# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # 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_4_0.5Cl_0.5PF6 _database_code_depnum_ccdc_archive 'CCDC 879776' #TrackingRef '11030_web_deposit_cif_file_0_WylieO_1335892389.Ohara_O_Lough_Morris_SI.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C16 H25 Cl N3 Ru), F6 P, C2 H3 N, Cl' _chemical_formula_sum 'C34 H53 Cl3 F6 N7 P Ru2' _chemical_formula_weight 1013.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.9637(3) _cell_length_b 26.6595(4) _cell_length_c 9.9118(7) _cell_angle_alpha 90 _cell_angle_beta 98.4270(13) _cell_angle_gamma 90 _cell_volume 4172.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 47538 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.613 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2056 _exptl_absorpt_coefficient_mu 1.016 # Absorption correction _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.604 _exptl_absorpt_correction_T_max 0.929 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f scans and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_reflns_number 35004 _diffrn_reflns_av_R_equivalents 0.0968 _diffrn_reflns_av_sigmaI/netI 0.0709 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7317 _reflns_number_gt 5380 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Collect (Nonius B.V., 1997-2002)' _computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction Denzo-SMN _computing_structure_solution 'SIR-92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXTL V6.1 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material 'SHELXTL V6.1' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0624P)^2^+17.7263P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7317 _refine_ls_number_parameters 486 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0828 _refine_ls_R_factor_gt 0.0530 _refine_ls_wR_factor_ref 0.1484 _refine_ls_wR_factor_gt 0.1226 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1A Ru 0.34007(3) 0.584362(16) 0.79928(5) 0.02647(15) Uani 1 1 d . . . Cl1A Cl 0.43490(10) 0.65195(5) 0.76300(16) 0.0345(4) Uani 1 1 d . . . N1A N 0.2361(3) 0.67706(18) 0.8650(5) 0.0364(12) Uani 1 1 d . . . N2A N 0.2805(3) 0.63406(18) 1.0449(5) 0.0344(12) Uani 1 1 d . . . N3A N 0.4276(3) 0.57162(17) 0.9817(5) 0.0300(11) Uani 1 1 d . . . H3AB H 0.4255 0.5379 1.0008 0.036 Uiso 1 1 calc R . . H3AC H 0.4809 0.5778 0.9605 0.036 Uiso 1 1 calc R . . C1A C 0.2828(4) 0.6357(2) 0.9083(6) 0.0302(14) Uani 1 1 d . . . C2A C 0.2047(4) 0.6993(2) 0.9730(7) 0.0432(17) Uani 1 1 d . . . H2AA H 0.1699 0.7283 0.9682 0.052 Uiso 1 1 calc R . . C3A C 0.2321(4) 0.6727(2) 1.0860(7) 0.0409(16) Uani 1 1 d . . . H3AA H 0.2205 0.6790 1.1758 0.049 Uiso 1 1 calc R . . C4A C 0.2212(5) 0.6963(2) 0.7261(7) 0.0459(17) Uani 1 1 d . . . H4AA H 0.2629 0.6818 0.6738 0.069 Uiso 1 1 calc R . . H4AB H 0.2268 0.7329 0.7277 0.069 Uiso 1 1 calc R . . H4AC H 0.1641 0.6870 0.6832 0.069 Uiso 1 1 calc R . . C5A C 0.3303(4) 0.5986(2) 1.1368(6) 0.0335(14) Uani 1 1 d . . . H5AA H 0.3061 0.5645 1.1222 0.040 Uiso 1 1 calc R . . H5AB H 0.3282 0.6083 1.2327 0.040 Uiso 1 1 calc R . . C6A C 0.4215(4) 0.5986(2) 1.1097(6) 0.0343(15) Uani 1 1 d . . . H6AA H 0.4414 0.6335 1.1028 0.041 Uiso 1 1 calc R . . H6AB H 0.4581 0.5821 1.1863 0.041 Uiso 1 1 calc R . . C7A C 0.3607(4) 0.5474(2) 0.6018(6) 0.0334(14) Uani 1 1 d . . . C8A C 0.2842(4) 0.5764(2) 0.5835(6) 0.0350(15) Uani 1 1 d . . . H8AA H 0.2801 0.6065 0.5228 0.042 Uiso 1 1 calc R . . C9A C 0.2209(4) 0.5680(2) 0.6653(6) 0.0355(15) Uani 1 1 d . . . H9AA H 0.1735 0.5927 0.6612 0.043 Uiso 1 1 calc R . . C10A C 0.2316(4) 0.5319(2) 0.7746(6) 0.0352(15) Uani 1 1 d . . . C11A C 0.3094(4) 0.5053(2) 0.7931(6) 0.0310(14) Uani 1 1 d . . . H11A H 0.3244 0.4852 0.8784 0.037 Uiso 1 1 calc R . . C12A C 0.3722(4) 0.5117(2) 0.7060(6) 0.0319(14) Uani 1 1 d . . . H12A H 0.4297 0.4968 0.7335 0.038 Uiso 1 1 calc R . . C13A C 0.4282(4) 0.5574(2) 0.5150(7) 0.0449(17) Uani 1 1 d . . . H13A H 0.4152 0.5391 0.4288 0.067 Uiso 1 1 calc R . . H13B H 0.4831 0.5462 0.5631 0.067 Uiso 1 1 calc R . . H13C H 0.4306 0.5934 0.4964 0.067 Uiso 1 1 calc R . . C14A C 0.1665(4) 0.5208(3) 0.8662(7) 0.0454(17) Uani 1 1 d . . . H14A H 0.1973 0.5176 0.9612 0.054 Uiso 1 1 calc R . . C15A C 0.1000(5) 0.5622(3) 0.8679(9) 0.062(2) Uani 1 1 d . . . H15A H 0.1284 0.5945 0.8884 0.094 Uiso 1 1 calc R . . H15B H 0.0644 0.5546 0.9379 0.094 Uiso 1 1 calc R . . H15C H 0.0646 0.5640 0.7784 0.094 Uiso 1 1 calc R . . C16A C 0.1250(5) 0.4700(3) 0.8274(8) 0.058(2) Uani 1 1 d . . . H16A H 0.1686 0.4439 0.8338 0.087 Uiso 1 1 calc R . . H16B H 0.0951 0.4715 0.7338 0.087 Uiso 1 1 calc R . . H16C H 0.0846 0.4620 0.8898 0.087 Uiso 1 1 calc R . . Ru1B Ru 0.26957(3) 0.353507(18) 0.37897(5) 0.03253(16) Uani 1 1 d . . . Cl1B Cl 0.30275(12) 0.26546(6) 0.38420(18) 0.0498(5) Uani 1 1 d . . . N1B N 0.1043(4) 0.3142(2) 0.2111(6) 0.0494(15) Uani 1 1 d . . . N2B N 0.1843(3) 0.34773(19) 0.0816(5) 0.0393(13) Uani 1 1 d . . . N3B N 0.3596(3) 0.35710(18) 0.2394(5) 0.0335(12) Uani 1 1 d . . . H3BB H 0.3771 0.3899 0.2368 0.040 Uiso 1 1 calc R . . H3BC H 0.4061 0.3387 0.2766 0.040 Uiso 1 1 calc R . . C1B C 0.1815(4) 0.3366(2) 0.2134(6) 0.0332(14) Uani 1 1 d . . . C2B C 0.0605(5) 0.3130(3) 0.0799(8) 0.058(2) Uani 1 1 d . . . H2BA H 0.0053 0.2998 0.0530 0.069 Uiso 1 1 calc R . . C3B C 0.1105(5) 0.3338(3) -0.0020(7) 0.053(2) Uani 1 1 d . . . H3BA H 0.0980 0.3381 -0.0980 0.064 Uiso 1 1 calc R . . C4B C 0.0713(5) 0.2905(3) 0.3294(8) 0.060(2) Uani 1 1 d . . . H4BA H 0.1180 0.2855 0.4041 0.090 Uiso 1 1 calc R . . H4BB H 0.0457 0.2580 0.3015 0.090 Uiso 1 1 calc R . . H4BC H 0.0285 0.3123 0.3601 0.090 Uiso 1 1 calc R . . C5B C 0.2597(4) 0.3667(3) 0.0306(7) 0.0448(17) Uani 1 1 d . . . H5BA H 0.2652 0.4032 0.0485 0.054 Uiso 1 1 calc R . . H5BB H 0.2538 0.3615 -0.0693 0.054 Uiso 1 1 calc R . . C6B C 0.3367(4) 0.3405(2) 0.0981(7) 0.0400(16) Uani 1 1 d . . . H6BA H 0.3264 0.3039 0.0964 0.048 Uiso 1 1 calc R . . H6BB H 0.3844 0.3472 0.0470 0.048 Uiso 1 1 calc R . . C7B C 0.3243(4) 0.3636(2) 0.6010(7) 0.0411(16) Uani 1 1 d . . . C8B C 0.3493(4) 0.4035(2) 0.5266(7) 0.0386(15) Uani 1 1 d . . . H8BA H 0.4108 0.4063 0.5185 0.046 Uiso 1 1 calc R . . C9B C 0.2916(4) 0.4318(2) 0.4355(7) 0.0363(15) Uani 1 1 d . . . H9BA H 0.3136 0.4553 0.3701 0.044 Uiso 1 1 calc R . . C10B C 0.2044(4) 0.4226(2) 0.4232(6) 0.0336(14) Uani 1 1 d . . . C11B C 0.1767(4) 0.3826(2) 0.5025(7) 0.0411(16) Uani 1 1 d . . . H11B H 0.1166 0.3709 0.4824 0.049 Uiso 1 1 calc R . . C12B C 0.2358(4) 0.3530(2) 0.5861(7) 0.0436(17) Uani 1 1 d . . . H12B H 0.2165 0.3209 0.6237 0.052 Uiso 1 1 calc R . . C13B C 0.3872(5) 0.3308(3) 0.6889(7) 0.0529(19) Uani 1 1 d . . . H13D H 0.3838 0.3372 0.7853 0.079 Uiso 1 1 calc R . . H13E H 0.4445 0.3384 0.6705 0.079 Uiso 1 1 calc R . . H13F H 0.3743 0.2954 0.6681 0.079 Uiso 1 1 calc R . . C14B C 0.1376(4) 0.4533(2) 0.3324(7) 0.0440(17) Uani 1 1 d . . . H14B H 0.0989 0.4291 0.2769 0.053 Uiso 1 1 calc R . . C15B C 0.1735(6) 0.4880(4) 0.2340(9) 0.078(3) Uani 1 1 d . . . H15D H 0.2104 0.4689 0.1821 0.117 Uiso 1 1 calc R . . H15E H 0.2062 0.5147 0.2853 0.117 Uiso 1 1 calc R . . H15F H 0.1270 0.5029 0.1711 0.117 Uiso 1 1 calc R . . C16B C 0.0850(4) 0.4821(3) 0.4232(8) 0.0505(18) Uani 1 1 d . . . H16D H 0.0543 0.4584 0.4735 0.076 Uiso 1 1 calc R . . H16E H 0.0444 0.5037 0.3665 0.076 Uiso 1 1 calc R . . H16F H 0.1225 0.5028 0.4878 0.076 Uiso 1 1 calc R . . P1 P -0.05925(11) 0.34273(6) 0.64140(18) 0.0374(4) Uani 1 1 d . . . F1 F -0.1592(3) 0.3484(2) 0.6116(5) 0.0813(16) Uani 1 1 d . . . F2 F 0.0406(2) 0.33477(19) 0.6684(4) 0.0648(12) Uani 1 1 d . . . F3 F -0.0668(3) 0.29321(16) 0.5494(5) 0.0712(13) Uani 1 1 d . . . F4 F -0.0680(3) 0.30919(17) 0.7728(4) 0.0616(12) Uani 1 1 d . . . F5 F -0.0517(4) 0.39035(18) 0.7334(6) 0.0953(18) Uani 1 1 d . . . F6 F -0.0505(3) 0.37445(16) 0.5077(4) 0.0618(12) Uani 1 1 d . . . Cl1 Cl 0.40395(10) 0.46985(5) 0.14870(17) 0.0369(4) Uani 1 1 d . . . N1S N 0.3811(5) 0.6877(3) 0.3703(8) 0.079(2) Uani 1 1 d . . . C1S C 0.4087(5) 0.7171(3) 0.4450(8) 0.0531(19) Uani 1 1 d . . . C2S C 0.4447(5) 0.7553(2) 0.5397(8) 0.057(2) Uani 1 1 d . . . H2S1 H 0.4099 0.7588 0.6129 0.085 Uiso 1 1 calc R . . H2S2 H 0.4460 0.7873 0.4916 0.085 Uiso 1 1 calc R . . H2S3 H 0.5024 0.7457 0.5788 0.085 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1A 0.0316(3) 0.0212(2) 0.0251(3) 0.00038(19) -0.0009(2) 0.00109(19) Cl1A 0.0407(9) 0.0260(7) 0.0367(8) 0.0023(6) 0.0051(7) -0.0029(6) N1A 0.047(3) 0.030(3) 0.030(3) 0.002(2) 0.000(2) 0.015(2) N2A 0.042(3) 0.029(3) 0.031(3) -0.001(2) 0.003(2) 0.001(2) N3A 0.029(3) 0.026(2) 0.032(3) 0.000(2) -0.004(2) 0.001(2) C1A 0.037(3) 0.018(3) 0.034(3) -0.004(2) 0.001(3) 0.000(2) C2A 0.039(4) 0.035(3) 0.054(5) -0.010(3) 0.004(3) 0.011(3) C3A 0.051(4) 0.036(4) 0.035(4) -0.009(3) 0.004(3) 0.009(3) C4A 0.053(4) 0.039(4) 0.043(4) 0.003(3) -0.003(3) 0.009(3) C5A 0.047(4) 0.030(3) 0.024(3) -0.002(3) 0.005(3) 0.004(3) C6A 0.044(4) 0.028(3) 0.027(3) 0.001(3) -0.009(3) 0.002(3) C7A 0.049(4) 0.024(3) 0.025(3) -0.007(3) 0.002(3) -0.005(3) C8A 0.045(4) 0.025(3) 0.031(3) 0.002(3) -0.008(3) 0.001(3) C9A 0.040(4) 0.035(3) 0.029(3) -0.009(3) -0.005(3) 0.001(3) C10A 0.033(3) 0.035(3) 0.034(4) -0.007(3) -0.007(3) -0.006(3) C11A 0.041(4) 0.026(3) 0.024(3) 0.000(2) -0.003(3) -0.008(3) C12A 0.036(3) 0.024(3) 0.035(3) -0.010(3) 0.002(3) 0.006(2) C13A 0.056(4) 0.038(4) 0.043(4) -0.008(3) 0.015(3) 0.000(3) C14A 0.041(4) 0.057(4) 0.038(4) 0.000(3) 0.006(3) -0.015(3) C15A 0.043(4) 0.079(6) 0.070(6) -0.017(5) 0.024(4) -0.012(4) C16A 0.046(4) 0.067(5) 0.058(5) 0.021(4) -0.005(4) -0.021(4) Ru1B 0.0390(3) 0.0284(3) 0.0289(3) -0.0012(2) 0.0007(2) -0.0007(2) Cl1B 0.0720(12) 0.0293(8) 0.0488(11) 0.0078(7) 0.0107(9) 0.0056(8) N1B 0.049(4) 0.052(3) 0.047(4) -0.016(3) 0.005(3) -0.017(3) N2B 0.045(3) 0.041(3) 0.030(3) -0.001(2) -0.001(3) -0.009(2) N3B 0.039(3) 0.029(3) 0.031(3) 0.002(2) 0.001(2) -0.004(2) C1B 0.033(3) 0.028(3) 0.037(4) -0.005(3) -0.001(3) -0.003(3) C2B 0.043(4) 0.077(5) 0.050(5) -0.020(4) -0.001(4) -0.012(4) C3B 0.055(5) 0.069(5) 0.031(4) -0.014(4) -0.010(4) -0.010(4) C4B 0.068(5) 0.066(5) 0.049(5) -0.013(4) 0.019(4) -0.037(4) C5B 0.053(4) 0.049(4) 0.033(4) 0.001(3) 0.005(3) -0.013(3) C6B 0.049(4) 0.035(3) 0.036(4) -0.007(3) 0.007(3) -0.005(3) C7B 0.049(4) 0.044(4) 0.029(4) -0.003(3) -0.001(3) -0.009(3) C8B 0.036(4) 0.042(4) 0.039(4) -0.004(3) 0.009(3) -0.007(3) C9B 0.045(4) 0.025(3) 0.040(4) -0.005(3) 0.009(3) -0.007(3) C10B 0.044(4) 0.027(3) 0.032(3) -0.010(3) 0.014(3) 0.003(3) C11B 0.039(4) 0.051(4) 0.035(4) -0.005(3) 0.008(3) -0.007(3) C12B 0.056(4) 0.044(4) 0.032(4) 0.002(3) 0.008(3) -0.010(3) C13B 0.058(5) 0.059(5) 0.037(4) 0.011(3) -0.010(3) -0.005(4) C14B 0.042(4) 0.044(4) 0.046(4) -0.007(3) 0.004(3) 0.006(3) C15B 0.077(6) 0.087(6) 0.076(6) 0.040(5) 0.032(5) 0.040(5) C16B 0.042(4) 0.054(4) 0.054(5) -0.012(4) 0.002(3) 0.010(3) P1 0.0368(9) 0.0382(9) 0.0357(10) 0.0052(7) 0.0002(8) 0.0018(7) F1 0.040(2) 0.132(5) 0.071(3) 0.033(3) 0.004(2) 0.024(3) F2 0.035(2) 0.103(4) 0.053(3) 0.024(2) -0.002(2) -0.006(2) F3 0.091(3) 0.054(3) 0.071(3) -0.015(2) 0.018(3) -0.016(2) F4 0.054(3) 0.084(3) 0.050(3) 0.031(2) 0.016(2) 0.018(2) F5 0.151(5) 0.057(3) 0.077(4) -0.023(3) 0.014(4) 0.004(3) F6 0.065(3) 0.064(3) 0.055(3) 0.030(2) 0.002(2) -0.002(2) Cl1 0.0374(8) 0.0276(7) 0.0459(9) 0.0087(7) 0.0066(7) 0.0017(6) N1S 0.110(6) 0.062(5) 0.058(5) -0.011(4) -0.011(4) -0.006(4) C1S 0.070(5) 0.038(4) 0.048(5) 0.003(4) 0.000(4) 0.006(4) C2S 0.089(6) 0.035(4) 0.045(4) 0.001(3) 0.003(4) -0.005(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1A C1A 2.041(6) . ? Ru1A N3A 2.144(4) . ? Ru1A C11A 2.162(5) . ? Ru1A C9A 2.199(6) . ? Ru1A C8A 2.204(6) . ? Ru1A C10A 2.211(6) . ? Ru1A C12A 2.239(5) . ? Ru1A C7A 2.258(6) . ? Ru1A Cl1A 2.4140(15) . ? N1A C1A 1.365(7) . ? N1A C2A 1.380(8) . ? N1A C4A 1.456(8) . ? N2A C1A 1.361(8) . ? N2A C3A 1.384(8) . ? N2A C5A 1.464(7) . ? N3A C6A 1.474(8) . ? C2A C3A 1.344(9) . ? C5A C6A 1.520(9) . ? C7A C12A 1.397(8) . ? C7A C8A 1.435(9) . ? C7A C13A 1.498(9) . ? C8A C9A 1.403(9) . ? C9A C10A 1.440(9) . ? C10A C11A 1.419(8) . ? C10A C14A 1.507(9) . ? C11A C12A 1.425(9) . ? C14A C16A 1.532(10) . ? C14A C15A 1.534(10) . ? Ru1B C1B 2.048(6) . ? Ru1B N3B 2.139(5) . ? Ru1B C9B 2.177(6) . ? Ru1B C10B 2.191(6) . ? Ru1B C11B 2.197(7) . ? Ru1B C12B 2.198(7) . ? Ru1B C8B 2.234(6) . ? Ru1B C7B 2.261(6) . ? Ru1B Cl1B 2.4051(16) . ? N1B C1B 1.367(8) . ? N1B C2B 1.383(9) . ? N1B C4B 1.495(9) . ? N2B C1B 1.347(8) . ? N2B C3B 1.388(8) . ? N2B C5B 1.463(8) . ? N3B C6B 1.464(8) . ? C2B C3B 1.340(11) . ? C5B C6B 1.486(9) . ? C7B C8B 1.385(9) . ? C7B C12B 1.427(9) . ? C7B C13B 1.510(9) . ? C8B C9B 1.411(9) . ? C9B C10B 1.402(9) . ? C10B C11B 1.433(9) . ? C10B C14B 1.528(9) . ? C11B C12B 1.402(9) . ? C14B C15B 1.518(11) . ? C14B C16B 1.525(9) . ? P1 F5 1.557(5) . ? P1 F1 1.587(5) . ? P1 F2 1.592(4) . ? P1 F6 1.595(4) . ? P1 F3 1.599(5) . ? P1 F4 1.602(4) . ? N1S C1S 1.123(9) . ? C1S C2S 1.446(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1A Ru1A N3A 87.0(2) . . ? C1A Ru1A C11A 123.5(2) . . ? N3A Ru1A C11A 89.2(2) . . ? C1A Ru1A C9A 92.2(2) . . ? N3A Ru1A C9A 151.3(2) . . ? C11A Ru1A C9A 67.5(2) . . ? C1A Ru1A C8A 115.4(2) . . ? N3A Ru1A C8A 157.6(2) . . ? C11A Ru1A C8A 79.7(2) . . ? C9A Ru1A C8A 37.2(2) . . ? C1A Ru1A C10A 94.5(2) . . ? N3A Ru1A C10A 113.4(2) . . ? C11A Ru1A C10A 37.8(2) . . ? C9A Ru1A C10A 38.1(2) . . ? C8A Ru1A C10A 68.4(2) . . ? C1A Ru1A C12A 161.2(2) . . ? N3A Ru1A C12A 92.9(2) . . ? C11A Ru1A C12A 37.7(2) . . ? C9A Ru1A C12A 79.0(2) . . ? C8A Ru1A C12A 66.5(2) . . ? C10A Ru1A C12A 68.3(2) . . ? C1A Ru1A C7A 152.3(2) . . ? N3A Ru1A C7A 120.1(2) . . ? C11A Ru1A C7A 67.1(2) . . ? C9A Ru1A C7A 67.3(2) . . ? C8A Ru1A C7A 37.5(2) . . ? C10A Ru1A C7A 80.8(2) . . ? C12A Ru1A C7A 36.2(2) . . ? C1A Ru1A Cl1A 85.28(17) . . ? N3A Ru1A Cl1A 84.16(14) . . ? C11A Ru1A Cl1A 150.16(17) . . ? C9A Ru1A Cl1A 124.36(17) . . ? C8A Ru1A Cl1A 95.79(17) . . ? C10A Ru1A Cl1A 162.47(16) . . ? C12A Ru1A Cl1A 113.45(17) . . ? C7A Ru1A Cl1A 91.27(16) . . ? C1A N1A C2A 110.3(5) . . ? C1A N1A C4A 125.9(5) . . ? C2A N1A C4A 123.7(5) . . ? C1A N2A C3A 111.5(5) . . ? C1A N2A C5A 123.3(5) . . ? C3A N2A C5A 124.9(5) . . ? C6A N3A Ru1A 122.1(3) . . ? N2A C1A N1A 104.2(5) . . ? N2A C1A Ru1A 125.8(4) . . ? N1A C1A Ru1A 129.9(4) . . ? C3A C2A N1A 108.0(5) . . ? C2A C3A N2A 105.9(6) . . ? N2A C5A C6A 109.7(5) . . ? N3A C6A C5A 109.8(5) . . ? C12A C7A C8A 118.6(6) . . ? C12A C7A C13A 121.2(6) . . ? C8A C7A C13A 120.1(6) . . ? C12A C7A Ru1A 71.2(3) . . ? C8A C7A Ru1A 69.2(3) . . ? C13A C7A Ru1A 129.0(4) . . ? C9A C8A C7A 120.8(6) . . ? C9A C8A Ru1A 71.2(3) . . ? C7A C8A Ru1A 73.3(3) . . ? C8A C9A C10A 121.7(6) . . ? C8A C9A Ru1A 71.6(3) . . ? C10A C9A Ru1A 71.4(3) . . ? C11A C10A C9A 115.9(6) . . ? C11A C10A C14A 119.5(6) . . ? C9A C10A C14A 124.7(6) . . ? C11A C10A Ru1A 69.2(3) . . ? C9A C10A Ru1A 70.5(3) . . ? C14A C10A Ru1A 131.0(4) . . ? C10A C11A C12A 122.9(5) . . ? C10A C11A Ru1A 72.9(3) . . ? C12A C11A Ru1A 74.1(3) . . ? C7A C12A C11A 120.1(5) . . ? C7A C12A Ru1A 72.7(3) . . ? C11A C12A Ru1A 68.2(3) . . ? C10A C14A C16A 109.5(6) . . ? C10A C14A C15A 113.9(6) . . ? C16A C14A C15A 111.4(6) . . ? C1B Ru1B N3B 86.5(2) . . ? C1B Ru1B C9B 118.9(2) . . ? N3B Ru1B C9B 91.4(2) . . ? C1B Ru1B C10B 93.2(2) . . ? N3B Ru1B C10B 118.4(2) . . ? C9B Ru1B C10B 37.4(2) . . ? C1B Ru1B C11B 94.8(2) . . ? N3B Ru1B C11B 156.5(2) . . ? C9B Ru1B C11B 67.4(2) . . ? C10B Ru1B C11B 38.1(2) . . ? C1B Ru1B C12B 120.9(3) . . ? N3B Ru1B C12B 152.2(2) . . ? C9B Ru1B C12B 79.5(2) . . ? C10B Ru1B C12B 68.2(2) . . ? C11B Ru1B C12B 37.2(2) . . ? C1B Ru1B C8B 156.1(2) . . ? N3B Ru1B C8B 91.4(2) . . ? C9B Ru1B C8B 37.3(2) . . ? C10B Ru1B C8B 67.0(2) . . ? C11B Ru1B C8B 78.0(2) . . ? C12B Ru1B C8B 65.5(2) . . ? C1B Ru1B C7B 158.0(3) . . ? N3B Ru1B C7B 115.1(2) . . ? C9B Ru1B C7B 67.1(2) . . ? C10B Ru1B C7B 80.3(2) . . ? C11B Ru1B C7B 67.2(2) . . ? C12B Ru1B C7B 37.3(2) . . ? C8B Ru1B C7B 35.9(2) . . ? C1B Ru1B Cl1B 85.70(17) . . ? N3B Ru1B Cl1B 83.73(14) . . ? C9B Ru1B Cl1B 154.64(18) . . ? C10B Ru1B Cl1B 157.76(17) . . ? C11B Ru1B Cl1B 119.76(18) . . ? C12B Ru1B Cl1B 93.31(18) . . ? C8B Ru1B Cl1B 117.72(17) . . ? C7B Ru1B Cl1B 92.45(17) . . ? C1B N1B C2B 110.9(6) . . ? C1B N1B C4B 126.3(6) . . ? C2B N1B C4B 122.7(6) . . ? C1B N2B C3B 112.0(6) . . ? C1B N2B C5B 123.9(5) . . ? C3B N2B C5B 123.7(6) . . ? C6B N3B Ru1B 120.5(4) . . ? N2B C1B N1B 103.7(5) . . ? N2B C1B Ru1B 127.8(4) . . ? N1B C1B Ru1B 128.4(5) . . ? C3B C2B N1B 107.2(6) . . ? C2B C3B N2B 106.1(6) . . ? N2B C5B C6B 110.5(5) . . ? N3B C6B C5B 111.3(5) . . ? C8B C7B C12B 117.1(6) . . ? C8B C7B C13B 122.1(6) . . ? C12B C7B C13B 120.7(6) . . ? C8B C7B Ru1B 71.0(4) . . ? C12B C7B Ru1B 68.9(4) . . ? C13B C7B Ru1B 128.5(5) . . ? C7B C8B C9B 122.6(6) . . ? C7B C8B Ru1B 73.1(4) . . ? C9B C8B Ru1B 69.2(3) . . ? C10B C9B C8B 120.5(6) . . ? C10B C9B Ru1B 71.8(3) . . ? C8B C9B Ru1B 73.5(3) . . ? C9B C10B C11B 117.8(6) . . ? C9B C10B C14B 123.8(6) . . ? C11B C10B C14B 118.4(6) . . ? C9B C10B Ru1B 70.7(3) . . ? C11B C10B Ru1B 71.2(4) . . ? C14B C10B Ru1B 130.0(4) . . ? C12B C11B C10B 120.5(6) . . ? C12B C11B Ru1B 71.4(4) . . ? C10B C11B Ru1B 70.7(4) . . ? C11B C12B C7B 121.4(6) . . ? C11B C12B Ru1B 71.4(4) . . ? C7B C12B Ru1B 73.8(4) . . ? C15B C14B C16B 111.3(6) . . ? C15B C14B C10B 114.1(6) . . ? C16B C14B C10B 108.6(6) . . ? F5 P1 F1 91.2(3) . . ? F5 P1 F2 91.2(3) . . ? F1 P1 F2 177.5(3) . . ? F5 P1 F6 92.6(3) . . ? F1 P1 F6 90.2(2) . . ? F2 P1 F6 90.1(2) . . ? F5 P1 F3 179.0(3) . . ? F1 P1 F3 89.0(3) . . ? F2 P1 F3 88.6(3) . . ? F6 P1 F3 88.4(3) . . ? F5 P1 F4 89.3(3) . . ? F1 P1 F4 90.0(2) . . ? F2 P1 F4 89.6(2) . . ? F6 P1 F4 178.1(3) . . ? F3 P1 F4 89.7(3) . . ? N1S C1S C2S 179.2(10) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3A H3AB Cl1 0.92 2.39 3.230(5) 151.8 1_556 N3A H3AC Cl1 0.92 2.60 3.337(5) 137.8 3_666 N3B H3BB Cl1 0.92 2.37 3.245(5) 159.9 . N3B H3BC Cl1A 0.92 2.64 3.292(5) 128.8 3_666 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.625 _refine_diff_density_min -1.437 _refine_diff_density_rms 0.133