# 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_ms448h _database_code_depnum_ccdc_archive 'CCDC 915463' #TrackingRef '915464.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H39 Cl3 N6 O3 P2 Ru S' _chemical_formula_weight 700.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 12.2596(3) _cell_length_b 18.5862(5) _cell_length_c 12.4045(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2826.48(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5325 _cell_measurement_theta_min 4.671 _cell_measurement_theta_max 49.407 _exptl_crystal_description Prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.132 _exptl_crystal_size_mid 0.110 _exptl_crystal_size_min 0.092 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.643 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 1.059 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13813 _diffrn_reflns_av_R_equivalents 0.0464 _diffrn_reflns_av_sigmaI/netI 0.0309 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 24.70 _reflns_number_total 2478 _reflns_number_gt 2188 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker APEX' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0550P)^2^+2.0016P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2478 _refine_ls_number_parameters 241 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0384 _refine_ls_R_factor_gt 0.0338 _refine_ls_wR_factor_ref 0.0931 _refine_ls_wR_factor_gt 0.0905 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.03341(3) 0.7500 0.00626(3) 0.01677(15) Uani 1 2 d S . . Cl1 Cl 0.71803(7) 0.53168(5) 0.99404(6) 0.0281(2) Uani 1 1 d . . . Cl2 Cl 0.57307(13) 0.7500 0.01797(10) 0.0420(4) Uani 1 2 d S . . P1 P 0.02339(6) 0.65914(4) 0.12935(6) 0.0157(2) Uani 1 1 d . . . N1 N 0.0163(2) 0.51177(13) 0.1614(2) 0.0224(6) Uani 1 1 d . . . N2 N -0.1087(2) 0.58400(14) 0.2709(2) 0.0225(6) Uani 1 1 d . . . N3 N 0.0868(2) 0.58311(14) 0.3098(2) 0.0218(6) Uani 1 1 d . . . S1D S 0.21773(9) 0.7500 0.00851(8) 0.0209(3) Uani 1 2 d S . . O1D O 0.2726(2) 0.7500 0.1145(2) 0.0265(7) Uani 1 2 d S . . C1D C 0.2755(3) 0.6770(2) -0.0667(3) 0.0327(8) Uani 1 1 d . . . C1 C 0.0339(3) 0.56654(16) 0.0772(3) 0.0208(7) Uani 1 1 d . . . C2 C -0.1065(3) 0.64823(17) 0.2019(3) 0.0228(7) Uani 1 1 d . . . C3 C 0.1167(3) 0.64817(17) 0.2451(3) 0.0216(7) Uani 1 1 d . . . C4 C -0.0929(3) 0.51766(17) 0.2095(3) 0.0234(7) Uani 1 1 d . . . C5 C -0.0298(3) 0.58830(19) 0.3554(3) 0.0250(7) Uani 1 1 d . . . C6 C 0.0976(3) 0.51455(18) 0.2443(3) 0.0230(7) Uani 1 1 d . . . C11 C 0.0205(4) 0.7500 -0.1731(4) 0.0363(12) Uani 1 2 d S . . C12 C -0.0317(4) 0.6894(2) -0.1351(3) 0.0419(11) Uani 1 1 d . . . C13 C -0.1200(3) 0.7124(3) -0.0713(3) 0.0501(12) Uani 1 1 d . . . O1W O 0.6470(4) 0.6464(3) 0.8246(4) 0.0499(17) Uiso 0.596(7) 1 d P A 1 O2W O 0.5569(6) 0.6269(4) 0.8621(6) 0.055(3) Uiso 0.404(7) 1 d P A 2 H1A H 0.104(3) 0.5610(16) 0.043(3) 0.015(8) Uiso 1 1 d . . . H2A H -0.119(3) 0.689(2) 0.249(3) 0.030(10) Uiso 1 1 d . . . H4A H -0.107(2) 0.4781(18) 0.256(2) 0.014(8) Uiso 1 1 d . . . H6B H 0.086(2) 0.4810(18) 0.295(3) 0.019(8) Uiso 1 1 d . . . H5B H -0.037(2) 0.5494(17) 0.410(3) 0.017(8) Uiso 1 1 d . . . H1N H 0.124(3) 0.5756(19) 0.362(3) 0.024(10) Uiso 1 1 d . . . H5A H -0.036(2) 0.6319(18) 0.391(2) 0.017(8) Uiso 1 1 d . . . H4B H -0.141(3) 0.5173(17) 0.154(3) 0.021(9) Uiso 1 1 d . . . H3A H 0.191(3) 0.6376(19) 0.220(3) 0.031(9) Uiso 1 1 d . . . H2B H -0.158(3) 0.6439(18) 0.150(3) 0.028(10) Uiso 1 1 d . . . H6A H 0.167(3) 0.5150(16) 0.215(2) 0.013(8) Uiso 1 1 d . . . H1B H -0.020(3) 0.562(2) 0.023(3) 0.028(10) Uiso 1 1 d . . . H3B H 0.112(2) 0.6876(18) 0.289(3) 0.022(9) Uiso 1 1 d . . . H1E H 0.244(3) 0.6768(17) -0.136(3) 0.021(9) Uiso 1 1 d . . . H1F H 0.251(4) 0.636(3) -0.030(4) 0.054(13) Uiso 1 1 d . . . H1G H 0.353(4) 0.685(2) -0.069(3) 0.040(11) Uiso 1 1 d . . . H12 H -0.014(4) 0.646(3) -0.149(4) 0.057(14) Uiso 1 1 d . . . H11 H 0.084(5) 0.7500 -0.222(5) 0.055(17) Uiso 1 2 d S . . H13 H -0.163(5) 0.685(3) -0.034(4) 0.082(18) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0195(2) 0.0151(2) 0.0157(2) 0.000 0.00020(13) 0.000 Cl1 0.0275(5) 0.0347(5) 0.0222(4) -0.0046(3) -0.0002(3) 0.0073(3) Cl2 0.0606(9) 0.0346(7) 0.0308(7) 0.000 0.0096(6) 0.000 P1 0.0163(4) 0.0139(4) 0.0171(4) 0.0001(3) 0.0002(3) -0.0004(3) N1 0.0282(14) 0.0156(12) 0.0233(15) 0.0014(11) -0.0027(11) -0.0002(11) N2 0.0200(14) 0.0204(13) 0.0270(15) 0.0061(12) 0.0026(11) -0.0012(11) N3 0.0229(15) 0.0232(14) 0.0193(15) 0.0044(12) -0.0058(12) -0.0026(11) S1D 0.0190(6) 0.0220(6) 0.0216(6) 0.000 0.0026(4) 0.000 O1D 0.0196(16) 0.0364(18) 0.0234(17) 0.000 -0.0007(13) 0.000 C1D 0.029(2) 0.032(2) 0.037(2) -0.0063(18) 0.0053(17) 0.0055(17) C1 0.0255(18) 0.0175(16) 0.0195(17) -0.0008(13) 0.0007(15) 0.0006(13) C2 0.0203(17) 0.0203(16) 0.0278(19) 0.0010(15) 0.0032(15) 0.0014(13) C3 0.0245(18) 0.0195(17) 0.0207(17) 0.0011(14) -0.0011(13) -0.0053(13) C4 0.0246(18) 0.0208(16) 0.0247(18) 0.0041(15) -0.0040(14) -0.0062(13) C5 0.031(2) 0.0225(17) 0.0214(17) 0.0012(15) 0.0053(14) -0.0036(14) C6 0.0253(18) 0.0197(16) 0.0240(18) 0.0040(14) 0.0002(14) 0.0029(14) C11 0.034(3) 0.054(4) 0.020(3) 0.000 -0.004(2) 0.000 C12 0.064(3) 0.029(2) 0.032(2) -0.0074(18) -0.024(2) 0.0043(19) C13 0.037(2) 0.085(3) 0.029(2) 0.019(2) -0.0168(17) -0.030(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C13 2.225(4) . ? Ru1 C13 2.225(4) 7_575 ? Ru1 C11 2.231(5) . ? Ru1 C12 2.232(4) . ? Ru1 C12 2.232(4) 7_575 ? Ru1 S1D 2.2599(12) . ? Ru1 P1 2.2800(8) 7_575 ? Ru1 P1 2.2800(8) . ? P1 C2 1.840(3) . ? P1 C1 1.843(3) . ? P1 C3 1.847(3) . ? N1 C6 1.432(4) . ? N1 C4 1.471(4) . ? N1 C1 1.475(4) . ? N2 C5 1.428(4) . ? N2 C4 1.462(4) . ? N2 C2 1.470(4) . ? N3 C3 1.497(4) . ? N3 C6 1.518(4) . ? N3 C5 1.540(4) . ? N3 H1N 0.80(4) . ? S1D O1D 1.478(3) . ? S1D C1D 1.791(4) . ? S1D C1D 1.791(4) 7_575 ? C1D H1E 0.94(3) . ? C1D H1F 0.94(5) . ? C1D H1G 0.96(4) . ? C1 H1A 0.96(3) . ? C1 H1B 0.95(4) . ? C2 H2A 0.97(4) . ? C2 H2B 0.90(4) . ? C3 H3A 0.99(4) . ? C3 H3B 0.91(3) . ? C4 H4A 0.95(3) . ? C4 H4B 0.90(3) . ? C5 H5B 0.99(3) . ? C5 H5A 0.93(3) . ? C6 H6B 0.90(3) . ? C6 H6A 0.93(3) . ? C11 C12 1.379(5) 7_575 ? C11 C12 1.379(5) . ? C11 H11 0.99(6) . ? C12 C13 1.407(6) . ? C12 H12 0.85(5) . ? C13 C13 1.399(10) 7_575 ? C13 H13 0.87(6) . ? 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 C13 Ru1 C13 36.7(2) . 7_575 ? C13 Ru1 C11 60.56(17) . . ? C13 Ru1 C11 60.56(17) 7_575 . ? C13 Ru1 C12 36.79(16) . . ? C13 Ru1 C12 61.10(15) 7_575 . ? C11 Ru1 C12 36.00(13) . . ? C13 Ru1 C12 61.10(15) . 7_575 ? C13 Ru1 C12 36.79(16) 7_575 7_575 ? C11 Ru1 C12 36.00(13) . 7_575 ? C12 Ru1 C12 60.6(2) . 7_575 ? C13 Ru1 S1D 148.25(13) . . ? C13 Ru1 S1D 148.25(13) 7_575 . ? C11 Ru1 S1D 94.79(14) . . ? C12 Ru1 S1D 111.56(12) . . ? C12 Ru1 S1D 111.56(12) 7_575 . ? C13 Ru1 P1 118.49(13) . 7_575 ? C13 Ru1 P1 90.64(11) 7_575 7_575 ? C11 Ru1 P1 131.62(3) . 7_575 ? C12 Ru1 P1 151.73(11) . 7_575 ? C12 Ru1 P1 97.64(11) 7_575 7_575 ? S1D Ru1 P1 92.61(3) . 7_575 ? C13 Ru1 P1 90.64(11) . . ? C13 Ru1 P1 118.49(13) 7_575 . ? C11 Ru1 P1 131.62(3) . . ? C12 Ru1 P1 97.64(11) . . ? C12 Ru1 P1 151.73(11) 7_575 . ? S1D Ru1 P1 92.61(3) . . ? P1 Ru1 P1 95.58(4) 7_575 . ? C2 P1 C1 97.41(15) . . ? C2 P1 C3 98.28(15) . . ? C1 P1 C3 97.28(15) . . ? C2 P1 Ru1 117.10(11) . . ? C1 P1 Ru1 116.92(10) . . ? C3 P1 Ru1 124.67(10) . . ? C6 N1 C4 109.9(3) . . ? C6 N1 C1 112.5(3) . . ? C4 N1 C1 111.7(2) . . ? C5 N2 C4 109.9(3) . . ? C5 N2 C2 111.7(3) . . ? C4 N2 C2 112.3(3) . . ? C3 N3 C6 111.7(2) . . ? C3 N3 C5 112.0(2) . . ? C6 N3 C5 109.3(2) . . ? C3 N3 H1N 116(3) . . ? C6 N3 H1N 104(3) . . ? C5 N3 H1N 104(3) . . ? O1D S1D C1D 106.46(17) . . ? O1D S1D C1D 106.46(17) . 7_575 ? C1D S1D C1D 98.4(3) . 7_575 ? O1D S1D Ru1 117.81(13) . . ? C1D S1D Ru1 112.87(14) . . ? C1D S1D Ru1 112.87(14) 7_575 . ? S1D C1D H1E 108.4(19) . . ? S1D C1D H1F 104(3) . . ? H1E C1D H1F 108(3) . . ? S1D C1D H1G 107(2) . . ? H1E C1D H1G 112(3) . . ? H1F C1D H1G 117(4) . . ? N1 C1 P1 112.7(2) . . ? N1 C1 H1A 111.4(19) . . ? P1 C1 H1A 108.5(19) . . ? N1 C1 H1B 110(2) . . ? P1 C1 H1B 106(2) . . ? H1A C1 H1B 108(3) . . ? N2 C2 P1 113.0(2) . . ? N2 C2 H2A 106(2) . . ? P1 C2 H2A 110(2) . . ? N2 C2 H2B 109(2) . . ? P1 C2 H2B 105(2) . . ? H2A C2 H2B 113(3) . . ? N3 C3 P1 110.7(2) . . ? N3 C3 H3A 104(2) . . ? P1 C3 H3A 110(2) . . ? N3 C3 H3B 108(2) . . ? P1 C3 H3B 110(2) . . ? H3A C3 H3B 114(3) . . ? N2 C4 N1 113.2(2) . . ? N2 C4 H4A 108.1(18) . . ? N1 C4 H4A 110.9(18) . . ? N2 C4 H4B 108(2) . . ? N1 C4 H4B 107(2) . . ? H4A C4 H4B 110(3) . . ? N2 C5 N3 110.8(3) . . ? N2 C5 H5B 113.4(17) . . ? N3 C5 H5B 106.8(16) . . ? N2 C5 H5A 110.3(19) . . ? N3 C5 H5A 107.5(19) . . ? H5B C5 H5A 108(2) . . ? N1 C6 N3 110.7(3) . . ? N1 C6 H6B 111(2) . . ? N3 C6 H6B 101(2) . . ? N1 C6 H6A 111.3(18) . . ? N3 C6 H6A 106.3(18) . . ? H6B C6 H6A 115(3) . . ? C12 C11 C12 109.6(5) 7_575 . ? C12 C11 Ru1 72.1(3) 7_575 . ? C12 C11 Ru1 72.1(3) . . ? C12 C11 H11 125.2(3) 7_575 . ? C12 C11 H11 125.2(3) . . ? Ru1 C11 H11 124(3) . . ? C11 C12 C13 107.5(4) . . ? C11 C12 Ru1 71.9(3) . . ? C13 C12 Ru1 71.3(2) . . ? C11 C12 H12 126(3) . . ? C13 C12 H12 127(3) . . ? Ru1 C12 H12 123(3) . . ? C13 C13 C12 107.7(3) 7_575 . ? C13 C13 Ru1 71.67(12) 7_575 . ? C12 C13 Ru1 71.9(2) . . ? C13 C13 H13 126(4) 7_575 . ? C12 C13 H13 126(4) . . ? Ru1 C13 H13 118(4) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 24.70 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.514 _refine_diff_density_min -0.762 _refine_diff_density_rms 0.086 data_c:\sir97\manuel\ms515w3\ms515s _database_code_depnum_ccdc_archive 'CCDC 915464' #TrackingRef '915463.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H35 Cl3 N6 O2 P2 Ru' _chemical_formula_weight 624.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2375(15) _cell_length_b 9.2500(15) _cell_length_c 15.217(3) _cell_angle_alpha 81.471(4) _cell_angle_beta 80.635(3) _cell_angle_gamma 87.202(3) _cell_volume 1268.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 1551 _cell_measurement_theta_min 4.878 _cell_measurement_theta_max 46.628 _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.221 _exptl_crystal_size_mid 0.145 _exptl_crystal_size_min 0.030 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.626 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 632 _exptl_absorpt_coefficient_mu 1.087 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.828 _exptl_absorpt_correction_T_max 0.968 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6927 _diffrn_reflns_av_R_equivalents 0.0385 _diffrn_reflns_av_sigmaI/netI 0.0851 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 25.05 _reflns_number_total 4411 _reflns_number_gt 3672 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker APEX' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1022P)^2^+1.9867P] 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 4411 _refine_ls_number_parameters 308 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0777 _refine_ls_R_factor_gt 0.0626 _refine_ls_wR_factor_ref 0.1841 _refine_ls_wR_factor_gt 0.1669 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.097 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 1.01160(6) 0.10319(6) 0.77022(3) 0.0135(2) Uani 1 1 d . . . P1 P 1.0577(2) 0.33829(19) 0.71321(11) 0.0149(4) Uani 1 1 d . . . P2 P 0.8054(2) 0.09108(19) 0.71083(12) 0.0155(4) Uani 1 1 d . . . Cl1 Cl 1.14980(19) 0.03060(19) 0.63042(11) 0.0198(4) Uani 1 1 d . . . Cl2 Cl 0.6105(2) 0.5816(2) 0.62963(16) 0.0373(5) Uani 1 1 d . . . Cl3 Cl 0.4235(8) 0.6497(7) 0.8431(5) 0.041(2) Uani 0.344(6) 1 d P A 1 Cl4 Cl 0.5100(11) 0.6041(11) 0.7725(7) 0.026(2) Uani 0.185(3) 1 d P A 1 Cl5 Cl 0.1164(12) 0.5003(10) 0.9847(6) 0.044(2) Uani 0.329(6) 1 d P . 2 Cl6 Cl 0.205(4) 0.455(3) 0.9782(17) 0.072(8) Uani 0.141(3) 1 d P A 2 N11 N 1.1256(6) 0.5615(6) 0.5714(4) 0.0166(13) Uani 1 1 d . . . N12 N 1.2648(7) 0.5579(6) 0.6982(4) 0.0226(14) Uani 1 1 d . . . H12 H 1.3543 0.5831 0.7115 0.027 Uiso 1 1 calc R . . N13 N 1.0017(6) 0.6353(6) 0.7141(4) 0.0170(13) Uani 1 1 d . . . N21 N 0.6503(7) 0.0988(7) 0.5673(4) 0.0197(13) Uani 1 1 d . . . N22 N 0.5072(6) 0.1431(7) 0.7115(4) 0.0210(14) Uani 1 1 d . . . N23 N 0.5956(7) -0.1071(7) 0.6906(4) 0.0234(14) Uani 1 1 d . . . H23 H 0.5660 -0.2036 0.7012 0.028 Uiso 1 1 calc R . . C11 C 1.2326(8) 0.3998(7) 0.7368(5) 0.0185(15) Uani 1 1 d . . . H11A H 1.2300 0.3878 0.8028 0.022 Uiso 1 1 calc R . . H11B H 1.3135 0.3365 0.7117 0.022 Uiso 1 1 calc R . . C12 C 0.9420(8) 0.4907(8) 0.7539(5) 0.0201(16) Uani 1 1 d . . . H12A H 0.8422 0.4845 0.7391 0.024 Uiso 1 1 calc R . . H12B H 0.9336 0.4808 0.8202 0.024 Uiso 1 1 calc R . . C13 C 1.0833(8) 0.4071(7) 0.5918(4) 0.0187(15) Uani 1 1 d . . . H13A H 1.1603 0.3466 0.5601 0.022 Uiso 1 1 calc R . . H13B H 0.9909 0.3964 0.5687 0.022 Uiso 1 1 calc R . . C14 C 1.2672(8) 0.5825(8) 0.5949(5) 0.0229(16) Uani 1 1 d . . . H14A H 1.2989 0.6831 0.5703 0.027 Uiso 1 1 calc R . . H14B H 1.3397 0.5136 0.5670 0.027 Uiso 1 1 calc R . . C15 C 1.1389(8) 0.6576(8) 0.7397(5) 0.0241(17) Uani 1 1 d . . . H15A H 1.1294 0.6382 0.8061 0.029 Uiso 1 1 calc R . . H15B H 1.1653 0.7612 0.7205 0.029 Uiso 1 1 calc R . . C16 C 1.0134(8) 0.6582(8) 0.6167(5) 0.0202(16) Uani 1 1 d . . . H16A H 1.0382 0.7614 0.5939 0.024 Uiso 1 1 calc R . . H16B H 0.9168 0.6413 0.6004 0.024 Uiso 1 1 calc R . . C21 C 0.7375(8) -0.0965(7) 0.7292(5) 0.0182(15) Uani 1 1 d . . . H21A H 0.8139 -0.1612 0.7008 0.022 Uiso 1 1 calc R . . H21B H 0.7195 -0.1319 0.7946 0.022 Uiso 1 1 calc R . . C22 C 0.7938(8) 0.1330(8) 0.5886(5) 0.0198(16) Uani 1 1 d . . . H22A H 0.8123 0.2381 0.5683 0.024 Uiso 1 1 calc R . . H22B H 0.8716 0.0762 0.5548 0.024 Uiso 1 1 calc R . . C23 C 0.6333(8) 0.1836(8) 0.7519(5) 0.0223(16) Uani 1 1 d . . . H23A H 0.6111 0.1584 0.8182 0.027 Uiso 1 1 calc R . . H23B H 0.6457 0.2907 0.7379 0.027 Uiso 1 1 calc R . . C24 C 0.4741(8) -0.0100(8) 0.7349(5) 0.0257(17) Uani 1 1 d . . . H24A H 0.3801 -0.0276 0.7153 0.031 Uiso 1 1 calc R . . H24B H 0.4621 -0.0367 0.8010 0.031 Uiso 1 1 calc R . . C25 C 0.6198(9) -0.0529(8) 0.5879(5) 0.0248(17) Uani 1 1 d . . . H25A H 0.7027 -0.1094 0.5583 0.030 Uiso 1 1 calc R . . H25B H 0.5309 -0.0716 0.5632 0.030 Uiso 1 1 calc R . . C26 C 0.5291(8) 0.1845(8) 0.6142(5) 0.0234(17) Uani 1 1 d . . . H26A H 0.5512 0.2898 0.5998 0.028 Uiso 1 1 calc R . . H26B H 0.4370 0.1696 0.5917 0.028 Uiso 1 1 calc R . . C31 C 1.1258(8) -0.0586(8) 0.8656(5) 0.0232(16) Uani 1 1 d . . . H31 H 1.2032 -0.1253 0.8486 0.028 Uiso 1 1 calc R . . C32 C 1.1452(9) 0.0856(9) 0.8817(5) 0.0243(17) Uani 1 1 d . . . H32 H 1.2363 0.1318 0.8768 0.029 Uiso 1 1 calc R . . C33 C 1.0029(9) 0.1489(9) 0.9066(5) 0.0276(18) Uani 1 1 d . . . H33 H 0.9819 0.2450 0.9210 0.033 Uiso 1 1 calc R . . C34 C 0.8972(9) 0.0397(9) 0.9056(5) 0.0286(19) Uani 1 1 d . . . H34 H 0.7937 0.0506 0.9203 0.034 Uiso 1 1 calc R . . C35 C 0.9758(9) -0.0886(9) 0.8785(5) 0.0270(18) Uani 1 1 d . . . H35 H 0.9340 -0.1768 0.8708 0.032 Uiso 1 1 calc R . . O1W O 0.5051(12) 0.9201(12) 0.9907(7) 0.054(4) Uiso 0.671(18) 1 d P . 1 O2W O 0.591(3) 0.785(3) 0.9666(16) 0.062(8) Uiso 0.329(18) 1 d P . 2 O3W O 0.6310(18) 0.4098(18) 0.9035(10) 0.098(6) Uiso 0.67(2) 1 d P B 1 O4W O 0.666(4) 0.699(4) 0.912(3) 0.129(16) Uiso 0.33(2) 1 d P . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0148(3) 0.0109(3) 0.0153(3) -0.0009(2) -0.0043(2) -0.0005(2) P1 0.0181(10) 0.0108(9) 0.0166(9) -0.0023(7) -0.0054(7) 0.0012(7) P2 0.0150(9) 0.0123(9) 0.0193(9) -0.0016(7) -0.0037(7) 0.0001(7) Cl1 0.0210(9) 0.0180(9) 0.0201(9) -0.0037(7) -0.0019(7) -0.0001(7) Cl2 0.0269(11) 0.0227(11) 0.0653(15) -0.0090(10) -0.0130(10) -0.0038(8) Cl3 0.044(4) 0.033(4) 0.048(4) -0.005(3) -0.014(3) 0.001(3) Cl4 0.031(6) 0.020(5) 0.029(5) 0.000(4) -0.015(4) 0.011(4) Cl5 0.067(6) 0.038(5) 0.034(4) -0.009(3) -0.022(4) -0.003(4) Cl6 0.09(2) 0.075(19) 0.053(13) 0.016(12) -0.036(15) -0.041(16) N11 0.018(3) 0.012(3) 0.018(3) 0.000(2) -0.002(2) 0.001(2) N12 0.021(3) 0.010(3) 0.032(3) 0.010(3) 0.000(3) 0.001(2) N13 0.018(3) 0.008(3) 0.024(3) -0.003(2) -0.004(3) 0.008(2) N21 0.022(3) 0.019(3) 0.018(3) -0.003(2) -0.004(3) 0.003(3) N22 0.012(3) 0.023(3) 0.028(3) -0.007(3) -0.001(3) 0.005(3) N23 0.025(4) 0.020(3) 0.030(3) -0.009(3) -0.016(3) 0.010(3) C11 0.020(4) 0.011(4) 0.025(4) 0.000(3) -0.009(3) 0.003(3) C12 0.021(4) 0.014(4) 0.024(4) -0.003(3) -0.002(3) 0.000(3) C13 0.029(4) 0.013(4) 0.015(3) -0.003(3) -0.004(3) 0.003(3) C14 0.016(4) 0.022(4) 0.027(4) -0.001(3) 0.004(3) 0.005(3) C15 0.031(4) 0.011(4) 0.034(4) -0.007(3) -0.011(4) -0.004(3) C16 0.022(4) 0.011(4) 0.028(4) -0.002(3) -0.004(3) 0.004(3) C21 0.018(4) 0.008(3) 0.030(4) -0.001(3) -0.012(3) 0.004(3) C22 0.014(4) 0.025(4) 0.018(3) 0.004(3) -0.003(3) -0.002(3) C23 0.021(4) 0.019(4) 0.029(4) -0.010(3) -0.008(3) 0.008(3) C24 0.019(4) 0.023(4) 0.034(4) 0.000(3) -0.005(3) 0.002(3) C25 0.032(4) 0.017(4) 0.026(4) -0.004(3) -0.009(3) 0.009(3) C26 0.022(4) 0.014(4) 0.035(4) -0.003(3) -0.009(3) 0.008(3) C31 0.023(4) 0.023(4) 0.023(4) 0.001(3) -0.008(3) 0.003(3) C32 0.031(5) 0.025(4) 0.022(4) 0.000(3) -0.018(3) -0.006(3) C33 0.047(5) 0.025(4) 0.013(3) -0.004(3) -0.011(3) 0.007(4) C34 0.023(4) 0.041(5) 0.017(4) 0.004(3) 0.002(3) 0.002(4) C35 0.031(5) 0.024(4) 0.024(4) 0.007(3) -0.005(3) -0.011(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C33 2.166(7) . ? Ru1 C34 2.168(7) . ? Ru1 C35 2.232(7) . ? Ru1 C32 2.237(7) . ? Ru1 P2 2.2515(19) . ? Ru1 P1 2.2525(18) . ? Ru1 C31 2.272(7) . ? Ru1 Cl1 2.4623(18) . ? P1 C13 1.843(7) . ? P1 C11 1.845(7) . ? P1 C12 1.847(7) . ? P2 C23 1.831(7) . ? P2 C21 1.841(7) . ? P2 C22 1.863(7) . ? Cl2 Cl4 2.255(11) . ? Cl3 Cl4 1.340(12) . ? Cl5 Cl6 0.90(3) . ? Cl5 Cl5 2.12(2) 2_567 ? N11 C14 1.440(9) . ? N11 C13 1.474(9) . ? N11 C16 1.486(9) . ? N12 C11 1.517(8) . ? N12 C14 1.551(9) . ? N12 C15 1.560(10) . ? N12 H12 0.9300 . ? N13 C15 1.418(9) . ? N13 C16 1.453(9) . ? N13 C12 1.478(9) . ? N21 C25 1.423(9) . ? N21 C22 1.474(9) . ? N21 C26 1.488(9) . ? N22 C24 1.443(10) . ? N22 C26 1.457(10) . ? N22 C23 1.490(9) . ? N23 C21 1.534(9) . ? N23 C24 1.535(10) . ? N23 C25 1.553(9) . ? N23 H23 0.9300 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C31 C35 1.404(11) . ? C31 C32 1.416(11) . ? C31 H31 0.9500 . ? C32 C33 1.429(12) . ? C32 H32 0.9500 . ? C33 C34 1.442(11) . ? C33 H33 0.9500 . ? C34 C35 1.438(12) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? O1W O1W 1.54(2) 2_677 ? O2W O4W 1.33(4) . ? 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 C33 Ru1 C34 38.9(3) . . ? C33 Ru1 C35 64.0(3) . . ? C34 Ru1 C35 38.1(3) . . ? C33 Ru1 C32 37.8(3) . . ? C34 Ru1 C32 63.2(3) . . ? C35 Ru1 C32 62.3(3) . . ? C33 Ru1 P2 121.3(2) . . ? C34 Ru1 P2 91.9(2) . . ? C35 Ru1 P2 98.5(2) . . ? C32 Ru1 P2 155.1(2) . . ? C33 Ru1 P1 91.7(2) . . ? C34 Ru1 P1 122.3(2) . . ? C35 Ru1 P1 155.6(2) . . ? C32 Ru1 P1 97.6(2) . . ? P2 Ru1 P1 96.18(7) . . ? C33 Ru1 C31 62.3(3) . . ? C34 Ru1 C31 61.9(3) . . ? C35 Ru1 C31 36.3(3) . . ? C32 Ru1 C31 36.6(3) . . ? P2 Ru1 C31 132.4(2) . . ? P1 Ru1 C31 131.2(2) . . ? C33 Ru1 Cl1 150.7(2) . . ? C34 Ru1 Cl1 148.8(2) . . ? C35 Ru1 Cl1 111.2(2) . . ? C32 Ru1 Cl1 113.2(2) . . ? P2 Ru1 Cl1 87.74(6) . . ? P1 Ru1 Cl1 88.72(6) . . ? C31 Ru1 Cl1 96.2(2) . . ? C13 P1 C11 97.7(3) . . ? C13 P1 C12 98.5(3) . . ? C11 P1 C12 96.6(3) . . ? C13 P1 Ru1 123.4(2) . . ? C11 P1 Ru1 113.2(2) . . ? C12 P1 Ru1 121.9(2) . . ? C23 P2 C21 98.0(3) . . ? C23 P2 C22 97.2(3) . . ? C21 P2 C22 97.5(3) . . ? C23 P2 Ru1 122.4(2) . . ? C21 P2 Ru1 111.7(2) . . ? C22 P2 Ru1 124.6(2) . . ? Cl3 Cl4 Cl2 161.3(7) . . ? Cl6 Cl5 Cl5 152(2) . 2_567 ? C14 N11 C13 112.0(6) . . ? C14 N11 C16 110.1(6) . . ? C13 N11 C16 111.6(5) . . ? C11 N12 C14 110.6(6) . . ? C11 N12 C15 108.7(5) . . ? C14 N12 C15 107.2(5) . . ? C11 N12 H12 110.1 . . ? C14 N12 H12 110.1 . . ? C15 N12 H12 110.1 . . ? C15 N13 C16 110.3(6) . . ? C15 N13 C12 112.3(6) . . ? C16 N13 C12 111.8(5) . . ? C25 N21 C22 112.7(6) . . ? C25 N21 C26 109.5(6) . . ? C22 N21 C26 111.4(6) . . ? C24 N22 C26 110.4(6) . . ? C24 N22 C23 112.7(6) . . ? C26 N22 C23 112.0(6) . . ? C21 N23 C24 110.2(5) . . ? C21 N23 C25 110.5(6) . . ? C24 N23 C25 107.6(6) . . ? C21 N23 H23 109.5 . . ? C24 N23 H23 109.5 . . ? C25 N23 H23 109.5 . . ? N12 C11 P1 113.5(5) . . ? N12 C11 H11A 108.9 . . ? P1 C11 H11A 108.9 . . ? N12 C11 H11B 108.9 . . ? P1 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? N13 C12 P1 112.5(5) . . ? N13 C12 H12A 109.1 . . ? P1 C12 H12A 109.1 . . ? N13 C12 H12B 109.1 . . ? P1 C12 H12B 109.1 . . ? H12A C12 H12B 107.8 . . ? N11 C13 P1 112.8(5) . . ? N11 C13 H13A 109.0 . . ? P1 C13 H13A 109.0 . . ? N11 C13 H13B 109.0 . . ? P1 C13 H13B 109.0 . . ? H13A C13 H13B 107.8 . . ? N11 C14 N12 112.1(6) . . ? N11 C14 H14A 109.2 . . ? N12 C14 H14A 109.2 . . ? N11 C14 H14B 109.2 . . ? N12 C14 H14B 109.2 . . ? H14A C14 H14B 107.9 . . ? N13 C15 N12 113.0(6) . . ? N13 C15 H15A 109.0 . . ? N12 C15 H15A 109.0 . . ? N13 C15 H15B 109.0 . . ? N12 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? N13 C16 N11 113.5(6) . . ? N13 C16 H16A 108.9 . . ? N11 C16 H16A 108.9 . . ? N13 C16 H16B 108.9 . . ? N11 C16 H16B 108.9 . . ? H16A C16 H16B 107.7 . . ? N23 C21 P2 112.7(5) . . ? N23 C21 H21A 109.1 . . ? P2 C21 H21A 109.1 . . ? N23 C21 H21B 109.1 . . ? P2 C21 H21B 109.1 . . ? H21A C21 H21B 107.8 . . ? N21 C22 P2 113.1(5) . . ? N21 C22 H22A 109.0 . . ? P2 C22 H22A 109.0 . . ? N21 C22 H22B 109.0 . . ? P2 C22 H22B 109.0 . . ? H22A C22 H22B 107.8 . . ? N22 C23 P2 112.7(5) . . ? N22 C23 H23A 109.0 . . ? P2 C23 H23A 109.0 . . ? N22 C23 H23B 109.0 . . ? P2 C23 H23B 109.0 . . ? H23A C23 H23B 107.8 . . ? N22 C24 N23 111.7(6) . . ? N22 C24 H24A 109.3 . . ? N23 C24 H24A 109.3 . . ? N22 C24 H24B 109.3 . . ? N23 C24 H24B 109.3 . . ? H24A C24 H24B 108.0 . . ? N21 C25 N23 112.6(6) . . ? N21 C25 H25A 109.1 . . ? N23 C25 H25A 109.1 . . ? N21 C25 H25B 109.1 . . ? N23 C25 H25B 109.1 . . ? H25A C25 H25B 107.8 . . ? N22 C26 N21 112.6(6) . . ? N22 C26 H26A 109.1 . . ? N21 C26 H26A 109.1 . . ? N22 C26 H26B 109.1 . . ? N21 C26 H26B 109.1 . . ? H26A C26 H26B 107.8 . . ? C35 C31 C32 110.1(7) . . ? C35 C31 Ru1 70.3(4) . . ? C32 C31 Ru1 70.4(4) . . ? C35 C31 H31 125.0 . . ? C32 C31 H31 125.0 . . ? Ru1 C31 H31 125.9 . . ? C31 C32 C33 107.7(7) . . ? C31 C32 Ru1 73.0(4) . . ? C33 C32 Ru1 68.4(4) . . ? C31 C32 H32 126.2 . . ? C33 C32 H32 126.2 . . ? Ru1 C32 H32 124.0 . . ? C32 C33 C34 107.1(7) . . ? C32 C33 Ru1 73.8(4) . . ? C34 C33 Ru1 70.6(4) . . ? C32 C33 H33 126.4 . . ? C34 C33 H33 126.4 . . ? Ru1 C33 H33 121.0 . . ? C35 C34 C33 108.1(7) . . ? C35 C34 Ru1 73.4(4) . . ? C33 C34 Ru1 70.5(4) . . ? C35 C34 H34 125.9 . . ? C33 C34 H34 125.9 . . ? Ru1 C34 H34 121.9 . . ? C31 C35 C34 107.0(7) . . ? C31 C35 Ru1 73.4(4) . . ? C34 C35 Ru1 68.5(4) . . ? C31 C35 H35 126.5 . . ? C34 C35 H35 126.5 . . ? Ru1 C35 H35 123.2 . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.376 _refine_diff_density_min -0.706 _refine_diff_density_rms 0.218