H14 0.980 no . 4_555 C12 H15 0.980 no . . C12 H15 0.980 no . 4_555 B1 H1 1.000 no . . H13 H14 0.884 no . 4_555 H13 H15 0.964 no . 4_555 H14 H14 0.964 no . 4_555 H15 H15 0.884 no . 4_555 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 Ru1 Ru1 Cl1 49.79(3) yes 4_555 . . Ru1 Ru1 O1 37.52(9) yes 4_555 . . Ru1 Ru1 N2 127.17(9) yes 4_555 . . Ru1 Ru1 N4 136.84(9) yes 4_555 . . Ru1 Ru1 N6 116.05(9) yes 4_555 . . Ru1 Ru1 N8 64.00(8) yes 4_555 . . Cl1 Ru1 O1 79.30(11) yes . . . Cl1 Ru1 N2 176.72(9) yes . . . Cl1 Ru1 N4 95.83(9) yes . . . Cl1 Ru1 N6 93.59(9) yes . . . Cl1 Ru1 N8 86.35(9) yes . . . O1 Ru1 N2 97.43(14) yes . . . O1 Ru1 N4 174.35(13) yes . . . O1 Ru1 N6 95.90(13) yes . . . O1 Ru1 N8 84.21(13) yes . . . N2 Ru1 N4 87.43(13) yes . . . N2 Ru1 N6 86.92(12) yes . . . N2 Ru1 N8 93.15(12) yes . . . N4 Ru1 N6 87.22(12) yes . . . N4 Ru1 N8 92.66(12) yes . . . N6 Ru1 N8 179.86(12) yes . . . Ru1 Cl1 Ru1 80.41(5) yes . . 4_555 C13 Cl2 C13 25.0(6) yes . . 4_545 C13 Cl3 C14 27.4(7) yes 4_545 . . Ru1 O1 Ru1 104.97(18) yes . . 4_555 Ru1 O1 C12 127.35(9) yes . . . Ru1 O1 C12 127.35(9) yes 4_555 . . Ru1 N2 N3 119.5(3) yes . . . Ru1 N2 C1 132.1(3) yes . . . N3 N2 C1 108.4(4) yes . . . N2 N3 C3 108.1(4) yes . . . N2 N3 B1 119.3(4) yes . . . C3 N3 B1 132.6(4) yes . . . Ru1 N4 N5 120.3(2) yes . . . Ru1 N4 C4 133.0(3) yes . . . N5 N4 C4 106.6(3) yes . . . N4 N5 C6 109.5(3) yes . . . N4 N5 B1 118.7(3) yes . . . C6 N5 B1 131.9(4) yes . . . Ru1 N6 N7 118.8(3) yes . . . Ru1 N6 C7 133.9(3) yes . . . N7 N6 C7 107.1(3) yes . . . N6 N7 C9 109.0(3) yes . . . N6 N7 B1 119.2(3) yes . . . C9 N7 B1 131.7(4) yes . . . Ru1 N8 N8 116.0(2) yes . . 4_555 Ru1 N8 C10 135.9(3) yes . . . N8 N8 C10 107.9(3) yes 4_555 . . N2 C1 C2 108.7(4) yes . . . C1 C2 C3 106.0(4) yes . . . N3 C3 C2 108.8(4) yes . . . N4 C4 C5 109.7(4) yes . . . C4 C5 C6 105.2(4) yes . . . N5 C6 C5 109.0(4) yes . . . N6 C7 C8 109.8(4) yes . . . C7 C8 C9 105.1(4) yes . . . N7 C9 C8 108.8(4) yes . . . N8 C10 C11 109.7(4) yes . . . C10 C11 C10 104.8(4) yes . . 4_555 Cl2 C13 Cl3 118.3(8) yes . . 4_545 Cl2 C13 C13 77.5(15) yes . . 4_545 Cl2 C13 C14 113.8(10) yes . . . Cl2 C13 C14 158(3) yes . . 4_545 Cl3 C13 C13 154(3) yes 4_545 . 4_545 Cl3 C13 C14 127.5(11) yes 4_545 . . Cl3 C13 C14 65.9(13) yes 4_545 . 4_545 C13 C13 C14 39.2(14) yes 4_545 . . C13 C13 C14 108(2) yes 4_545 . 4_545 C14 C13 C14 69.0(14) yes . . 4_545 Cl3 C14 C13 115.3(12) yes . . . Cl3 C14 C13 86.7(14) yes . . 4_545 Cl3 C14 C14 145.3(13) yes . . 4_545 C13 C14 C13 32.5(11) yes . . 4_545 C13 C14 C14 39.2(9) yes . . 4_545 C13 C14 C14 71.8(14) yes 4_545 . 4_545 N3 B1 N5 107.5(4) yes . . . N3 B1 N7 108.0(3) yes . . . N5 B1 N7 107.0(4) yes . . . F1 B2 F2 110.6(5) yes . . . F1 B2 F3 108.3(4) yes . . . F1 B2 F3 108.3(4) yes . . 4_555 F2 B2 F3 108.0(4) yes . . . F2 B2 F3 108.0(4) yes . . 4_555 F3 B2 F3 113.7(5) yes . . 4_555 N2 C1 H2 125.653 no . . . C2 C1 H2 125.649 no . . . C1 C2 H3 127.001 no . . . C3 C2 H3 127.005 no . . . N3 C3 H4 125.594 no . . . C2 C3 H4 125.600 no . . . N4 C4 H5 125.162 no . . . C5 C4 H5 125.161 no . . . C4 C5 H6 127.381 no . . . C6 C5 H6 127.381 no . . . N5 C6 H7 125.503 no . . . C5 C6 H7 125.506 no . . . N6 C7 H8 125.081 no . . . C8 C7 H8 125.082 no . . . C7 C8 H9 127.434 no . . . C9 C8 H9 127.427 no . . . N7 C9 H10 125.575 no . . . C8 C9 H10 125.578 no . . . N8 C10 H11 125.161 no . . . C11 C10 H11 125.165 no . . . C10 C11 H12 127.576 no . . . C10 C11 H12 127.576 no 4_555 . . O1 C12 H13 109.473 no . . . O1 C12 H13 109.473 no . . 4_555 O1 C12 H14 109.479 no . . . O1 C12 H14 109.479 no . . 4_555 O1 C12 H15 109.466 no . . . O1 C12 H15 109.466 no . . 4_555 H13 C12 H13 140.956 no . . 4_555 H13 C12 H14 109.489 no . . . H13 C12 H14 53.604 no . . 4_555 H13 C12 H15 109.454 no . . . H13 C12 H15 58.888 no . . 4_555 H13 C12 H14 53.604 no 4_555 . . H13 C12 H14 109.489 no 4_555 . 4_555 H13 C12 H15 58.888 no 4_555 . . H13 C12 H15 109.454 no 4_555 . 4_555 H14 C12 H14 58.914 no . . 4_555 H14 C12 H15 109.466 no . . . H14 C12 H15 140.952 no . . 4_555 H14 C12 H15 140.952 no 4_555 . . H14 C12 H15 109.466 no 4_555 . 4_555 H15 C12 H15 53.589 no . . 4_555 N3 B1 H1 111.373 no . . . N5 B1 H1 111.372 no . . . N7 B1 H1 111.367 no . . . C12 H13 H14 63.181 no . . 4_555 C12 H13 H15 60.568 no . . 4_555 H14 H13 H15 119.996 no 4_555 . 4_555 C12 H14 H13 63.216 no . . 4_555 C12 H14 H14 60.543 no . . 4_555 H13 H14 H14 120.004 no 4_555 . 4_555 C12 H15 H13 60.545 no . . 4_555 C12 H15 H15 63.205 no . . 4_555 H13 H15 H15 119.999 no 4_555 . 4_555 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 Ru1 Ru1 Cl1 Ru1 0.0 no 4_555 . . 4_555 Cl1 Ru1 Ru1 Cl1 0.00(4) no . . 4_555 . Cl1 Ru1 Ru1 O1 -134.56(4) no . . 4_555 . Cl1 Ru1 Ru1 N2 -178.42(4) no . . 4_555 4_555 Cl1 Ru1 Ru1 N4 45.02(4) no . . 4_555 4_555 Cl1 Ru1 Ru1 N6 -71.22(4) no . . 4_555 4_555 Cl1 Ru1 Ru1 N8 108.63(4) no . . 4_555 4_555 Ru1 Ru1 O1 Ru1 0.0 no 4_555 . . 4_555 Ru1 Ru1 O1 C12 -173.7(5) no 4_555 . . . O1 Ru1 Ru1 Cl1 134.56(19) no . . 4_555 . O1 Ru1 Ru1 O1 0.00(19) no . . 4_555 . O1 Ru1 Ru1 N2 -43.86(19) no . . 4_555 4_555 O1 Ru1 Ru1 N4 179.58(19) no . . 4_555 4_555 O1 Ru1 Ru1 N6 63.33(19) no . . 4_555 4_555 O1 Ru1 Ru1 N8 -116.81(19) no . . 4_555 4_555 Ru1 Ru1 N2 N3 -164.59(13) no 4_555 . . . Ru1 Ru1 N2 C1 14.9(3) no 4_555 . . . N2 Ru1 Ru1 Cl1 178.42(10) no . . 4_555 . N2 Ru1 Ru1 O1 43.86(10) no . . 4_555 . N2 Ru1 Ru1 N2 0.00(11) no . . 4_555 4_555 N2 Ru1 Ru1 N4 -136.56(10) no . . 4_555 4_555 N2 Ru1 Ru1 N6 107.19(10) no . . 4_555 4_555 N2 Ru1 Ru1 N8 -72.95(10) no . . 4_555 4_555 Ru1 Ru1 N4 N5 168.81(12) no 4_555 . . . Ru1 Ru1 N4 C4 -7.6(4) no 4_555 . . . N4 Ru1 Ru1 Cl1 -45.02(13) no . . 4_555 . N4 Ru1 Ru1 O1 -179.58(13) no . . 4_555 . N4 Ru1 Ru1 N2 136.56(13) no . . 4_555 4_555 N4 Ru1 Ru1 N4 0.00(14) no . . 4_555 4_555 N4 Ru1 Ru1 N6 -116.25(13) no . . 4_555 4_555 N4 Ru1 Ru1 N8 63.61(13) no . . 4_555 4_555 Ru1 Ru1 N6 N7 174.77(14) no 4_555 . . . Ru1 Ru1 N6 C7 -9.3(3) no 4_555 . . . N6 Ru1 Ru1 Cl1 71.22(9) no . . 4_555 . N6 Ru1 Ru1 O1 -63.33(9) no . . 4_555 . N6 Ru1 Ru1 N2 -107.19(9) no . . 4_555 4_555 N6 Ru1 Ru1 N4 116.25(9) no . . 4_555 4_555 N6 Ru1 Ru1 N6 0.00(9) no . . 4_555 4_555 N6 Ru1 Ru1 N8 179.86(9) no . . 4_555 4_555 Ru1 Ru1 N8 N8 0.00(14) no 4_555 . . 4_555 Ru1 Ru1 N8 C10 -174.8(3) no 4_555 . . . N8 Ru1 Ru1 Cl1 -108.63(10) no . . 4_555 . N8 Ru1 Ru1 O1 116.81(10) no . . 4_555 . N8 Ru1 Ru1 N2 72.95(10) no . . 4_555 4_555 N8 Ru1 Ru1 N4 -63.61(10) no . . 4_555 4_555 N8 Ru1 Ru1 N6 -179.86(10) no . . 4_555 4_555 N8 Ru1 Ru1 N8 0.00(10) no . . 4_555 4_555 Cl1 Ru1 O1 Ru1 33.63(14) no . . . 4_555 Cl1 Ru1 O1 C12 -140.1(3) no . . . . O1 Ru1 Cl1 Ru1 -26.21(10) no . . . 4_555 Cl1 Ru1 N4 N5 135.9(2) no . . . . Cl1 Ru1 N4 C4 -40.4(3) no . . . . N4 Ru1 Cl1 Ru1 150.89(9) no . . . 4_555 Cl1 Ru1 N6 N7 -138.80(18) no . . . . Cl1 Ru1 N6 C7 37.1(3) no . . . . N6 Ru1 Cl1 Ru1 -121.54(9) no . . . 4_555 Cl1 Ru1 N8 N8 -46.48(18) no . . . 4_555 Cl1 Ru1 N8 C10 138.7(3) no . . . . N8 Ru1 Cl1 Ru1 58.59(8) no . . . 4_555 O1 Ru1 N2 N3 -139.4(2) no . . . . O1 Ru1 N2 C1 40.1(3) no . . . . N2 Ru1 O1 Ru1 -146.17(16) no . . . 4_555 N2 Ru1 O1 C12 40.1(3) no . . . . O1 Ru1 N6 N7 141.6(2) no . . . . O1 Ru1 N6 C7 -42.5(3) no . . . . N6 Ru1 O1 Ru1 126.18(16) no . . . 4_555 N6 Ru1 O1 C12 -47.6(3) no . . . . O1 Ru1 N8 N8 33.1(2) no . . . 4_555 O1 Ru1 N8 C10 -141.7(3) no . . . . N8 Ru1 O1 Ru1 -53.74(17) no . . . 4_555 N8 Ru1 O1 C12 132.5(3) no . . . . N2 Ru1 N4 N5 -44.4(3) no . . . . N2 Ru1 N4 C4 139.2(3) no . . . . N4 Ru1 N2 N3 43.5(2) no . . . . N4 Ru1 N2 C1 -137.0(3) no . . . . N2 Ru1 N6 N7 44.4(2) no . . . . N2 Ru1 N6 C7 -139.6(3) no . . . . N6 Ru1 N2 N3 -43.85(19) no . . . . N6 Ru1 N2 C1 135.7(3) no . . . . N2 Ru1 N8 N8 130.3(2) no . . . 4_555 N2 Ru1 N8 C10 -44.6(3) no . . . . N8 Ru1 N2 N3 136.03(19) no . . . . N8 Ru1 N2 C1 -44.5(3) no . . . . N4 Ru1 N6 N7 -43.1(2) no . . . . N4 Ru1 N6 C7 132.8(3) no . . . . N6 Ru1 N4 N5 42.6(3) no . . . . N6 Ru1 N4 C4 -133.8(3) no . . . . N4 Ru1 N8 N8 -142.2(2) no . . . 4_555 N4 Ru1 N8 C10 43.0(3) no . . . . N8 Ru1 N4 N5 -137.5(3) no . . . . N8 Ru1 N4 C4 46.2(3) no . . . . C13 Cl2 C13 Cl3 -157(3) no . . 4_545 . C13 Cl2 C13 C13 0.0(16) no . . 4_545 . C13 Cl2 C13 C14 15.3(16) no . . 4_545 4_545 C13 Cl2 C13 C14 108(5) no . . 4_545 . C13 Cl2 C13 Cl3 157(3) no 4_545 . . 4_545 C13 Cl2 C13 C13 0.0(16) no 4_545 . . 4_545 C13 Cl2 C13 C14 -15.3(16) no 4_545 . . . C13 Cl2 C13 C14 -108(5) no 4_545 . . 4_545 C13 Cl3 C14 C13 -16.0(12) no 4_545 . . . C13 Cl3 C14 C13 0.0(12) no 4_545 . . 4_545 C13 Cl3 C14 C14 -50.7(18) no 4_545 . . 4_545 C14 Cl3 C13 Cl2 -155(3) no . . 4_545 . C14 Cl3 C13 C13 82(4) no . . 4_545 . C14 Cl3 C13 C14 33.0(13) no . . 4_545 4_545 C14 Cl3 C13 C14 0.0(11) no . . 4_545 . Ru1 N2 N3 C3 -179.98(16) no . . . . Ru1 N2 N3 B1 0.4(4) no . . . . Ru1 N2 C1 C2 -179.60(19) no . . . . N3 N2 C1 C2 -0.1(4) no . . . . C1 N2 N3 C3 0.4(4) no . . . . C1 N2 N3 B1 -179.2(3) no . . . . N2 N3 C3 C2 -0.6(4) no . . . . N2 N3 B1 N5 -57.2(4) no . . . . N2 N3 B1 N7 58.0(4) no . . . . C3 N3 B1 N5 123.3(4) no . . . . C3 N3 B1 N7 -121.6(4) no . . . . B1 N3 C3 C2 179.0(4) no . . . . Ru1 N4 N5 C6 -177.26(18) no . . . . Ru1 N4 N5 B1 1.4(4) no . . . . Ru1 N4 C4 C5 176.9(3) no . . . . N5 N4 C4 C5 0.2(4) no . . . . C4 N4 N5 C6 -0.0(4) no . . . . C4 N4 N5 B1 178.7(3) no . . . . N4 N5 C6 C5 -0.1(5) no . . . . N4 N5 B1 N3 56.2(5) no . . . . N4 N5 B1 N7 -59.6(5) no . . . . C6 N5 B1 N3 -125.4(5) no . . . . C6 N5 B1 N7 118.7(5) no . . . . B1 N5 C6 C5 -178.6(4) no . . . . Ru1 N6 N7 C9 176.86(16) no . . . . Ru1 N6 N7 B1 -1.0(4) no . . . . Ru1 N6 C7 C8 -176.2(2) no . . . . N7 N6 C7 C8 0.1(4) no . . . . C7 N6 N7 C9 -0.1(4) no . . . . C7 N6 N7 B1 -177.9(3) no . . . . N6 N7 C9 C8 0.0(4) no . . . . N6 N7 B1 N3 -56.9(4) no . . . . N6 N7 B1 N5 58.6(4) no . . . . C9 N7 B1 N3 125.8(4) no . . . . C9 N7 B1 N5 -118.7(4) no . . . . B1 N7 C9 C8 177.5(4) no . . . . Ru1 N8 N8 Ru1 0.0(3) no . . 4_555 4_555 Ru1 N8 N8 C10 -176.24(16) no . . 4_555 4_555 Ru1 N8 C10 C11 175.4(3) no . . . . N8 N8 C10 C11 0.3(4) no 4_555 . . . C10 N8 N8 Ru1 176.2(3) no . . 4_555 4_555 C10 N8 N8 C10 0.0(4) no . . 4_555 4_555 N2 C1 C2 C3 -0.3(4) no . . . . C1 C2 C3 N3 0.6(4) no . . . . N4 C4 C5 C6 -0.2(5) no . . . . C4 C5 C6 N5 0.2(5) no . . . . N6 C7 C8 C9 -0.1(4) no . . . . C7 C8 C9 N7 0.0(5) no . . . . N8 C10 C11 C10 -0.5(5) no . . . 4_555 Cl2 C13 C13 Cl2 0.00(7) no . . 4_545 . Cl2 C13 C13 Cl3 130(5) no . . 4_545 . Cl2 C13 C13 C14 -158(3) no . . 4_545 4_545 Cl2 C13 C13 C14 -158(3) no . . 4_545 . Cl2 C13 C14 Cl3 54.9(18) no . . . . Cl2 C13 C14 C13 24.1(12) no . . . 4_545 Cl2 C13 C14 C14 -156(2) no . . . 4_545 Cl2 C13 C14 Cl3 -106(4) no . . 4_545 4_545 Cl2 C13 C14 C13 102(5) no . . 4_545 4_545 Cl2 C13 C14 C14 102(4) no . . 4_545 . Cl3 C13 C13 Cl2 -130(5) no 4_545 . 4_545 . Cl3 C13 C13 Cl3 0(9) no 4_545 . 4_545 . Cl3 C13 C13 C14 72(4) no 4_545 . 4_545 4_545 Cl3 C13 C13 C14 72(6) no 4_545 . 4_545 . Cl3 C13 C14 Cl3 -117.0(14) no 4_545 . . . Cl3 C13 C14 C13 -148(3) no 4_545 . . 4_545 Cl3 C13 C14 C14 32.2(10) no 4_545 . . 4_545 Cl3 C13 C14 Cl3 0.00(8) no 4_545 . 4_545 4_545 Cl3 C13 C14 C13 -152(2) no 4_545 . 4_545 4_545 Cl3 C13 C14 C14 -152.4(10) no 4_545 . 4_545 . C13 C13 C14 Cl3 31(3) no 4_545 . . . C13 C13 C14 C13 0(3) no 4_545 . . 4_545 C14 C13 C13 Cl2 158(3) no . . 4_545 . C14 C13 C13 Cl3 -72(4) no . . 4_545 . C14 C13 C13 C14 0(4) no . . 4_545 4_545 C14 C13 C13 C14 0.0(11) no . . 4_545 . C13 C13 C14 Cl3 152(3) no 4_545 . 4_545 4_545 C13 C13 C14 C13 0.0(16) no 4_545 . 4_545 4_545 C13 C13 C14 C14 0(3) no 4_545 . 4_545 . C14 C13 C13 Cl2 158(3) no 4_545 . 4_545 . C14 C13 C13 Cl3 -72(6) no 4_545 . 4_545 . C14 C13 C13 C14 0.0(11) no 4_545 . 4_545 4_545 C14 C13 C13 C14 0(4) no 4_545 . 4_545 . C14 C13 C14 Cl3 152.4(12) no . . 4_545 4_545 C14 C13 C14 C13 0.0(19) no . . 4_545 4_545 C14 C13 C14 C14 0.0(8) no . . 4_545 . C14 C13 C14 Cl3 -149.2(18) no 4_545 . . . C14 C13 C14 C14 0.0(11) no 4_545 . . 4_545 Cl3 C14 C14 Cl3 0(4) no . . 4_545 4_545 Cl3 C14 C14 C13 54.4(17) no . . 4_545 4_545 Cl3 C14 C14 C13 54(3) no . . 4_545 . C13 C14 C14 Cl3 -54(3) no . . 4_545 4_545 C13 C14 C14 C13 0.0(16) no . . 4_545 4_545 C13 C14 C14 C13 0.0(14) no . . 4_545 . C13 C14 C14 Cl3 -54(3) no 4_545 . 4_545 4_545 C13 C14 C14 C13 0.0(14) no 4_545 . 4_545 4_545 C13 C14 C14 C13 0.0(16) no 4_545 . 4_545 . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Ru1 B1 3.138(5) no . . Cl1 N4 3.320(3) no . 4_555 Cl1 N6 3.301(3) no . 4_555 Cl1 N8 3.082(4) no . 4_555 Cl2 Cl3 3.279(3) no . . O1 N2 3.015(4) no . 4_555 O1 N6 3.014(4) no . 4_555 O1 N8 2.700(5) no . 4_555 O1 C1 3.463(5) no . . O1 C1 3.463(5) no . 4_555 O1 C7 3.502(5) no . . O1 C7 3.502(5) no . 4_555 N2 N5 2.973(5) no . . N2 N7 2.981(5) no . . N2 C10 3.454(5) no . . N2 C12 3.391(4) no . . N3 N4 2.958(5) no . . N3 N6 2.966(5) no . . N4 N7 2.973(4) no . . N4 C10 3.423(5) no . . N5 N6 2.966(4) no . . N6 C12 3.426(5) no . . N7 C6 3.597(5) no . . N8 C1 3.382(5) no . . N8 C4 3.385(5) no . . C1 C12 3.540(6) no . . Cl1 C6 3.540(5) no . 2_657 Cl1 C6 3.540(5) no . 3_657 Cl3 N3 3.563(4) no . 4_445 Cl3 N5 3.381(4) no . 4_445 Cl3 C6 3.386(6) no . 4_445 F1 C3 3.260(6) no . 2_756 F1 C3 3.260(6) no . 3_756 F1 C12 3.254(7) no . 1_655 F1 C14 3.514(16) no . 2_656 F1 C14 3.514(16) no . 3_656 F2 C1 3.394(5) no . . F2 C1 3.394(5) no . 4_555 F2 C7 3.324(5) no . 1_655 F2 C7 3.324(5) no . 4_655 F2 C8 3.582(5) no . 1_655 F2 C8 3.582(5) no . 4_655 F3 C1 3.315(6) no . . F3 C2 3.502(6) no . . F3 C2 3.491(6) no . 3_756 F3 C9 3.128(6) no . 3_656 F3 C14 3.451(17) no . 2_656 N3 Cl3 3.563(4) no . 4_645 N4 C5 3.571(6) no . 3_657 N5 Cl3 3.381(4) no . 4_645 N6 C5 3.569(6) no . 3_657 C1 F2 3.394(5) no . . C1 F3 3.315(6) no . . C2 F3 3.502(6) no . . C2 F3 3.491(6) no . 3_756 C2 C8 3.567(6) no . 3_656 C2 C9 3.566(6) no . 3_656 C3 F1 3.260(6) no . 2_746 C3 C14 3.384(15) no . 4_645 C4 C6 3.532(7) no . 3_657 C5 N4 3.571(6) no . 3_657 C5 N6 3.569(6) no . 3_657 C6 Cl1 3.540(5) no . 2_647 C6 Cl3 3.386(6) no . 4_645 C6 C4 3.532(7) no . 3_657 C7 F2 3.324(5) no . 1_455 C8 F2 3.582(5) no . 1_455 C8 C2 3.567(6) no . 3_656 C9 F3 3.128(6) no . 3_656 C9 C2 3.566(6) no . 3_656 C12 F1 3.254(7) no . 1_455 C14 F1 3.514(16) no . 2_646 C14 F3 3.451(17) no . 2_646 C14 C3 3.384(15) no . 4_445 Ru1 H2 3.3330 no . . Ru1 H5 3.3366 no . . Ru1 H8 3.3898 no . . Ru1 H11 3.4105 no . . Ru1 H13 3.0200 no . . Ru1 H14 3.2676 no . 4_555 Ru1 H15 3.2353 no . 4_555 Cl1 H5 3.3945 no . . Cl1 H5 3.3945 no . 4_555 Cl1 H8 3.3357 no . . Cl1 H8 3.3357 no . 4_555 O1 H2 3.2671 no . . O1 H2 3.2671 no . 4_555 O1 H8 3.3076 no . . O1 H8 3.3076 no . 4_555 N2 H1 3.3307 no . . N2 H3 3.1365 no . . N2 H4 3.1135 no . . N2 H11 3.3396 no . . N2 H13 2.8729 no . . N2 H14 3.0056 no . 4_555 N2 H15 3.5778 no . 4_555 N3 H2 3.1103 no . . N3 H3 3.1361 no . . N4 H1 3.3327 no . . N4 H6 3.1533 no . . N4 H7 3.1160 no . . N4 H11 3.2475 no . . N5 H5 3.0864 no . . N5 H6 3.1217 no . . N6 H1 3.3210 no . . N6 H9 3.1454 no . . N6 H10 3.1147 no . . N6 H13 3.0415 no . . N6 H15 2.9720 no . 4_555 N7 H8 3.0806 no . . N7 H9 3.1249 no . . N8 H2 3.2029 no . . N8 H5 3.2060 no . . N8 H11 3.1111 no . 4_555 N8 H12 3.1463 no . . C1 H4 3.1260 no . . C1 H11 3.5076 no . . C1 H13 3.0352 no . . C1 H14 2.8353 no . 4_555 C3 H1 2.8206 no . . C3 H2 3.1249 no . . C4 H7 3.1115 no . . C4 H11 3.3877 no . . C6 H1 2.8129 no . . C6 H5 3.1078 no . . C7 H8 3.1830 no . 4_555 C7 H10 3.1102 no . . C7 H13 3.3890 no . . C7 H15 3.5128 no . . C7 H15 2.9547 no . 4_555 C9 H1 2.7966 no . . C9 H8 3.1055 no . . C10 H2 3.4150 no . . C10 H5 3.3968 no . . C10 H11 3.1183 no . 4_555 C11 H11 2.0842 no . 4_555 C12 H2 3.3203 no . . C12 H2 3.3203 no . 4_555 C12 H8 3.4627 no . . C12 H8 3.4627 no . 4_555 B1 H4 2.9699 no . . B1 H7 2.9527 no . . B1 H10 2.9445 no . . H1 H4 2.8077 no . . H1 H7 2.7875 no . . H1 H10 2.7738 no . . H2 H2 3.4843 no . 4_555 H2 H3 2.5125 no . . H2 H11 3.4923 no . . H2 H13 3.0308 no . . H2 H14 3.1538 no . . H2 H14 2.5669 no . 4_555 H3 H4 2.4998 no . . H5 H6 2.5129 no . . H5 H11 3.3487 no . . H6 H7 2.4952 no . . H8 H8 2.2596 no . 4_555 H8 H9 2.5142 no . . H8 H13 3.4217 no . . H8 H15 3.1041 no . . H8 H15 2.7638 no . 4_555 H9 H10 2.4945 no . . H11 H12 2.5136 no . . Cl1 H6 3.4633 no . 2_657 Cl1 H6 3.4633 no . 3_657 Cl1 H7 2.9599 no . 2_657 Cl1 H7 2.9599 no . 3_657 Cl1 H12 3.4705 no . 1_455 Cl2 H5 2.8495 no . 2_647 Cl2 H5 2.8495 no . 3_657 Cl2 H10 3.0831 no . . Cl2 H10 3.0831 no . 4_545 Cl3 H5 3.0553 no . 2_647 Cl3 H9 3.4800 no . 4_545 Cl3 H11 3.1174 no . 4_445 F1 H3 3.4039 no . 2_756 F1 H3 3.4039 no . 3_756 F1 H4 2.4948 no . 2_756 F1 H4 2.4948 no . 3_756 F1 H8 3.1785 no . 1_655 F1 H8 3.1785 no . 4_655 F1 H13 3.2336 no . 1_655 F1 H13 3.2336 no . 4_655 F1 H15 2.4501 no . 1_655 F1 H15 2.4501 no . 4_655 F2 H2 2.4838 no . . F2 H2 2.4838 no . 4_555 F2 H8 2.6652 no . 1_655 F2 H8 2.6652 no . 4_655 F2 H9 3.2434 no . 1_655 F2 H9 3.2434 no . 4_655 F3 H2 2.6633 no . . F3 H3 3.0847 no . . F3 H3 2.9505 no . 3_756 F3 H4 3.4929 no . 3_756 F3 H9 3.4764 no . 1_655 F3 H9 3.4772 no . 3_656 F3 H10 2.4082 no . 3_656 N4 H6 3.5365 no . 3_657 N6 H6 2.8350 no . 3_657 N7 H3 3.5961 no . 3_656 N7 H6 3.1390 no . 3_657 C1 H9 2.7404 no . 1_655 C2 H9 2.7422 no . 1_655 C3 H13 3.1389 no . 3_656 C3 H15 3.2852 no . 2_646 C5 H11 3.3760 no . 3_757 C5 H12 3.4522 no . 2_747 C6 H5 3.5386 no . 3_657 C6 H7 3.4546 no . 4_545 C6 H12 3.5227 no . 2_747 C7 H3 3.3387 no . 3_656 C7 H6 2.7118 no . 3_657 C8 H2 3.5546 no . 1_455 C8 H3 3.4873 no . 1_455 C8 H3 2.7521 no . 3_656 C8 H6 2.9828 no . 3_657 C8 H11 3.4478 no . 1_455 C9 H3 2.9596 no . 3_656 C9 H6 3.2212 no . 3_657 C10 H6 3.4585 no . 3_757 C10 H9 3.5806 no . 1_655 C11 H6 3.4885 no . 2_757 C11 H6 3.4885 no . 3_757 C11 H8 3.3776 no . 1_655 C11 H8 3.3776 no . 4_655 C12 H4 3.2114 no . 2_656 C12 H4 3.2114 no . 3_656 C13 H5 3.4072 no . 3_657 C13 H10 3.2704 no . . C14 H4 3.1556 no . 4_445 C14 H10 3.4284 no . 4_545 B2 H2 3.1059 no . . B2 H2 3.1059 no . 4_555 B2 H4 3.5557 no . 2_756 B2 H4 3.5557 no . 3_756 B2 H8 3.4156 no . 1_655 B2 H8 3.4156 no . 4_655 H1 H1 3.3715 no . 4_545 H2 F2 2.4838 no . . H2 F3 2.6633 no . . H2 C8 3.5546 no . 1_655 H2 B2 3.1059 no . . H2 H9 2.6903 no . 1_655 H3 F1 3.4039 no . 2_746 H3 F3 3.0847 no . . H3 F3 2.9505 no . 3_756 H3 N7 3.5961 no . 3_656 H3 C7 3.3387 no . 3_656 H3 C8 3.4873 no . 1_655 H3 C8 2.7521 no . 3_656 H3 C9 2.9596 no . 3_656 H3 H3 3.0531 no . 3_756 H3 H9 2.7081 no . 1_655 H3 H9 2.8184 no . 3_656 H3 H10 3.1710 no . 3_656 H4 F1 2.4948 no . 2_746 H4 F3 3.4929 no . 3_756 H4 C12 3.2114 no . 2_646 H4 C14 3.1556 no . 4_645 H4 B2 3.5557 no . 2_746 H4 H4 3.3551 no . 4_545 H4 H13 3.5694 no . 2_646 H4 H13 2.5578 no . 3_656 H4 H14 3.0812 no . 2_646 H4 H14 3.5675 no . 3_656 H4 H15 2.5607 no . 2_646 H4 H15 3.0858 no . 3_656 H5 Cl2 2.8495 no . 2_657 H5 Cl3 3.0553 no . 2_657 H5 C6 3.5386 no . 3_657 H5 C13 3.4072 no . 3_657 H5 H7 3.5473 no . 3_657 H6 Cl1 3.4633 no . 2_647 H6 N4 3.5365 no . 3_657 H6 N6 2.8350 no . 3_657 H6 N7 3.1390 no . 3_657 H6 C7 2.7118 no . 3_657 H6 C8 2.9828 no . 3_657 H6 C9 3.2212 no . 3_657 H6 C10 3.4585 no . 3_757 H6 C11 3.4885 no . 2_747 H6 H8 3.0277 no . 3_657 H6 H9 3.4602 no . 3_657 H6 H11 2.8749 no . 3_757 H6 H12 2.9751 no . 2_747 H7 Cl1 2.9599 no . 2_647 H7 C6 3.4546 no . 4_545 H7 H5 3.5473 no . 3_657 H7 H7 2.5122 no . 4_545 H7 H12 3.1002 no . 2_747 H8 F1 3.1785 no . 1_455 H8 F2 2.6652 no . 1_455 H8 C11 3.3776 no . 1_455 H8 B2 3.4156 no . 1_455 H8 H6 3.0277 no . 3_657 H8 H12 3.0513 no . 1_455 H9 Cl3 3.4800 no . 4_545 H9 F2 3.2434 no . 1_455 H9 F3 3.4764 no . 1_455 H9 F3 3.4772 no . 3_656 H9 C1 2.7404 no . 1_455 H9 C2 2.7422 no . 1_455 H9 C10 3.5806 no . 1_455 H9 H2 2.6903 no . 1_455 H9 H3 2.7081 no . 1_455 H9 H3 2.8184 no . 3_656 H9 H6 3.4602 no . 3_657 H9 H11 3.1009 no . 1_455 H10 Cl2 3.0831 no . . H10 F3 2.4082 no . 3_656 H10 C13 3.2704 no . . H10 C14 3.4284 no . 4_545 H10 H3 3.1710 no . 3_656 H11 Cl3 3.1174 no . 4_645 H11 C5 3.3760 no . 3_757 H11 C8 3.4478 no . 1_655 H11 H6 2.8749 no . 3_757 H11 H9 3.1009 no . 1_655 H12 Cl1 3.4705 no . 1_655 H12 C5 3.4522 no . 2_757 H12 C5 3.4522 no . 3_757 H12 C6 3.5227 no . 2_757 H12 C6 3.5227 no . 3_757 H12 H6 2.9751 no . 2_757 H12 H6 2.9751 no . 3_757 H12 H7 3.1002 no . 2_757 H12 H7 3.1002 no . 3_757 H12 H8 3.0513 no . 1_655 H12 H8 3.0513 no . 4_655 H13 F1 3.2336 no . 1_455 H13 C3 3.1389 no . 3_656 H13 H4 3.5694 no . 2_656 H13 H4 2.5578 no . 3_656 H14 H4 3.0812 no . 2_656 H14 H4 3.5675 no . 3_656 H15 F1 2.4501 no . 1_455 H15 C3 3.2852 no . 2_656 H15 H4 2.5607 no . 2_656 H15 H4 3.0858 no . 3_656 #============================================================================== #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== _database_code_depnum_ccdc_archive 'CCDC 939834' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1014a #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C24 H31 B4 Cl7 F8 N15 O2 Ru2' _chemical_formula_moiety 'C24 H31 B4 Cl7 F8 N15 O2 Ru2' _chemical_formula_weight 1207.15 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 +X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 11.2451(15) _cell_length_b 11.8268(15) _cell_length_c 33.225(5) _cell_angle_alpha 90.0000 _cell_angle_beta 98.519(3) _cell_angle_gamma 90.0000 _cell_volume 4369.9(10) _cell_formula_units_Z 4 _cell_measurement_reflns_used 12449 _cell_measurement_theta_min 3.02 _cell_measurement_theta_max 27.49 _cell_measurement_temperature 93 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour darkPurple _exptl_crystal_size_max 0.230 _exptl_crystal_size_mid 0.210 _exptl_crystal_size_min 0.130 _exptl_crystal_density_diffrn 1.835 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2380.00 _exptl_absorpt_coefficient_mu 1.200 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_correction_T_min 0.726 _exptl_absorpt_correction_T_max 0.856 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 93 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku Saturn724+' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.111 _diffrn_reflns_number 32374 _diffrn_reflns_av_R_equivalents 0.0297 _diffrn_reflns_theta_max 27.47 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 43 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # 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 9940 _reflns_number_gt 8449 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0571 _refine_ls_wR_factor_ref 0.1521 _refine_ls_number_restraints 155 _refine_ls_hydrogen_treatment mixed _refine_ls_number_reflns 9940 _refine_ls_number_parameters 563 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0722P)^2^+22.3630P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.001 _refine_diff_density_max 2.060 _refine_diff_density_min -1.450 _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 0.0033 0.0016 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.0061 0.0033 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; B B 0.0013 0.0007 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.1484 0.1585 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; F F 0.0171 0.0103 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.0106 0.0060 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ru Ru -1.2594 0.8363 ; 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 Ru1 Ru 0.16800(3) 0.89034(3) 0.856153(11) 0.01991(11) Uani 1.0 4 d . . . Ru2 Ru 0.44093(3) 0.76365(3) 0.918274(11) 0.01994(11) Uani 1.0 4 d . . . Cl1 Cl 0.25989(9) 0.86340(9) 0.92472(3) 0.0217(3) Uani 1.0 4 d . . . Cl2 Cl -0.2325(2) 0.72140(18) 0.72224(6) 0.0652(6) Uani 1.0 4 d . . . Cl3 Cl -0.1732(3) 0.7169(3) 0.81029(6) 0.0848(8) Uani 1.0 4 d . . . Cl4 Cl 0.5549(3) 0.2613(3) 0.86361(7) 0.0897(9) Uani 1.0 4 d . . . Cl5 Cl 0.6823(2) 0.3910(2) 0.80906(6) 0.0701(6) Uani 1.0 4 d . . . Cl6 Cl 0.0211(3) 0.8599(4) 1.01224(12) 0.1352(17) Uani 1.0 4 d . . . Cl7 Cl 0.16257(15) 0.74396(15) 1.07952(6) 0.0506(4) Uani 1.0 4 d . . . F1 F 0.0261(4) 0.4688(4) 0.89465(12) 0.0690(13) Uiso 1.0 4 d . . . F2 F 0.0730(6) 0.4724(6) 0.96328(13) 0.094(3) Uiso 0.7000 4 d . . . F3 F 0.2206(3) 0.4856(4) 0.92380(14) 0.0381(11) Uiso 0.7000 4 d . . . F4 F 0.0928(5) 0.6321(3) 0.92691(16) 0.0526(15) Uiso 0.7000 4 d . . . F5 F 0.2809(3) 0.6739(3) 0.78404(11) 0.0492(9) Uiso 1.0 4 d . . . F6 F 0.4747(4) 0.6517(4) 0.77241(17) 0.0623(17) Uiso 0.7000 4 d . . . F7 F 0.3355(4) 0.5140(4) 0.75428(13) 0.0450(13) Uiso 0.7000 4 d . . . F8 F 0.4017(5) 0.5479(4) 0.82089(10) 0.0529(15) Uiso 0.7000 4 d . . . F9 F 0.2028(8) 0.4476(9) 0.9376(4) 0.068(5) Uiso 0.3000 4 d . . . F10 F 0.0420(10) 0.5215(13) 0.9608(2) 0.206(18) Uiso 0.3000 4 d . . . F11 F 0.1333(11) 0.6244(5) 0.9167(3) 0.057(4) Uiso 0.3000 4 d . . . F13 F 0.4424(8) 0.5881(9) 0.82085(16) 0.060(4) Uiso 0.3000 4 d . . . F14 F 0.3301(7) 0.4925(4) 0.7693(4) 0.059(4) Uiso 0.3000 4 d . . . F15 F 0.4476(7) 0.6389(7) 0.7555(3) 0.059(4) Uiso 0.3000 4 d . . . O1 O 0.1023(5) 0.6556(4) 0.83700(16) 0.0269(11) Uani 0.7000 4 d . . . O2 O 0.3384(6) 0.6387(6) 0.8881(2) 0.0256(13) Uani 0.7000 4 d . . . O3 O 0.3470(12) 0.5408(11) 0.8838(4) 0.033(3) Uiso 0.3000 4 d . . . O4 O 0.1689(16) 0.7238(16) 0.8456(6) 0.032(6) Uiso 0.3000 4 d . . . N1 N 0.1363(7) 0.7441(7) 0.8457(3) 0.0223(16) Uani 0.7000 4 d . . . N2 N 0.0896(4) 0.9260(4) 0.79774(13) 0.0267(9) Uani 1.0 4 d . . . N3 N -0.0004(4) 1.0049(4) 0.79177(14) 0.0286(9) Uani 1.0 4 d . . . N4 N 0.1742(4) 1.0635(4) 0.86396(14) 0.0276(9) Uani 1.0 4 d . . . N5 N 0.0749(4) 1.1272(4) 0.85064(13) 0.0265(9) Uani 1.0 4 d . . . N6 N 0.0006(4) 0.9033(4) 0.87416(13) 0.0252(9) Uani 1.0 4 d . . . N7 N -0.0789(4) 0.9841(4) 0.85742(14) 0.0285(9) Uani 1.0 4 d . . . N8 N 0.5997(4) 0.6809(4) 0.91565(12) 0.0233(8) Uani 1.0 4 d . . . N9 N 0.6851(4) 0.6773(4) 0.95008(13) 0.0243(9) Uani 1.0 4 d . . . N10 N 0.5446(4) 0.8889(4) 0.94724(12) 0.0207(8) Uani 1.0 4 d . . . N11 N 0.6339(4) 0.8623(4) 0.97803(12) 0.0211(8) Uani 1.0 4 d . . . N12 N 0.4418(4) 0.6935(4) 0.97485(12) 0.0209(8) Uani 1.0 4 d . . . N13 N 0.5462(4) 0.6861(4) 1.00116(12) 0.0233(8) Uani 1.0 4 d . . . N14 N 0.3395(4) 0.8950(4) 0.84182(12) 0.0225(8) Uani 1.0 4 d . . . N15 N 0.4387(4) 0.8447(4) 0.86388(12) 0.0214(8) Uani 1.0 4 d . . . N16 N 0.3739(15) 0.6288(16) 0.8965(6) 0.014(4) Uiso 0.3000 4 d . . . C1 C 0.1061(6) 0.8864(5) 0.76149(17) 0.0374(13) Uani 1.0 4 d . . . C2 C 0.0268(7) 0.9387(6) 0.73182(19) 0.0470(16) Uani 1.0 4 d . . . C3 C -0.0385(6) 1.0121(6) 0.75153(17) 0.0375(13) Uani 1.0 4 d . . . C4 C 0.2547(7) 1.1331(5) 0.8831(3) 0.0529(19) Uani 1.0 4 d . . . C5 C 0.2084(8) 1.2437(6) 0.8821(3) 0.066(3) Uani 1.0 4 d . . . C6 C 0.0944(6) 1.2338(5) 0.86153(19) 0.0388(13) Uani 1.0 4 d . . . C7 C -0.0504(5) 0.8477(5) 0.90248(16) 0.0290(11) Uani 1.0 4 d . . . C8 C -0.1636(5) 0.8932(5) 0.90412(19) 0.0360(13) Uani 1.0 4 d . . . C9 C -0.1771(5) 0.9789(5) 0.87567(18) 0.0350(12) Uani 1.0 4 d . . . C10 C 0.6425(5) 0.6210(5) 0.88681(16) 0.0288(11) Uani 1.0 4 d . . . C11 C 0.7555(5) 0.5782(5) 0.90203(18) 0.0343(13) Uani 1.0 4 d . . . C12 C 0.7789(5) 0.6155(4) 0.94169(17) 0.0291(11) Uani 1.0 4 d . . . C13 C 0.5471(5) 1.0011(5) 0.94263(18) 0.0304(11) Uani 1.0 4 d . . . C14 C 0.6378(5) 1.0478(5) 0.97081(19) 0.0334(12) Uani 1.0 4 d . . . C15 C 0.6907(5) 0.9569(5) 0.99204(17) 0.0286(11) Uani 1.0 4 d . . . C16 C 0.3542(5) 0.6485(4) 0.99373(15) 0.0260(10) Uani 1.0 4 d . . . C17 C 0.4039(5) 0.6122(5) 1.03205(16) 0.0307(11) Uani 1.0 4 d . . . C18 C 0.5232(5) 0.6373(5) 1.03575(15) 0.0284(11) Uani 1.0 4 d . . . C19 C 0.3767(5) 0.9508(5) 0.81081(17) 0.0322(12) Uani 1.0 4 d . . . C20 C 0.4995(5) 0.9372(5) 0.81205(16) 0.0287(11) Uani 1.0 4 d . . . C21 C 0.5343(5) 0.8710(5) 0.84536(15) 0.0271(11) Uani 1.0 4 d . . . C22 C 0.0385(7) 0.7391(7) 1.0419(3) 0.100(4) Uani 1.0 4 d . . . C23 C -0.2725(6) 0.7618(7) 0.76851(6) 0.0583(19) Uani 1.0 4 d . . . C24 C 0.5559(5) 0.3122(6) 0.81473(14) 0.0595(19) Uani 1.0 4 d . . . B1 B -0.0387(6) 1.0700(5) 0.82742(19) 0.0294(12) Uani 1.0 4 d . . . B2 B 0.6611(5) 0.7366(5) 0.98899(17) 0.0241(11) Uani 1.0 4 d . . . B3 B 0.1024(3) 0.5154(3) 0.92713(10) 0.0422(16) Uani 1.0 4 d . . . B4 B 0.3742(3) 0.5977(3) 0.78256(9) 0.0335(13) Uani 1.0 4 d . . . H1 H -0.104(5) 1.132(5) 0.8186(17) 0.021(14) Uiso 1.0 4 d . . . H2 H 0.742(6) 0.731(6) 1.013(2) 0.042(18) Uiso 1.0 4 d . . . H3 H 0.1636 0.8309 0.7569 0.0449 Uiso 1.0 4 calc R . . H4 H 0.0190 0.9263 0.7033 0.0564 Uiso 1.0 4 calc R . . H5 H -0.1006 1.0603 0.7389 0.0450 Uiso 1.0 4 calc R . . H6 H 0.3328 1.1117 0.8957 0.0635 Uiso 1.0 4 calc R . . H7 H 0.2476 1.3103 0.8932 0.0790 Uiso 1.0 4 calc R . . H8 H 0.0382 1.2938 0.8560 0.0466 Uiso 1.0 4 calc R . . H9 H -0.0149 0.7871 0.9188 0.0348 Uiso 1.0 4 calc R . . H10 H -0.2197 0.8701 0.9212 0.0432 Uiso 1.0 4 calc R . . H11 H -0.2454 1.0267 0.8699 0.0419 Uiso 1.0 4 calc R . . H12 H 0.6018 0.6094 0.8600 0.0345 Uiso 1.0 4 calc R . . H13 H 0.8059 0.5328 0.8880 0.0412 Uiso 1.0 4 calc R . . H14 H 0.8498 0.6001 0.9602 0.0349 Uiso 1.0 4 calc R . . H15 H 0.4947 1.0428 0.9230 0.0365 Uiso 1.0 4 calc R . . H16 H 0.6584 1.1253 0.9745 0.0400 Uiso 1.0 4 calc R . . H17 H 0.7572 0.9607 1.0133 0.0343 Uiso 1.0 4 calc R . . H18 H 0.2717 0.6429 0.9824 0.0312 Uiso 1.0 4 calc R . . H19 H 0.3631 0.5770 1.0518 0.0368 Uiso 1.0 4 calc R . . H20 H 0.5810 0.6226 1.0590 0.0340 Uiso 1.0 4 calc R . . H21 H 0.3262 0.9935 0.7909 0.0386 Uiso 1.0 4 calc R . . H22 H 0.5486 0.9673 0.7937 0.0345 Uiso 1.0 4 calc R . . H23 H 0.6145 0.8469 0.8543 0.0325 Uiso 1.0 4 calc R . . H24 H 0.0462 0.6732 1.0241 0.1199 Uiso 1.0 4 calc R . . H25 H -0.0346 0.7281 1.0547 0.1199 Uiso 1.0 4 calc R . . H26 H -0.2780 0.8453 0.7692 0.0700 Uiso 1.0 4 calc R . . H27 H -0.3533 0.7310 0.7706 0.0700 Uiso 1.0 4 calc R . . H28 H 0.5505 0.2473 0.7957 0.0714 Uiso 1.0 4 calc R . . H29 H 0.4837 0.3597 0.8070 0.0714 Uiso 1.0 4 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru1 0.01889(18) 0.02031(19) 0.02137(19) 0.00422(13) 0.00575(14) 0.00195(14) Ru2 0.01603(17) 0.0263(2) 0.01848(18) 0.00217(14) 0.00599(13) 0.00095(14) Cl1 0.0184(5) 0.0261(6) 0.0217(5) 0.0015(4) 0.0069(4) -0.0016(5) Cl2 0.0824(14) 0.0695(13) 0.0462(10) -0.0183(11) 0.0175(9) -0.0221(9) Cl3 0.0678(14) 0.135(3) 0.0482(11) -0.0166(15) -0.0046(10) -0.0000(13) Cl4 0.0704(14) 0.127(3) 0.0675(14) -0.0341(15) -0.0030(11) 0.0238(15) Cl5 0.0751(14) 0.0852(15) 0.0551(11) -0.0133(12) 0.0261(10) -0.0156(11) Cl6 0.0719(16) 0.166(3) 0.152(3) -0.0489(19) -0.0388(18) 0.110(3) Cl7 0.0383(8) 0.0520(10) 0.0609(10) 0.0041(7) 0.0049(7) 0.0091(8) O1 0.027(3) 0.017(3) 0.036(3) -0.006(2) 0.002(2) -0.008(2) O2 0.024(4) 0.025(3) 0.027(4) 0.003(3) 0.004(3) 0.000(3) N1 0.013(3) 0.031(4) 0.024(4) 0.006(3) 0.007(3) 0.002(3) N2 0.029(3) 0.025(2) 0.026(2) 0.0033(17) 0.0039(17) 0.0019(17) N3 0.023(2) 0.030(3) 0.032(3) 0.0035(17) 0.0003(17) 0.0079(18) N4 0.027(2) 0.021(2) 0.034(3) 0.0031(17) 0.0028(18) 0.0057(18) N5 0.028(2) 0.020(2) 0.032(3) 0.0064(17) 0.0069(17) 0.0039(17) N6 0.0216(19) 0.025(2) 0.029(2) 0.0034(16) 0.0050(16) 0.0058(17) N7 0.021(2) 0.029(3) 0.035(3) 0.0054(17) 0.0034(17) 0.0064(19) N8 0.0231(19) 0.0205(19) 0.028(2) 0.0008(16) 0.0100(16) -0.0007(16) N9 0.0209(19) 0.023(2) 0.030(3) 0.0045(16) 0.0075(16) 0.0019(17) N10 0.0161(17) 0.0208(19) 0.026(2) 0.0035(15) 0.0045(15) 0.0035(16) N11 0.0196(18) 0.0213(19) 0.0223(19) 0.0020(15) 0.0031(15) -0.0000(16) N12 0.0202(18) 0.0210(19) 0.0226(19) 0.0016(15) 0.0070(15) 0.0008(16) N13 0.025(2) 0.0201(19) 0.025(2) 0.0029(16) 0.0046(16) 0.0016(16) N14 0.0214(19) 0.0233(19) 0.024(2) 0.0027(16) 0.0078(16) 0.0046(16) N15 0.0180(18) 0.0242(19) 0.0231(19) 0.0022(15) 0.0066(15) 0.0031(16) C1 0.049(4) 0.035(3) 0.028(3) 0.005(3) 0.005(3) -0.000(3) C2 0.061(5) 0.050(4) 0.027(3) 0.003(4) -0.002(3) -0.001(3) C3 0.036(3) 0.043(4) 0.031(3) -0.002(3) -0.004(3) 0.009(3) C4 0.044(4) 0.023(3) 0.082(5) -0.001(3) -0.026(4) 0.003(3) C5 0.066(5) 0.026(3) 0.093(7) 0.002(3) -0.033(5) -0.001(4) C6 0.046(4) 0.026(3) 0.043(4) 0.006(3) -0.001(3) 0.003(3) C7 0.023(3) 0.031(3) 0.034(3) -0.003(2) 0.008(2) 0.004(3) C8 0.024(3) 0.042(3) 0.044(4) 0.001(3) 0.014(3) 0.005(3) C9 0.019(3) 0.040(3) 0.046(4) 0.005(3) 0.006(3) 0.003(3) C10 0.032(3) 0.027(3) 0.031(3) -0.001(2) 0.015(2) -0.004(2) C11 0.035(3) 0.026(3) 0.049(4) 0.003(3) 0.025(3) -0.001(3) C12 0.022(3) 0.021(3) 0.046(3) 0.0061(19) 0.012(3) 0.005(3) C13 0.023(3) 0.023(3) 0.046(3) 0.0025(19) 0.007(3) 0.010(3) C14 0.026(3) 0.020(3) 0.056(4) -0.002(2) 0.013(3) -0.008(3) C15 0.024(3) 0.028(3) 0.036(3) -0.003(2) 0.010(2) -0.012(3) C16 0.027(3) 0.023(3) 0.031(3) -0.0040(19) 0.013(2) -0.002(2) C17 0.041(3) 0.023(3) 0.031(3) -0.001(3) 0.015(3) 0.001(2) C18 0.039(3) 0.023(3) 0.023(3) 0.005(2) 0.006(2) 0.0049(19) C19 0.032(3) 0.036(3) 0.032(3) 0.007(3) 0.015(3) 0.011(3) C20 0.030(3) 0.030(3) 0.029(3) -0.004(2) 0.015(2) 0.004(2) C21 0.019(3) 0.038(3) 0.026(3) -0.001(2) 0.0089(19) 0.002(2) C22 0.055(6) 0.143(11) 0.093(8) -0.016(6) -0.018(5) 0.050(8) C23 0.053(5) 0.073(6) 0.051(4) 0.011(4) 0.014(4) -0.002(4) C24 0.058(5) 0.062(5) 0.055(5) 0.003(4) -0.004(4) -0.014(4) B1 0.026(3) 0.029(3) 0.034(3) 0.005(3) 0.006(3) 0.003(3) B2 0.025(3) 0.023(3) 0.024(3) 0.007(2) 0.002(2) 0.002(2) B3 0.032(4) 0.039(4) 0.056(5) 0.004(3) 0.010(3) 0.012(4) B4 0.033(3) 0.035(4) 0.033(3) 0.002(3) 0.006(3) -0.006(3) #============================================================================== _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'Il Milione (Burla, et al., 2007)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # 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 Ru1 Cl1 2.3794(11) yes . . Ru1 O4 2.001(19) yes . . Ru1 N1 1.789(8) yes . . Ru1 N2 2.053(5) yes . . Ru1 N4 2.064(5) yes . . Ru1 N6 2.064(5) yes . . Ru1 N14 2.054(5) yes . . Ru2 Cl1 2.3898(12) yes . . Ru2 O2 2.043(7) yes . . Ru2 N8 2.049(4) yes . . Ru2 N10 2.036(4) yes . . Ru2 N12 2.053(4) yes . . Ru2 N15 2.042(4) yes . . Ru2 N16 1.864(18) yes . . Cl2 C23 1.731(5) yes . . Cl3 C23 1.730(5) yes . . Cl4 C24 1.733(6) yes . . Cl5 C24 1.733(7) yes . . Cl6 C22 1.730(9) yes . . Cl7 C22 1.731(8) yes . . F1 B3 1.389(5) yes . . F2 B3 1.389(7) yes . . F3 B3 1.395(5) yes . . F4 B3 1.385(5) yes . . F5 B4 1.389(5) yes . . F6 B4 1.383(6) yes . . F7 B4 1.390(5) yes . . F8 B4 1.396(5) yes . . F9 B3 1.386(10) yes . . F10 B3 1.393(10) yes . . F11 B3 1.393(8) yes . . F13 B4 1.390(7) yes . . F14 B4 1.387(7) yes . . F15 B4 1.396(10) yes . . O1 N1 1.137(10) yes . . O3 N16 1.15(3) yes . . N2 N3 1.369(6) yes . . N2 C1 1.331(8) yes . . N3 C3 1.345(7) yes . . N3 B1 1.528(8) yes . . N4 N5 1.365(6) yes . . N4 C4 1.315(8) yes . . N5 C6 1.321(7) yes . . N5 B1 1.547(7) yes . . N6 N7 1.368(6) yes . . N6 C7 1.344(7) yes . . N7 C9 1.338(8) yes . . N7 B1 1.538(8) yes . . N8 N9 1.381(6) yes . . N8 C10 1.337(7) yes . . N9 C12 1.346(7) yes . . N9 B2 1.530(8) yes . . N10 N11 1.360(5) yes . . N10 C13 1.337(7) yes . . N11 C15 1.337(7) yes . . N11 B2 1.550(7) yes . . N12 N13 1.359(6) yes . . N12 C16 1.353(7) yes . . N13 C18 1.345(7) yes . . N13 B2 1.531(8) yes . . N14 N15 1.376(6) yes . . N14 C19 1.342(8) yes . . N15 C21 1.352(7) yes . . C1 C2 1.375(9) yes . . C2 C3 1.365(10) yes . . C4 C5 1.407(10) yes . . C5 C6 1.365(10) yes . . C7 C8 1.390(8) yes . . C8 C9 1.379(9) yes . . C10 C11 1.392(8) yes . . C11 C12 1.378(8) yes . . C13 C14 1.392(8) yes . . C14 C15 1.371(8) yes . . C16 C17 1.381(7) yes . . C17 C18 1.362(8) yes . . C19 C20 1.384(8) yes . . C20 C21 1.365(8) yes . . C1 H3 0.950 no . . C2 H4 0.950 no . . C3 H5 0.950 no . . C4 H6 0.950 no . . C5 H7 0.950 no . . C6 H8 0.950 no . . C7 H9 0.950 no . . C8 H10 0.950 no . . C9 H11 0.950 no . . C10 H12 0.950 no . . C11 H13 0.950 no . . C12 H14 0.950 no . . C13 H15 0.950 no . . C14 H16 0.950 no . . C15 H17 0.950 no . . C16 H18 0.950 no . . C17 H19 0.950 no . . C18 H20 0.950 no . . C19 H21 0.950 no . . C20 H22 0.950 no . . C21 H23 0.950 no . . C22 H24 0.990 no . . C22 H25 0.990 no . . C23 H26 0.990 no . . C23 H27 0.990 no . . C24 H28 0.990 no . . C24 H29 0.990 no . . B1 H1 1.05(6) no . . B2 H2 1.11(7) 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 Cl1 Ru1 O4 91.3(6) yes . . . Cl1 Ru1 N1 95.8(3) yes . . . Cl1 Ru1 N2 175.84(13) yes . . . Cl1 Ru1 N4 90.62(13) yes . . . Cl1 Ru1 N6 91.02(12) yes . . . Cl1 Ru1 N14 86.34(11) yes . . . O4 Ru1 N2 92.8(6) yes . . . O4 Ru1 N4 176.1(6) yes . . . O4 Ru1 N6 98.8(6) yes . . . O4 Ru1 N14 87.5(6) yes . . . N1 Ru1 N2 88.3(3) yes . . . N1 Ru1 N4 170.2(3) yes . . . N1 Ru1 N6 87.9(3) yes . . . N1 Ru1 N14 98.5(3) yes . . . N2 Ru1 N4 85.23(17) yes . . . N2 Ru1 N6 88.64(17) yes . . . N2 Ru1 N14 93.55(17) yes . . . N4 Ru1 N6 84.54(17) yes . . . N4 Ru1 N14 89.28(17) yes . . . N6 Ru1 N14 173.25(16) yes . . . Cl1 Ru2 O2 88.55(19) yes . . . Cl1 Ru2 N8 177.09(11) yes . . . Cl1 Ru2 N10 91.98(12) yes . . . Cl1 Ru2 N12 90.34(12) yes . . . Cl1 Ru2 N15 87.06(12) yes . . . Cl1 Ru2 N16 99.0(5) yes . . . O2 Ru2 N8 93.8(3) yes . . . O2 Ru2 N10 178.8(3) yes . . . O2 Ru2 N12 94.7(3) yes . . . O2 Ru2 N15 88.5(3) yes . . . N8 Ru2 N10 85.75(16) yes . . . N8 Ru2 N12 87.70(16) yes . . . N8 Ru2 N15 94.77(16) yes . . . N8 Ru2 N16 83.1(6) yes . . . N10 Ru2 N12 86.36(16) yes . . . N10 Ru2 N15 90.47(16) yes . . . N10 Ru2 N16 167.4(5) yes . . . N12 Ru2 N15 175.83(16) yes . . . N12 Ru2 N16 87.4(6) yes . . . N15 Ru2 N16 96.2(6) yes . . . Ru1 Cl1 Ru2 103.60(5) yes . . . Ru1 N1 O1 171.5(7) yes . . . Ru1 N2 N3 118.8(4) yes . . . Ru1 N2 C1 133.3(4) yes . . . N3 N2 C1 107.9(5) yes . . . N2 N3 C3 107.9(5) yes . . . N2 N3 B1 121.3(5) yes . . . C3 N3 B1 130.8(5) yes . . . Ru1 N4 N5 119.8(3) yes . . . Ru1 N4 C4 133.6(4) yes . . . N5 N4 C4 106.4(5) yes . . . N4 N5 C6 110.1(5) yes . . . N4 N5 B1 119.7(4) yes . . . C6 N5 B1 130.2(5) yes . . . Ru1 N6 N7 120.2(4) yes . . . Ru1 N6 C7 132.0(4) yes . . . N7 N6 C7 107.8(5) yes . . . N6 N7 C9 108.5(5) yes . . . N6 N7 B1 119.2(5) yes . . . C9 N7 B1 131.7(5) yes . . . Ru2 N8 N9 118.8(3) yes . . . Ru2 N8 C10 133.8(4) yes . . . N9 N8 C10 107.3(4) yes . . . N8 N9 C12 108.4(4) yes . . . N8 N9 B2 119.9(4) yes . . . C12 N9 B2 131.7(4) yes . . . Ru2 N10 N11 119.7(3) yes . . . Ru2 N10 C13 133.5(4) yes . . . N11 N10 C13 106.8(4) yes . . . N10 N11 C15 109.3(4) yes . . . N10 N11 B2 119.7(4) yes . . . C15 N11 B2 130.8(4) yes . . . Ru2 N12 N13 120.1(3) yes . . . Ru2 N12 C16 132.7(3) yes . . . N13 N12 C16 107.2(4) yes . . . N12 N13 C18 108.7(4) yes . . . N12 N13 B2 119.2(4) yes . . . C18 N13 B2 132.1(4) yes . . . Ru1 N14 N15 125.4(3) yes . . . Ru1 N14 C19 127.0(4) yes . . . N15 N14 C19 107.5(4) yes . . . Ru2 N15 N14 125.2(4) yes . . . Ru2 N15 C21 127.2(3) yes . . . N14 N15 C21 107.1(4) yes . . . Ru2 N16 O3 171.5(15) yes . . . N2 C1 C2 109.2(6) yes . . . C1 C2 C3 106.3(6) yes . . . N3 C3 C2 108.8(6) yes . . . N4 C4 C5 110.1(6) yes . . . C4 C5 C6 104.4(6) yes . . . N5 C6 C5 108.9(6) yes . . . N6 C7 C8 109.0(5) yes . . . C7 C8 C9 105.4(6) yes . . . N7 C9 C8 109.2(5) yes . . . N8 C10 C11 109.8(5) yes . . . C10 C11 C12 105.4(5) yes . . . N9 C12 C11 109.1(5) yes . . . N10 C13 C14 110.0(5) yes . . . C13 C14 C15 104.7(5) yes . . . N11 C15 C14 109.1(5) yes . . . N12 C16 C17 109.1(5) yes . . . C16 C17 C18 105.9(5) yes . . . N13 C18 C17 109.1(5) yes . . . N14 C19 C20 110.1(5) yes . . . C19 C20 C21 104.9(5) yes . . . N15 C21 C20 110.4(5) yes . . . Cl6 C22 Cl7 113.3(5) yes . . . Cl2 C23 Cl3 114.0(4) yes . . . Cl4 C24 Cl5 114.1(3) yes . . . N3 B1 N5 107.5(5) yes . . . N3 B1 N7 108.2(5) yes . . . N5 B1 N7 105.4(5) yes . . . N9 B2 N11 107.1(4) yes . . . N9 B2 N13 107.8(4) yes . . . N11 B2 N13 107.0(4) yes . . . F1 B3 F2 109.1(4) yes . . . F1 B3 F3 108.9(4) yes . . . F1 B3 F4 110.7(4) yes . . . F1 B3 F9 110.6(5) yes . . . F1 B3 F10 109.0(5) yes . . . F1 B3 F11 108.8(5) yes . . . F2 B3 F3 109.1(4) yes . . . F2 B3 F4 110.0(5) yes . . . F3 B3 F4 109.0(4) yes . . . F9 B3 F10 107.7(8) yes . . . F9 B3 F11 112.0(7) yes . . . F10 B3 F11 108.8(8) yes . . . F5 B4 F6 111.0(3) yes . . . F5 B4 F7 108.9(3) yes . . . F5 B4 F8 107.9(4) yes . . . F5 B4 F13 109.8(5) yes . . . F5 B4 F14 110.9(4) yes . . . F5 B4 F15 108.6(4) yes . . . F6 B4 F7 110.5(4) yes . . . F6 B4 F8 109.8(4) yes . . . F7 B4 F8 108.7(4) yes . . . F13 B4 F14 109.9(6) yes . . . F13 B4 F15 108.6(5) yes . . . F14 B4 F15 109.0(6) yes . . . N2 C1 H3 125.411 no . . . C2 C1 H3 125.439 no . . . C1 C2 H4 126.866 no . . . C3 C2 H4 126.881 no . . . N3 C3 H5 125.615 no . . . C2 C3 H5 125.607 no . . . N4 C4 H6 124.917 no . . . C5 C4 H6 124.933 no . . . C4 C5 H7 127.792 no . . . C6 C5 H7 127.794 no . . . N5 C6 H8 125.524 no . . . C5 C6 H8 125.536 no . . . N6 C7 H9 125.486 no . . . C8 C7 H9 125.464 no . . . C7 C8 H10 127.282 no . . . C9 C8 H10 127.268 no . . . N7 C9 H11 125.387 no . . . C8 C9 H11 125.386 no . . . N8 C10 H12 125.110 no . . . C11 C10 H12 125.114 no . . . C10 C11 H13 127.317 no . . . C12 C11 H13 127.303 no . . . N9 C12 H14 125.425 no . . . C11 C12 H14 125.427 no . . . N10 C13 H15 124.981 no . . . C14 C13 H15 124.994 no . . . C13 C14 H16 127.633 no . . . C15 C14 H16 127.641 no . . . N11 C15 H17 125.449 no . . . C14 C15 H17 125.439 no . . . N12 C16 H18 125.443 no . . . C17 C16 H18 125.468 no . . . C16 C17 H19 127.045 no . . . C18 C17 H19 127.045 no . . . N13 C18 H20 125.420 no . . . C17 C18 H20 125.433 no . . . N14 C19 H21 124.960 no . . . C20 C19 H21 124.970 no . . . C19 C20 H22 127.570 no . . . C21 C20 H22 127.578 no . . . N15 C21 H23 124.773 no . . . C20 C21 H23 124.810 no . . . Cl6 C22 H24 108.912 no . . . Cl6 C22 H25 108.911 no . . . Cl7 C22 H24 108.923 no . . . Cl7 C22 H25 108.931 no . . . H24 C22 H25 107.745 no . . . Cl2 C23 H26 108.755 no . . . Cl2 C23 H27 108.743 no . . . Cl3 C23 H26 108.756 no . . . Cl3 C23 H27 108.765 no . . . H26 C23 H27 107.653 no . . . Cl4 C24 H28 108.729 no . . . Cl4 C24 H29 108.742 no . . . Cl5 C24 H28 108.740 no . . . Cl5 C24 H29 108.741 no . . . H28 C24 H29 107.637 no . . . N3 B1 H1 114(3) no . . . N5 B1 H1 109(3) no . . . N7 B1 H1 112(4) no . . . N9 B2 H2 110(4) no . . . N11 B2 H2 110(4) no . . . N13 B2 H2 115(4) no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 O4 Ru1 Cl1 Ru2 56.7(6) no . . . . N1 Ru1 Cl1 Ru2 67.5(3) no . . . . Cl1 Ru1 N4 N5 -133.5(3) no . . . . Cl1 Ru1 N4 C4 39.9(5) no . . . . N4 Ru1 Cl1 Ru2 -119.96(13) no . . . . Cl1 Ru1 N6 N7 137.6(3) no . . . . Cl1 Ru1 N6 C7 -39.0(4) no . . . . N6 Ru1 Cl1 Ru2 155.50(12) no . . . . Cl1 Ru1 N14 N15 25.5(3) no . . . . Cl1 Ru1 N14 C19 -151.2(3) no . . . . N14 Ru1 Cl1 Ru2 -30.72(12) no . . . . O4 Ru1 N2 N3 137.4(6) no . . . . O4 Ru1 N2 C1 -41.6(7) no . . . . O4 Ru1 N6 N7 -130.8(6) no . . . . O4 Ru1 N6 C7 52.5(7) no . . . . O4 Ru1 N14 N15 -66.0(6) no . . . . O4 Ru1 N14 C19 117.3(6) no . . . . N1 Ru1 N2 N3 126.7(4) no . . . . N1 Ru1 N2 C1 -52.4(5) no . . . . N1 Ru1 N6 N7 -126.6(4) no . . . . N1 Ru1 N6 C7 56.8(4) no . . . . N1 Ru1 N14 N15 -69.8(4) no . . . . N1 Ru1 N14 C19 113.4(4) no . . . . N2 Ru1 N4 N5 46.6(4) no . . . . N2 Ru1 N4 C4 -140.1(5) no . . . . N4 Ru1 N2 N3 -45.9(3) no . . . . N4 Ru1 N2 C1 135.0(4) no . . . . N2 Ru1 N6 N7 -38.2(3) no . . . . N2 Ru1 N6 C7 145.1(4) no . . . . N6 Ru1 N2 N3 38.7(3) no . . . . N6 Ru1 N2 C1 -140.4(4) no . . . . N2 Ru1 N14 N15 -158.6(3) no . . . . N2 Ru1 N14 C19 24.6(4) no . . . . N14 Ru1 N2 N3 -134.9(3) no . . . . N14 Ru1 N2 C1 46.0(4) no . . . . N4 Ru1 N6 N7 47.1(3) no . . . . N4 Ru1 N6 C7 -129.5(4) no . . . . N6 Ru1 N4 N5 -42.5(4) no . . . . N6 Ru1 N4 C4 130.8(5) no . . . . N4 Ru1 N14 N15 116.2(3) no . . . . N4 Ru1 N14 C19 -60.6(4) no . . . . N14 Ru1 N4 N5 140.2(4) no . . . . N14 Ru1 N4 C4 -46.5(5) no . . . . O2 Ru2 Cl1 Ru1 -59.04(19) no . . . . Cl1 Ru2 N10 N11 131.3(3) no . . . . Cl1 Ru2 N10 C13 -49.5(4) no . . . . N10 Ru2 Cl1 Ru1 119.89(12) no . . . . Cl1 Ru2 N12 N13 -137.4(3) no . . . . Cl1 Ru2 N12 C16 42.7(4) no . . . . N12 Ru2 Cl1 Ru1 -153.74(11) no . . . . Cl1 Ru2 N15 N14 -19.2(3) no . . . . Cl1 Ru2 N15 C21 152.1(3) no . . . . N15 Ru2 Cl1 Ru1 29.53(12) no . . . . N16 Ru2 Cl1 Ru1 -66.3(6) no . . . . O2 Ru2 N8 N9 -135.6(3) no . . . . O2 Ru2 N8 C10 41.1(4) no . . . . O2 Ru2 N12 N13 134.0(4) no . . . . O2 Ru2 N12 C16 -45.9(4) no . . . . O2 Ru2 N15 N14 69.4(4) no . . . . O2 Ru2 N15 C21 -119.2(4) no . . . . N8 Ru2 N10 N11 -46.9(3) no . . . . N8 Ru2 N10 C13 132.3(4) no . . . . N10 Ru2 N8 N9 45.4(3) no . . . . N10 Ru2 N8 C10 -137.8(4) no . . . . N8 Ru2 N12 N13 40.4(3) no . . . . N8 Ru2 N12 C16 -139.5(4) no . . . . N12 Ru2 N8 N9 -41.1(3) no . . . . N12 Ru2 N8 C10 135.7(4) no . . . . N8 Ru2 N15 N14 163.1(3) no . . . . N8 Ru2 N15 C21 -25.6(4) no . . . . N15 Ru2 N8 N9 135.6(3) no . . . . N15 Ru2 N8 C10 -47.7(4) no . . . . N16 Ru2 N8 N9 -128.8(6) no . . . . N16 Ru2 N8 C10 48.0(7) no . . . . N10 Ru2 N12 N13 -45.5(3) no . . . . N10 Ru2 N12 C16 134.7(4) no . . . . N12 Ru2 N10 N11 41.1(3) no . . . . N12 Ru2 N10 C13 -139.7(4) no . . . . N10 Ru2 N15 N14 -111.2(3) no . . . . N10 Ru2 N15 C21 60.2(4) no . . . . N15 Ru2 N10 N11 -141.6(3) no . . . . N15 Ru2 N10 C13 37.6(4) no . . . . N16 Ru2 N12 N13 123.6(6) no . . . . N16 Ru2 N12 C16 -56.3(6) no . . . . N16 Ru2 N15 N14 79.5(6) no . . . . N16 Ru2 N15 C21 -109.1(6) no . . . . Ru1 N2 N3 C3 -179.0(3) no . . . . Ru1 N2 N3 B1 2.9(6) no . . . . Ru1 N2 C1 C2 178.8(3) no . . . . N3 N2 C1 C2 -0.3(6) no . . . . C1 N2 N3 C3 0.3(6) no . . . . C1 N2 N3 B1 -177.8(4) no . . . . N2 N3 C3 C2 -0.2(6) no . . . . N2 N3 B1 N5 55.0(6) no . . . . N2 N3 B1 N7 -58.4(6) no . . . . C3 N3 B1 N5 -122.7(6) no . . . . C3 N3 B1 N7 123.9(6) no . . . . B1 N3 C3 C2 177.7(5) no . . . . Ru1 N4 N5 C6 174.8(3) no . . . . Ru1 N4 N5 B1 -3.8(6) no . . . . Ru1 N4 C4 C5 -174.4(4) no . . . . N5 N4 C4 C5 -0.4(8) no . . . . C4 N4 N5 C6 -0.2(7) no . . . . C4 N4 N5 B1 -178.8(5) no . . . . N4 N5 C6 C5 0.7(7) no . . . . N4 N5 B1 N3 -54.0(6) no . . . . N4 N5 B1 N7 61.3(6) no . . . . C6 N5 B1 N3 127.7(6) no . . . . C6 N5 B1 N7 -117.0(6) no . . . . B1 N5 C6 C5 179.2(5) no . . . . Ru1 N6 N7 C9 -176.6(3) no . . . . Ru1 N6 N7 B1 -4.3(6) no . . . . Ru1 N6 C7 C8 176.8(3) no . . . . N7 N6 C7 C8 -0.2(5) no . . . . C7 N6 N7 C9 0.7(5) no . . . . C7 N6 N7 B1 173.0(4) no . . . . N6 N7 C9 C8 -1.0(6) no . . . . N6 N7 B1 N3 58.6(6) no . . . . N6 N7 B1 N5 -56.1(6) no . . . . C9 N7 B1 N3 -131.2(6) no . . . . C9 N7 B1 N5 114.1(6) no . . . . B1 N7 C9 C8 -172.0(5) no . . . . Ru2 N8 N9 C12 177.7(3) no . . . . Ru2 N8 N9 B2 -1.2(5) no . . . . Ru2 N8 C10 C11 -177.1(3) no . . . . N9 N8 C10 C11 -0.1(6) no . . . . C10 N8 N9 C12 0.2(5) no . . . . C10 N8 N9 B2 -178.8(4) no . . . . N8 N9 C12 C11 -0.2(5) no . . . . N8 N9 B2 N11 -56.3(6) no . . . . N8 N9 B2 N13 58.5(6) no . . . . C12 N9 B2 N11 125.0(5) no . . . . C12 N9 B2 N13 -120.2(6) no . . . . B2 N9 C12 C11 178.6(5) no . . . . Ru2 N10 N11 C15 179.2(3) no . . . . Ru2 N10 N11 B2 3.8(5) no . . . . Ru2 N10 C13 C14 -179.8(3) no . . . . N11 N10 C13 C14 -0.5(6) no . . . . C13 N10 N11 C15 -0.2(5) no . . . . C13 N10 N11 B2 -175.6(4) no . . . . N10 N11 C15 C14 0.9(6) no . . . . N10 N11 B2 N9 55.3(6) no . . . . N10 N11 B2 N13 -60.1(6) no . . . . C15 N11 B2 N9 -119.0(6) no . . . . C15 N11 B2 N13 125.7(6) no . . . . B2 N11 C15 C14 175.6(5) no . . . . Ru2 N12 N13 C18 -179.9(3) no . . . . Ru2 N12 N13 B2 3.4(5) no . . . . Ru2 N12 C16 C17 179.6(3) no . . . . N13 N12 C16 C17 -0.3(5) no . . . . C16 N12 N13 C18 0.0(5) no . . . . C16 N12 N13 B2 -176.7(4) no . . . . N12 N13 C18 C17 0.2(5) no . . . . N12 N13 B2 N9 -59.7(5) no . . . . N12 N13 B2 N11 55.2(5) no . . . . C18 N13 B2 N9 124.5(5) no . . . . C18 N13 B2 N11 -120.6(6) no . . . . B2 N13 C18 C17 176.4(5) no . . . . Ru1 N14 N15 Ru2 -4.8(6) no . . . . Ru1 N14 N15 C21 -177.6(3) no . . . . Ru1 N14 C19 C20 177.6(3) no . . . . N15 N14 C19 C20 0.4(6) no . . . . C19 N14 N15 Ru2 172.5(4) no . . . . C19 N14 N15 C21 -0.3(5) no . . . . Ru2 N15 C21 C20 -172.4(3) no . . . . N14 N15 C21 C20 0.2(5) no . . . . N2 C1 C2 C3 0.2(7) no . . . . C1 C2 C3 N3 0.0(8) no . . . . N4 C4 C5 C6 0.9(10) no . . . . C4 C5 C6 N5 -0.9(9) no . . . . N6 C7 C8 C9 -0.4(6) no . . . . C7 C8 C9 N7 0.9(6) no . . . . N8 C10 C11 C12 -0.0(6) no . . . . C10 C11 C12 N9 0.2(6) no . . . . N10 C13 C14 C15 1.0(7) no . . . . C13 C14 C15 N11 -1.2(7) no . . . . N12 C16 C17 C18 0.4(6) no . . . . C16 C17 C18 N13 -0.4(6) no . . . . N14 C19 C20 C21 -0.3(6) no . . . . C19 C20 C21 N15 0.1(6) no . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Ru1 B1 3.190(6) no . . Ru2 B2 3.167(6) no . . Cl1 C4 3.474(7) no . . Cl1 C7 3.463(5) no . . Cl1 C13 3.587(5) no . . Cl1 C16 3.481(5) no . . O1 O2 2.939(8) no . . O1 N2 3.449(7) no . . O1 N6 3.440(7) no . . O2 N1 2.785(10) no . . O2 N14 3.401(8) no . . O2 C10 3.432(9) no . . O2 C16 3.488(9) no . . O3 O4 3.09(3) no . . O3 N8 3.324(13) no . . O3 N12 3.548(14) no . . O3 C10 3.443(14) no . . O4 N15 3.327(18) no . . O4 N16 2.88(3) no . . O4 C1 3.38(2) no . . N1 N15 3.569(9) no . . N1 C1 3.240(10) no . . N1 C7 3.261(10) no . . N2 N5 2.978(6) no . . N2 N7 3.017(7) no . . N2 C19 3.207(7) no . . N3 N4 2.948(6) no . . N3 N6 2.988(7) no . . N4 N7 2.974(6) no . . N4 C19 3.358(8) no . . N5 N6 2.918(6) no . . N5 C9 3.536(8) no . . N7 C6 3.530(8) no . . N8 N11 2.969(6) no . . N8 N13 2.991(6) no . . N8 C21 3.247(7) no . . N9 N10 2.953(6) no . . N9 N12 2.977(6) no . . N9 C15 3.586(7) no . . N10 N13 2.991(6) no . . N10 C21 3.376(7) no . . N11 N12 2.933(6) no . . N14 C1 3.456(7) no . . N14 C4 3.332(8) no . . N15 C10 3.509(7) no . . N15 C13 3.288(7) no . . N16 C10 3.086(18) no . . N16 C16 3.277(19) no . . C1 C19 3.324(8) no . . C10 C21 3.409(8) no . . C13 C21 3.563(8) no . . Cl1 F4 3.325(4) no . . Cl1 F11 3.158(8) no . . Cl1 C15 3.466(6) no . 3_677 Cl2 F14 3.414(6) no . 2_556 Cl2 N4 3.561(5) no . 2_546 Cl2 N5 3.394(5) no . 2_546 Cl2 C5 3.525(10) no . 2_546 Cl2 C6 3.385(8) no . 2_546 Cl3 O1 3.178(6) no . . Cl3 N1 3.520(8) no . . Cl3 N6 3.458(5) no . . Cl3 C7 3.525(6) no . . Cl4 Cl7 3.448(3) no . 3_667 Cl5 C1 3.579(7) no . 2_646 Cl6 Cl6 3.427(6) no . 3_577 Cl7 Cl4 3.448(3) no . 3_667 Cl7 F1 3.480(5) no . 3_567 Cl7 C9 3.594(7) no . 3_577 F1 Cl7 3.480(5) no . 3_567 F1 O1 3.126(7) no . . F1 C5 3.423(9) no . 1_545 F1 C6 3.127(7) no . 1_545 F1 C11 3.349(7) no . 1_455 F1 C22 3.388(10) no . 3_567 F2 F2 3.204(8) no . 3_567 F2 C12 3.502(7) no . 3_667 F2 C22 2.792(11) no . 3_567 F3 O2 2.627(8) no . . F3 C5 3.173(9) no . 1_545 F3 C16 3.215(7) no . . F3 C18 3.327(7) no . 3_667 F4 Cl1 3.325(4) no . . F4 O1 3.018(8) no . . F4 O2 3.216(9) no . . F4 N1 3.108(10) no . . F4 C7 3.061(7) no . . F4 C16 3.416(7) no . . F5 O1 2.868(7) no . . F5 O2 3.449(8) no . . F5 O4 2.62(2) no . . F5 N1 2.920(9) no . . F5 N14 3.253(6) no . . F5 N15 3.587(5) no . . F5 C1 3.210(7) no . . F5 C3 3.397(7) no . 2_546 F5 C19 3.520(7) no . . F6 C21 3.546(8) no . . F6 C23 3.147(8) no . 1_655 F6 C24 3.436(8) no . 2_656 F7 C3 3.317(8) no . 2_546 F7 C20 3.216(8) no . 2_646 F7 C23 3.133(9) no . 2_546 F8 O2 2.669(8) no . . F8 C10 3.334(7) no . . F8 C24 3.306(9) no . . F9 O3 2.809(18) no . . F9 N13 3.593(10) no . 3_667 F9 N16 3.31(2) no . . F9 C5 3.043(14) no . 1_545 F9 C16 3.330(11) no . . F9 C18 3.237(10) no . 3_667 F9 B2 3.455(12) no . 3_667 F10 F10 2.946(12) no . 3_567 F10 C11 3.574(11) no . 1_455 F10 C12 3.137(12) no . 1_455 F10 C22 3.210(17) no . 3_567 F11 Cl1 3.158(8) no . . F11 O3 2.952(18) no . . F11 O4 2.72(3) no . . F11 N16 2.88(2) no . . F11 C7 3.343(11) no . . F11 C16 3.305(11) no . . F13 O3 2.551(16) no . . F13 N8 3.550(8) no . . F13 N15 3.357(11) no . . F13 N16 2.779(19) no . . F13 C10 2.925(9) no . . F13 C21 3.561(11) no . . F13 C24 3.521(12) no . . F14 Cl2 3.414(6) no . 2_546 F14 C3 3.258(9) no . 2_546 F14 C20 3.597(12) no . 2_646 F14 C23 3.034(10) no . 2_546 F14 C24 3.485(9) no . . F15 C20 3.387(11) no . 2_646 F15 C23 3.436(11) no . 1_655 F15 C24 3.101(11) no . 2_656 O1 Cl3 3.178(6) no . . O1 F1 3.126(7) no . . O1 F4 3.018(8) no . . O1 F5 2.868(7) no . . O1 C2 3.596(9) no . 2_546 O1 C3 3.380(8) no . 2_546 O1 B3 3.423(7) no . . O2 F3 2.627(8) no . . O2 F4 3.216(9) no . . O2 F5 3.449(8) no . . O2 F8 2.669(8) no . . O2 B3 3.444(8) no . . O3 F9 2.809(18) no . . O3 F11 2.952(18) no . . O3 F13 2.551(16) no . . O3 C18 3.543(14) no . 3_667 O3 B3 3.301(14) no . . O3 B4 3.489(14) no . . O4 F5 2.62(2) no . . O4 F11 2.72(3) no . . N1 Cl3 3.520(8) no . . N1 F4 3.108(10) no . . N1 F5 2.920(9) no . . N4 Cl2 3.561(5) no . 2_556 N5 Cl2 3.394(5) no . 2_556 N6 Cl3 3.458(5) no . . N8 F13 3.550(8) no . . N9 C8 3.538(8) no . 1_655 N13 F9 3.593(10) no . 3_667 N14 F5 3.253(6) no . . N15 F5 3.587(5) no . . N15 F13 3.357(11) no . . N16 F9 3.31(2) no . . N16 F11 2.88(2) no . . N16 F13 2.779(19) no . . C1 Cl5 3.579(7) no . 2_656 C1 F5 3.210(7) no . . C2 O1 3.596(9) no . 2_556 C3 F5 3.397(7) no . 2_556 C3 F7 3.317(8) no . 2_556 C3 F14 3.258(9) no . 2_556 C3 O1 3.380(8) no . 2_556 C5 Cl2 3.525(10) no . 2_556 C5 F1 3.423(9) no . 1_565 C5 F3 3.173(9) no . 1_565 C5 F9 3.043(14) no . 1_565 C6 Cl2 3.385(8) no . 2_556 C6 F1 3.127(7) no . 1_565 C7 Cl3 3.525(6) no . . C7 F4 3.061(7) no . . C7 F11 3.343(11) no . . C8 N9 3.538(8) no . 1_455 C9 Cl7 3.594(7) no . 3_577 C9 C21 3.493(7) no . 1_455 C10 F8 3.334(7) no . . C10 F13 2.925(9) no . . C11 F1 3.349(7) no . 1_655 C11 F10 3.574(11) no . 1_655 C12 F2 3.502(7) no . 3_667 C12 F10 3.137(12) no . 1_655 C12 C17 3.573(8) no . 3_667 C15 Cl1 3.466(6) no . 3_677 C16 F3 3.215(7) no . . C16 F4 3.416(7) no . . C16 F9 3.330(11) no . . C16 F11 3.305(11) no . . C17 C12 3.573(8) no . 3_667 C18 F3 3.327(7) no . 3_667 C18 F9 3.237(10) no . 3_667 C18 O3 3.543(14) no . 3_667 C19 F5 3.520(7) no . . C20 F7 3.216(8) no . 2_656 C20 F14 3.597(12) no . 2_656 C20 F15 3.387(11) no . 2_656 C21 F6 3.546(8) no . . C21 F13 3.561(11) no . . C21 C9 3.493(7) no . 1_655 C22 F1 3.388(10) no . 3_567 C22 F2 2.792(11) no . 3_567 C22 F10 3.210(17) no . 3_567 C23 F6 3.147(8) no . 1_455 C23 F7 3.133(9) no . 2_556 C23 F14 3.034(10) no . 2_556 C23 F15 3.436(11) no . 1_455 C24 F6 3.436(8) no . 2_646 C24 F8 3.306(9) no . . C24 F13 3.521(12) no . . C24 F14 3.485(9) no . . C24 F15 3.101(11) no . 2_646 B2 F9 3.455(12) no . 3_667 B3 O1 3.423(7) no . . B3 O2 3.444(8) no . . B3 O3 3.301(14) no . . B4 O3 3.489(14) no . . Ru1 H3 3.3663 no . . Ru1 H6 3.3606 no . . Ru1 H9 3.3637 no . . Ru1 H21 3.2393 no . . Ru2 H12 3.3750 no . . Ru2 H15 3.3559 no . . Ru2 H18 3.3774 no . . Ru2 H23 3.2447 no . . Cl1 H6 3.2344 no . . Cl1 H9 3.1967 no . . Cl1 H15 3.3945 no . . Cl1 H18 3.2284 no . . O1 H3 3.5221 no . . O1 H9 3.5488 no . . O2 H12 3.2544 no . . O2 H18 3.3279 no . . O3 H12 3.1893 no . . O4 H3 3.2004 no . . O4 H9 3.4973 no . . N1 H3 3.1837 no . . N1 H9 3.2021 no . . N2 H1 3.41(6) no . . N2 H4 3.1202 no . . N2 H5 3.1112 no . . N2 H21 2.8193 no . . N3 H3 3.1003 no . . N3 H4 3.1206 no . . N4 H1 3.37(6) no . . N4 H7 3.1475 no . . N4 H8 3.1157 no . . N4 H21 3.2754 no . . N5 H6 3.0659 no . . N5 H7 3.1051 no . . N6 H1 3.39(6) no . . N6 H10 3.1442 no . . N6 H11 3.1125 no . . N7 H9 3.1088 no . . N7 H10 3.1329 no . . N8 H2 3.43(7) no . . N8 H13 3.1483 no . . N8 H14 3.1272 no . . N8 H23 2.8534 no . . N9 H12 3.1071 no . . N9 H13 3.1375 no . . N10 H2 3.42(7) no . . N10 H16 3.1523 no . . N10 H17 3.1139 no . . N10 H23 3.3345 no . . N11 H15 3.0823 no . . N11 H16 3.1262 no . . N12 H2 3.45(7) no . . N12 H19 3.1443 no . . N12 H20 3.1114 no . . N13 H18 3.0995 no . . N13 H19 3.1242 no . . N14 H3 3.2866 no . . N14 H6 3.1335 no . . N14 H15 3.4617 no . . N14 H22 3.1511 no . . N14 H23 3.1111 no . . N15 H6 3.5891 no . . N15 H12 3.3455 no . . N15 H15 3.0626 no . . N15 H21 3.1087 no . . N15 H22 3.1493 no . . N16 H12 3.0033 no . . N16 H18 3.2344 no . . C1 H5 3.1110 no . . C1 H21 2.8229 no . . C3 H1 2.83(6) no . . C3 H3 3.1093 no . . C4 H8 3.1145 no . . C4 H15 3.0206 no . . C6 H1 2.74(6) no . . C6 H6 3.1078 no . . C7 H11 3.1235 no . . C9 H1 2.83(6) no . . C9 H9 3.1227 no . . C10 H14 3.1235 no . . C10 H23 2.8819 no . . C12 H2 2.80(7) no . . C12 H12 3.1208 no . . C13 H6 2.9730 no . . C13 H17 3.1108 no . . C15 H2 2.80(7) no . . C15 H15 3.1071 no . . C16 H20 3.1091 no . . C18 H2 2.90(7) no . . C18 H18 3.1073 no . . C19 H3 3.1141 no . . C19 H6 3.4972 no . . C19 H23 3.0986 no . . C21 H12 3.2057 no . . C21 H15 3.3645 no . . C21 H21 3.0969 no . . B1 H5 2.9225 no . . B1 H8 2.8997 no . . B1 H11 2.9384 no . . B2 H14 2.9379 no . . B2 H17 2.9296 no . . B2 H20 2.9443 no . . H1 H5 2.7869 no . . H1 H8 2.6795 no . . H1 H11 2.7895 no . . H2 H14 2.7410 no . . H2 H17 2.7248 no . . H2 H20 2.8502 no . . H3 H4 2.4952 no . . H3 H21 2.7767 no . . H4 H5 2.4879 no . . H6 H7 2.5333 no . . H6 H15 2.0766 no . . H7 H8 2.4991 no . . H9 H10 2.5164 no . . H10 H11 2.5046 no . . H12 H13 2.5143 no . . H12 H23 2.8203 no . . H13 H14 2.5041 no . . H15 H16 2.5174 no . . H16 H17 2.5026 no . . H18 H19 2.5046 no . . H19 H20 2.4849 no . . H21 H22 2.5079 no . . H22 H23 2.4865 no . . Cl1 H16 3.3407 no . 3_677 Cl1 H17 2.9536 no . 3_677 Cl2 H21 2.9038 no . 2_546 Cl2 H28 3.5499 no . 2_556 Cl2 H29 3.2830 no . 2_556 Cl3 H12 3.4609 no . 1_455 Cl3 H13 3.4132 no . 1_455 Cl3 H23 3.3513 no . 1_455 Cl4 H6 3.3603 no . 1_545 Cl4 H11 3.5563 no . 1_645 Cl4 H15 3.3804 no . 1_545 Cl4 H19 3.4118 no . 3_667 Cl4 H20 3.4623 no . 3_667 Cl5 H3 3.0709 no . 2_646 Cl5 H4 3.4693 no . 2_646 Cl5 H12 3.2875 no . . Cl5 H13 3.2482 no . . Cl5 H21 3.5239 no . 2_646 Cl6 H2 3.49(7) no . 1_455 Cl6 H9 3.1907 no . . Cl6 H16 3.5694 no . 3_677 Cl6 H17 3.2033 no . 1_455 Cl6 H17 3.4732 no . 3_677 Cl7 H8 3.3653 no . 3_577 Cl7 H11 3.2528 no . 3_577 Cl7 H13 3.4482 no . 3_667 Cl7 H16 3.2765 no . 3_677 Cl7 H19 3.2330 no . . F1 H4 3.2579 no . 2_546 F1 H7 3.1235 no . 1_545 F1 H8 2.4506 no . 1_545 F1 H13 2.5678 no . 1_455 F1 H14 3.5154 no . 1_455 F1 H24 3.3791 no . 3_567 F1 H25 2.8654 no . 3_567 F2 H2 3.20(7) no . 3_667 F2 H14 2.9183 no . 1_455 F2 H14 2.7023 no . 3_667 F2 H18 3.0068 no . . F2 H24 3.1615 no . . F2 H24 2.2590 no . 3_567 F2 H25 2.4671 no . 3_567 F3 H2 3.31(7) no . 3_667 F3 H7 2.3490 no . 1_545 F3 H18 2.6930 no . . F3 H20 2.5615 no . 3_667 F3 H25 3.4222 no . 3_567 F4 H9 2.1912 no . . F4 H13 3.4965 no . 1_455 F4 H14 3.1184 no . 1_455 F4 H18 2.5231 no . . F4 H24 3.3822 no . . F5 H3 2.3764 no . . F5 H5 2.4576 no . 2_546 F5 H28 3.5859 no . 2_656 F6 H12 3.0862 no . . F6 H22 3.0796 no . 2_646 F6 H27 2.1590 no . 1_655 F6 H28 2.5081 no . 2_656 F7 H1 3.56(5) no . 2_546 F7 H5 2.7396 no . 2_546 F7 H22 2.2726 no . 2_646 F7 H26 2.2050 no . 2_546 F7 H27 3.4600 no . 2_546 F7 H28 3.5563 no . 2_656 F7 H29 2.8830 no . . F8 H12 2.5326 no . . F8 H29 2.4792 no . . F9 H2 2.70(7) no . 3_667 F9 H7 2.2999 no . 1_545 F9 H8 3.5493 no . 1_545 F9 H14 3.5785 no . 3_667 F9 H18 2.7951 no . . F9 H20 2.5562 no . 3_667 F9 H24 3.5434 no . 3_567 F9 H25 2.8459 no . 3_567 F10 H9 3.4584 no . . F10 H13 3.3177 no . 1_455 F10 H14 2.3503 no . 1_455 F10 H14 3.0825 no . 3_667 F10 H18 2.9495 no . . F10 H24 2.7606 no . . F10 H24 2.5854 no . 3_567 F10 H25 2.9946 no . 3_567 F11 H9 2.5530 no . . F11 H18 2.4972 no . . F13 H12 2.0676 no . . F13 H27 3.4735 no . 1_655 F13 H29 2.7910 no . . F14 H5 2.6774 no . 2_546 F14 H22 2.6794 no . 2_646 F14 H26 2.1887 no . 2_546 F14 H27 3.3891 no . 2_546 F14 H29 2.5259 no . . F15 H22 2.6098 no . 2_646 F15 H27 2.4741 no . 1_655 F15 H28 2.1330 no . 2_656 F15 H29 3.4927 no . 2_656 O1 H4 3.2353 no . 2_546 O1 H5 2.7595 no . 2_546 O3 H7 2.9804 no . 1_545 O3 H20 2.7456 no . 3_667 O4 H5 3.4014 no . 2_546 N1 H5 3.5300 no . 2_546 N8 H10 3.0088 no . 1_655 N8 H19 3.2417 no . 3_667 N9 H10 2.7509 no . 1_655 N9 H19 3.0545 no . 3_667 N10 H10 2.9148 no . 1_655 N11 H10 2.6831 no . 1_655 N12 H16 3.0418 no . 3_677 N13 H16 3.3867 no . 3_677 N16 H20 3.3238 no . 3_667 C2 H8 3.3688 no . 2_546 C3 H26 3.4586 no . . C5 H2 3.48(7) no . 3_677 C5 H20 3.2512 no . 3_677 C5 H25 3.0915 no . 3_577 C6 H4 3.2614 no . 2_556 C6 H25 2.9918 no . 3_577 C8 H23 2.8361 no . 1_455 C9 H23 2.8173 no . 1_455 C10 H10 3.4439 no . 1_655 C10 H19 3.1121 no . 3_667 C11 H9 3.5575 no . 1_655 C11 H10 3.5139 no . 1_655 C11 H19 2.8473 no . 3_667 C12 H9 3.2559 no . 1_655 C12 H10 3.0867 no . 1_655 C12 H19 2.8074 no . 3_667 C13 H10 3.2144 no . 1_655 C14 H10 3.2373 no . 1_655 C15 H10 2.8823 no . 1_655 C16 H16 2.8862 no . 3_677 C17 H16 3.1823 no . 3_677 C18 H7 3.2870 no . 3_677 C18 H16 3.4588 no . 3_677 C20 H11 3.3785 no . 1_655 C20 H26 3.2444 no . 1_655 C20 H27 3.3564 no . 1_655 C21 H10 3.4547 no . 1_655 C21 H11 3.0968 no . 1_655 C21 H26 3.5395 no . 1_655 C21 H27 3.3832 no . 1_655 C22 H2 3.34(7) no . 1_455 C22 H14 3.5868 no . 1_455 C23 H22 3.3404 no . 1_455 C23 H23 3.4389 no . 1_455 C23 H28 3.5184 no . 2_556 C23 H29 3.3920 no . 2_556 C24 H27 3.4972 no . 2_546 B2 H10 3.2017 no . 1_655 B3 H7 3.2200 no . 1_545 B3 H8 3.5318 no . 1_545 B3 H9 3.4688 no . . B3 H13 3.4009 no . 1_455 B3 H14 3.3465 no . 1_455 B3 H18 2.8700 no . . B3 H24 3.3458 no . 3_567 B3 H25 3.0612 no . 3_567 B4 H5 3.0853 no . 2_546 B4 H12 3.3521 no . . B4 H22 3.1952 no . 2_646 B4 H26 3.5346 no . 2_546 B4 H27 3.5217 no . 1_655 B4 H28 3.3562 no . 2_656 B4 H29 3.1313 no . . H1 F7 3.56(5) no . 2_556 H1 H3 3.4305 no . 2_556 H2 Cl6 3.49(7) no . 1_655 H2 F2 3.20(7) no . 3_667 H2 F3 3.31(7) no . 3_667 H2 F9 2.70(7) no . 3_667 H2 C5 3.48(7) no . 3_677 H2 C22 3.34(7) no . 1_655 H2 H7 3.1564 no . 3_677 H2 H10 3.5341 no . 1_655 H2 H24 3.4562 no . 1_655 H2 H25 2.6925 no . 1_655 H3 Cl5 3.0709 no . 2_656 H3 F5 2.3764 no . . H3 H1 3.4305 no . 2_546 H3 H5 3.2847 no . 2_546 H4 Cl5 3.4693 no . 2_656 H4 F1 3.2579 no . 2_556 H4 O1 3.2353 no . 2_556 H4 C6 3.2614 no . 2_546 H4 H8 2.5245 no . 2_546 H5 F5 2.4576 no . 2_556 H5 F7 2.7396 no . 2_556 H5 F14 2.6774 no . 2_556 H5 O1 2.7595 no . 2_556 H5 O4 3.4014 no . 2_556 H5 N1 3.5300 no . 2_556 H5 B4 3.0853 no . 2_556 H5 H3 3.2847 no . 2_556 H5 H26 3.4728 no . . H6 Cl4 3.3603 no . 1_565 H6 H17 3.4361 no . 3_677 H6 H20 3.5562 no . 3_677 H7 F1 3.1235 no . 1_565 H7 F3 2.3490 no . 1_565 H7 F9 2.2999 no . 1_565 H7 O3 2.9804 no . 1_565 H7 C18 3.2870 no . 3_677 H7 B3 3.2200 no . 1_565 H7 H2 3.1564 no . 3_677 H7 H20 2.4418 no . 3_677 H7 H25 3.1886 no . 3_577 H8 Cl7 3.3653 no . 3_577 H8 F1 2.4506 no . 1_565 H8 F9 3.5493 no . 1_565 H8 C2 3.3688 no . 2_556 H8 B3 3.5318 no . 1_565 H8 H4 2.5245 no . 2_556 H8 H25 2.9845 no . 3_577 H9 Cl6 3.1907 no . . H9 F4 2.1912 no . . H9 F10 3.4584 no . . H9 F11 2.5530 no . . H9 C11 3.5575 no . 1_455 H9 C12 3.2559 no . 1_455 H9 B3 3.4688 no . . H9 H14 3.1169 no . 1_455 H10 N8 3.0088 no . 1_455 H10 N9 2.7509 no . 1_455 H10 N10 2.9148 no . 1_455 H10 N11 2.6831 no . 1_455 H10 C10 3.4439 no . 1_455 H10 C11 3.5139 no . 1_455 H10 C12 3.0867 no . 1_455 H10 C13 3.2144 no . 1_455 H10 C14 3.2373 no . 1_455 H10 C15 2.8823 no . 1_455 H10 C21 3.4547 no . 1_455 H10 B2 3.2017 no . 1_455 H10 H2 3.5341 no . 1_455 H10 H14 3.4896 no . 1_455 H10 H17 3.2880 no . 1_455 H10 H23 2.6957 no . 1_455 H11 Cl4 3.5563 no . 1_465 H11 Cl7 3.2528 no . 3_577 H11 C20 3.3785 no . 1_455 H11 C21 3.0968 no . 1_455 H11 H22 3.2451 no . 1_455 H11 H23 2.6514 no . 1_455 H12 Cl3 3.4609 no . 1_655 H12 Cl5 3.2875 no . . H12 F6 3.0862 no . . H12 F8 2.5326 no . . H12 F13 2.0676 no . . H12 B4 3.3521 no . . H12 H27 3.4049 no . 1_655 H12 H29 3.5913 no . . H13 Cl3 3.4132 no . 1_655 H13 Cl5 3.2482 no . . H13 Cl7 3.4482 no . 3_667 H13 F1 2.5678 no . 1_655 H13 F4 3.4965 no . 1_655 H13 F10 3.3177 no . 1_655 H13 B3 3.4009 no . 1_655 H13 H19 3.2280 no . 3_667 H14 F1 3.5154 no . 1_655 H14 F2 2.9183 no . 1_655 H14 F2 2.7023 no . 3_667 H14 F4 3.1184 no . 1_655 H14 F9 3.5785 no . 3_667 H14 F10 2.3503 no . 1_655 H14 F10 3.0825 no . 3_667 H14 C22 3.5868 no . 1_655 H14 B3 3.3465 no . 1_655 H14 H9 3.1169 no . 1_655 H14 H10 3.4896 no . 1_655 H14 H19 3.1622 no . 3_667 H14 H24 2.9571 no . 1_655 H14 H24 3.4506 no . 3_667 H14 H25 3.5550 no . 1_655 H15 Cl4 3.3804 no . 1_565 H16 Cl1 3.3407 no . 3_677 H16 Cl6 3.5694 no . 3_677 H16 Cl7 3.2765 no . 3_677 H16 N12 3.0418 no . 3_677 H16 N13 3.3867 no . 3_677 H16 C16 2.8862 no . 3_677 H16 C17 3.1823 no . 3_677 H16 C18 3.4588 no . 3_677 H16 H18 3.1380 no . 3_677 H17 Cl1 2.9536 no . 3_677 H17 Cl6 3.2033 no . 1_655 H17 Cl6 3.4732 no . 3_677 H17 H6 3.4361 no . 3_677 H17 H10 3.2880 no . 1_655 H18 F2 3.0068 no . . H18 F3 2.6930 no . . H18 F4 2.5231 no . . H18 F9 2.7951 no . . H18 F10 2.9495 no . . H18 F11 2.4972 no . . H18 B3 2.8700 no . . H18 H16 3.1380 no . 3_677 H18 H24 3.0847 no . . H19 Cl4 3.4118 no . 3_667 H19 Cl7 3.2330 no . . H19 N8 3.2417 no . 3_667 H19 N9 3.0545 no . 3_667 H19 C10 3.1121 no . 3_667 H19 C11 2.8473 no . 3_667 H19 C12 2.8074 no . 3_667 H19 H13 3.2280 no . 3_667 H19 H14 3.1622 no . 3_667 H20 Cl4 3.4623 no . 3_667 H20 F3 2.5615 no . 3_667 H20 F9 2.5562 no . 3_667 H20 O3 2.7456 no . 3_667 H20 N16 3.3238 no . 3_667 H20 C5 3.2512 no . 3_677 H20 H6 3.5562 no . 3_677 H20 H7 2.4418 no . 3_677 H21 Cl2 2.9038 no . 2_556 H21 Cl5 3.5239 no . 2_656 H21 H27 3.5134 no . 2_556 H22 F6 3.0796 no . 2_656 H22 F7 2.2726 no . 2_656 H22 F14 2.6794 no . 2_656 H22 F15 2.6098 no . 2_656 H22 C23 3.3404 no . 1_655 H22 B4 3.1952 no . 2_656 H22 H11 3.2451 no . 1_655 H22 H26 2.6494 no . 1_655 H22 H27 3.1417 no . 1_655 H22 H28 3.3122 no . 1_565 H22 H29 3.5482 no . 2_656 H23 Cl3 3.3513 no . 1_655 H23 C8 2.8361 no . 1_655 H23 C9 2.8173 no . 1_655 H23 C23 3.4389 no . 1_655 H23 H10 2.6957 no . 1_655 H23 H11 2.6514 no . 1_655 H23 H26 3.2347 no . 1_655 H23 H27 3.1698 no . 1_655 H24 F1 3.3791 no . 3_567 H24 F2 3.1615 no . . H24 F2 2.2590 no . 3_567 H24 F4 3.3822 no . . H24 F9 3.5434 no . 3_567 H24 F10 2.7606 no . . H24 F10 2.5854 no . 3_567 H24 B3 3.3458 no . 3_567 H24 H2 3.4562 no . 1_455 H24 H14 2.9571 no . 1_455 H24 H14 3.4506 no . 3_667 H24 H18 3.0847 no . . H25 F1 2.8654 no . 3_567 H25 F2 2.4671 no . 3_567 H25 F3 3.4222 no . 3_567 H25 F9 2.8459 no . 3_567 H25 F10 2.9946 no . 3_567 H25 C5 3.0915 no . 3_577 H25 C6 2.9918 no . 3_577 H25 B3 3.0612 no . 3_567 H25 H2 2.6925 no . 1_455 H25 H7 3.1886 no . 3_577 H25 H8 2.9845 no . 3_577 H25 H14 3.5550 no . 1_455 H26 F7 2.2050 no . 2_556 H26 F14 2.1887 no . 2_556 H26 C3 3.4586 no . . H26 C20 3.2444 no . 1_455 H26 C21 3.5395 no . 1_455 H26 B4 3.5346 no . 2_556 H26 H5 3.4728 no . . H26 H22 2.6494 no . 1_455 H26 H23 3.2347 no . 1_455 H26 H29 3.1706 no . 2_556 H27 F6 2.1590 no . 1_455 H27 F7 3.4600 no . 2_556 H27 F13 3.4735 no . 1_455 H27 F14 3.3891 no . 2_556 H27 F15 2.4741 no . 1_455 H27 C20 3.3564 no . 1_455 H27 C21 3.3832 no . 1_455 H27 C24 3.4972 no . 2_556 H27 B4 3.5217 no . 1_455 H27 H12 3.4049 no . 1_455 H27 H21 3.5134 no . 2_546 H27 H22 3.1417 no . 1_455 H27 H23 3.1698 no . 1_455 H27 H28 2.8909 no . 2_556 H27 H29 3.1594 no . 2_556 H28 Cl2 3.5499 no . 2_546 H28 F5 3.5859 no . 2_646 H28 F6 2.5081 no . 2_646 H28 F7 3.5563 no . 2_646 H28 F15 2.1330 no . 2_646 H28 C23 3.5184 no . 2_546 H28 B4 3.3562 no . 2_646 H28 H22 3.3122 no . 1_545 H28 H27 2.8909 no . 2_546 H29 Cl2 3.2830 no . 2_546 H29 F7 2.8830 no . . H29 F8 2.4792 no . . H29 F13 2.7910 no . . H29 F14 2.5259 no . . H29 F15 3.4927 no . 2_646 H29 C23 3.3920 no . 2_546 H29 B4 3.1313 no . . H29 H12 3.5913 no . . H29 H22 3.5482 no . 2_646 H29 H26 3.1706 no . 2_546 H29 H27 3.1594 no . 2_546 #============================================================================== #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== _database_code_depnum_ccdc_archive 'CCDC 939835'