# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1580 data_3 _audit_creation_method SHELXL _chemical_name_systematic ; - ; _chemical_name_common - _chemical_formula_moiety 'C29 H31 Cl N O3 P Ru S2' _chemical_formula_structural 'C29 H31 Cl N O3 P Ru S2' _chemical_formula_analytical 'C29 H31 Cl N O3 P Ru S2' _chemical_formula_sum 'C29 H31 Cl N O3 P Ru S2' _chemical_formula_weight 673.16 _chemical_melting_point - _chemical_compound_source - 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5381(2) _cell_length_b 12.0819(2) _cell_length_c 13.0204(2) _cell_angle_alpha 76.4610(10) _cell_angle_beta 82.0010(10) _cell_angle_gamma 80.0140(10) _cell_volume 1429.02(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 37 _cell_measurement_theta_min 12 _cell_measurement_theta_max 166 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max .1 _exptl_crystal_size_mid .2 _exptl_crystal_size_min .4 _exptl_crystal_density_meas - _exptl_crystal_density_diffrn 1.564 _exptl_crystal_density_method - _exptl_crystal_F_000 688 _exptl_absorpt_coefficient_mu 0.876 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.26666 _exptl_absorpt_correction_T_max 0.40765 _exptl_special_details ; - ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device SMART _diffrn_measurement_method CCD _diffrn_standards_number - _diffrn_standards_interval_count - _diffrn_standards_interval_time - _diffrn_standards_decay_% - _diffrn_reflns_number 8802 _diffrn_reflns_av_R_equivalents 0.0292 _diffrn_reflns_av_sigmaI/netI 0.0371 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 28.73 _reflns_number_total 6386 _reflns_number_observed 5452 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART' _computing_cell_refinement 'SMART/SAINT' _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXTL' _computing_structure_refinement 'SHELXTL' _computing_molecular_graphics 'SHELXTL' _computing_publication_material 'SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0359P)^2^+0.8643P] 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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6386 _refine_ls_number_parameters 344 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0409 _refine_ls_R_factor_obs 0.0308 _refine_ls_wR_factor_all 0.0837 _refine_ls_wR_factor_obs 0.0765 _refine_ls_goodness_of_fit_all 1.063 _refine_ls_goodness_of_fit_obs 1.057 _refine_ls_restrained_S_all 1.063 _refine_ls_restrained_S_obs 1.057 _refine_ls_shift/esd_max -0.836 _refine_ls_shift/esd_mean 0.003 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ru1 Ru 0.20447(2) 0.24155(2) 0.233921(15) 0.02903(7) Uani 1 d . . Cl1 Cl 0.07539(7) 0.35366(6) 0.08704(5) 0.0405(2) Uani 1 d . . N1 N 0.3893(2) 0.2617(2) 0.1259(2) 0.0331(5) Uani 1 d . . C1 C 0.4140(3) 0.2152(2) 0.0430(2) 0.0395(6) Uani 1 d . . H1A H 0.4908(3) 0.2376(2) -0.0052(2) 0.047 Uiso 1 calc R . C2 C 0.3393(3) 0.1348(2) 0.0157(2) 0.0411(6) Uani 1 d . . C3 C 0.2267(3) 0.0827(2) 0.0811(2) 0.0416(6) Uani 1 d . . O3 O 0.1717(2) 0.1028(2) 0.1741(2) 0.0450(5) Uani 1 d . . C4 C 0.1722(4) 0.0001(3) 0.0426(3) 0.0592(9) Uani 1 d . . H4A H 0.0998(4) -0.0373(3) 0.0843(3) 0.071 Uiso 1 calc R . C5 C 0.2220(4) -0.0268(3) -0.0538(3) 0.0658(10) Uani 1 d . . H5A H 0.1833(4) -0.0821(3) -0.0754(3) 0.079 Uiso 1 calc R . C6 C 0.3286(4) 0.0266(3) -0.1195(3) 0.0658(10) Uani 1 d . . H6A H 0.3595(4) 0.0098(3) -0.1858(3) 0.079 Uiso 1 calc R . C7 C 0.3877(4) 0.1047(3) -0.0845(3) 0.0551(8) Uani 1 d . . H7A H 0.4615(4) 0.1394(3) -0.1272(3) 0.066 Uiso 1 calc R . C8 C 0.4781(3) 0.3448(2) 0.1312(2) 0.0339(5) Uani 1 d . . P1 P 0.26101(7) 0.39824(6) 0.28283(5) 0.03077(14) Uani 1 d . . C9 C 0.4234(3) 0.4239(2) 0.1950(2) 0.0350(5) Uani 1 d . . C10 C 0.4986(3) 0.5146(3) 0.1944(2) 0.0441(6) Uani 1 d . . H10A H 0.4600(3) 0.5689(3) 0.2347(2) 0.053 Uiso 1 calc R . C11 C 0.6288(3) 0.5238(3) 0.1348(2) 0.0463(7) Uani 1 d . . H11A H 0.6779(3) 0.5840(3) 0.1344(2) 0.056 Uiso 1 calc R . C12 C 0.6858(3) 0.4418(3) 0.0754(2) 0.0491(7) Uani 1 d . . H12A H 0.7747(3) 0.4468(3) 0.0362(2) 0.059 Uiso 1 calc R . C13 C 0.6133(3) 0.3535(3) 0.0734(2) 0.0447(7) Uani 1 d . . H13A H 0.6538(3) 0.2992(3) 0.0335(2) 0.054 Uiso 1 calc R . C14 C 0.1584(3) 0.5453(2) 0.2679(2) 0.0380(6) Uani 1 d . . C15 C 0.0803(3) 0.5917(3) 0.1808(2) 0.0459(7) Uani 1 d . . H15A H 0.0747(3) 0.5464(3) 0.1332(2) 0.055 Uiso 1 calc R . C16 C 0.0105(4) 0.7051(3) 0.1637(3) 0.0593(9) Uani 1 d . . H16A H -0.0402(4) 0.7353(3) 0.1049(3) 0.071 Uiso 1 calc R . C17 C 0.0175(4) 0.7721(3) 0.2354(3) 0.0648(10) Uani 1 d . . H17A H -0.0306(4) 0.8471(3) 0.2252(3) 0.078 Uiso 1 calc R . C18 C 0.0948(4) 0.7290(3) 0.3215(3) 0.0606(9) Uani 1 d . . H18A H 0.1005(4) 0.7751(3) 0.3683(3) 0.073 Uiso 1 calc R . C19 C 0.1649(3) 0.6153(3) 0.3383(3) 0.0499(7) Uani 1 d . . H19A H 0.2163(3) 0.5861(3) 0.3969(3) 0.060 Uiso 1 calc R . C20 C 0.3203(3) 0.3753(2) 0.4155(2) 0.0376(6) Uani 1 d . . C21 C 0.4642(3) 0.3492(3) 0.4322(2) 0.0482(7) Uani 1 d . . H21A H 0.5332(3) 0.3475(3) 0.3744(2) 0.058 Uiso 1 calc R . C22 C 0.5066(4) 0.3256(3) 0.5336(3) 0.0649(10) Uani 1 d . . H22A H 0.6033(4) 0.3083(3) 0.5435(3) 0.078 Uiso 1 calc R . C23 C 0.4054(5) 0.3278(3) 0.6195(3) 0.0725(12) Uani 1 d . . H23A H 0.4338(5) 0.3116(3) 0.6876(3) 0.087 Uiso 1 calc R . C24 C 0.2629(5) 0.3536(3) 0.6053(3) 0.0702(11) Uani 1 d . . H24A H 0.1951(5) 0.3555(3) 0.6638(3) 0.084 Uiso 1 calc R . C25 C 0.2187(4) 0.3772(3) 0.5033(2) 0.0536(8) Uani 1 d . . H25A H 0.1217(4) 0.3941(3) 0.4942(2) 0.064 Uiso 1 calc R . S1 S 0.34291(7) 0.11071(6) 0.35093(6) 0.0389(2) Uani 1 d . . O1 O 0.4968(2) 0.1219(2) 0.3370(2) 0.0575(6) Uani 1 d . . C26 C 0.3330(5) -0.0321(3) 0.3397(4) 0.0786(13) Uani 1 d . . H26A H 0.3587(5) -0.0387(3) 0.2672(4) 0.118 Uiso 1 calc R . H26B H 0.2372(5) -0.0487(3) 0.3619(4) 0.118 Uiso 1 calc R . H26C H 0.3978(5) -0.0858(3) 0.3841(4) 0.118 Uiso 1 calc R . C27 C 0.2900(4) 0.0903(3) 0.4909(2) 0.0638(10) Uani 1 d . . H27A H 0.2888(4) 0.1608(3) 0.5132(2) 0.096 Uiso 1 calc R . H27B H 0.3567(4) 0.0310(3) 0.5284(2) 0.096 Uiso 1 calc R . H27C H 0.1961(4) 0.0682(3) 0.5061(2) 0.096 Uiso 1 calc R . S2 S -0.01179(7) 0.22676(6) 0.33466(5) 0.0380(2) Uani 1 d . . O2 O -0.0212(3) 0.1697(2) 0.4483(2) 0.0637(7) Uani 1 d . . C28 C -0.1225(4) 0.1613(4) 0.2731(3) 0.0662(10) Uani 1 d . . H28A H -0.0780(4) 0.0844(4) 0.2700(3) 0.099 Uiso 1 calc R . H28B H -0.1345(4) 0.2055(4) 0.2025(3) 0.099 Uiso 1 calc R . H28C H -0.2143(4) 0.1590(4) 0.3139(3) 0.099 Uiso 1 calc R . C29 C -0.1204(3) 0.3636(3) 0.3288(3) 0.0586(9) Uani 1 d . . H29A H -0.0749(3) 0.4110(3) 0.3597(3) 0.088 Uiso 1 calc R . H29B H -0.2123(3) 0.3535(3) 0.3674(3) 0.088 Uiso 1 calc R . H29C H -0.1325(3) 0.4001(3) 0.2560(3) 0.088 Uiso 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 Ru1 0.02736(11) 0.03292(12) 0.02776(11) -0.00788(8) -0.00400(7) -0.00425(7) Cl1 0.0376(3) 0.0481(4) 0.0357(3) -0.0068(3) -0.0121(3) -0.0028(3) N1 0.0310(11) 0.0379(12) 0.0295(10) -0.0083(9) -0.0036(8) -0.0010(9) C1 0.0353(14) 0.046(2) 0.0344(13) -0.0090(12) -0.0013(11) 0.0019(11) C2 0.043(2) 0.0423(15) 0.0382(14) -0.0149(12) -0.0093(12) 0.0057(12) C3 0.046(2) 0.0381(15) 0.043(2) -0.0141(12) -0.0138(12) 0.0034(12) O3 0.0544(12) 0.0423(11) 0.0423(11) -0.0141(9) -0.0042(9) -0.0122(9) C4 0.068(2) 0.057(2) 0.063(2) -0.027(2) -0.013(2) -0.010(2) C5 0.071(2) 0.065(2) 0.075(2) -0.042(2) -0.024(2) 0.004(2) C6 0.071(2) 0.076(2) 0.057(2) -0.041(2) -0.019(2) 0.015(2) C7 0.056(2) 0.067(2) 0.044(2) -0.025(2) -0.0089(14) 0.009(2) C8 0.0290(12) 0.0411(14) 0.0289(12) -0.0021(10) -0.0054(10) -0.0035(10) P1 0.0279(3) 0.0368(3) 0.0295(3) -0.0097(3) -0.0025(2) -0.0066(3) C9 0.0315(13) 0.0435(15) 0.0309(12) -0.0076(11) -0.0029(10) -0.0085(11) C10 0.046(2) 0.048(2) 0.042(2) -0.0086(13) -0.0054(12) -0.0161(13) C11 0.040(2) 0.053(2) 0.046(2) 0.0020(14) -0.0088(12) -0.0201(13) C12 0.0322(14) 0.068(2) 0.041(2) 0.0029(14) -0.0024(12) -0.0134(14) C13 0.0320(14) 0.059(2) 0.0407(15) -0.0103(13) 0.0000(11) -0.0028(13) C14 0.0392(14) 0.0383(14) 0.0372(14) -0.0115(11) 0.0022(11) -0.0081(11) C15 0.058(2) 0.042(2) 0.0360(14) -0.0108(12) -0.0040(13) -0.0005(13) C16 0.073(2) 0.050(2) 0.048(2) -0.0047(15) -0.010(2) 0.004(2) C17 0.083(3) 0.040(2) 0.065(2) -0.012(2) -0.001(2) 0.002(2) C18 0.076(2) 0.044(2) 0.068(2) -0.026(2) -0.006(2) -0.007(2) C19 0.056(2) 0.046(2) 0.055(2) -0.0208(14) -0.0105(15) -0.0088(14) C20 0.0411(14) 0.0428(15) 0.0328(13) -0.0107(11) -0.0047(11) -0.0125(12) C21 0.047(2) 0.056(2) 0.044(2) -0.0041(14) -0.0125(13) -0.0170(14) C22 0.075(2) 0.067(2) 0.061(2) 0.001(2) -0.038(2) -0.028(2) C23 0.122(4) 0.066(2) 0.042(2) -0.006(2) -0.033(2) -0.035(2) C24 0.105(3) 0.076(3) 0.036(2) -0.018(2) 0.002(2) -0.028(2) C25 0.058(2) 0.066(2) 0.039(2) -0.0164(15) 0.0017(14) -0.013(2) S1 0.0384(4) 0.0368(3) 0.0395(4) -0.0043(3) -0.0091(3) -0.0016(3) O1 0.0377(11) 0.0690(15) 0.0591(14) 0.0009(11) -0.0137(10) -0.0026(10) C26 0.103(3) 0.037(2) 0.100(3) -0.012(2) -0.045(3) 0.001(2) C27 0.064(2) 0.075(2) 0.037(2) 0.008(2) -0.0084(15) 0.006(2) S2 0.0326(3) 0.0488(4) 0.0345(3) -0.0104(3) -0.0018(3) -0.0110(3) O2 0.0532(13) 0.093(2) 0.0377(11) -0.0020(11) 0.0031(10) -0.0140(13) C28 0.054(2) 0.089(3) 0.071(2) -0.031(2) -0.004(2) -0.036(2) C29 0.035(2) 0.064(2) 0.074(2) -0.019(2) 0.0022(15) -0.0001(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 O3 2.092(2) . ? Ru1 N1 2.108(2) . ? Ru1 S1 2.2960(7) . ? Ru1 S2 2.2961(7) . ? Ru1 P1 2.3009(7) . ? Ru1 Cl1 2.4232(7) . ? N1 C1 1.305(3) . ? N1 C8 1.439(3) . ? C1 C2 1.432(4) . ? C2 C3 1.415(4) . ? C2 C7 1.429(4) . ? C3 O3 1.310(3) . ? C3 C4 1.416(4) . ? C4 C5 1.370(5) . ? C5 C6 1.381(6) . ? C6 C7 1.369(5) . ? C8 C9 1.398(4) . ? C8 C13 1.408(4) . ? P1 C9 1.819(3) . ? P1 C20 1.837(3) . ? P1 C14 1.855(3) . ? C9 C10 1.409(4) . ? C10 C11 1.376(4) . ? C11 C12 1.390(5) . ? C12 C13 1.376(4) . ? C14 C15 1.396(4) . ? C14 C19 1.399(4) . ? C15 C16 1.398(4) . ? C16 C17 1.386(5) . ? C17 C18 1.377(5) . ? C18 C19 1.401(5) . ? C20 C21 1.389(4) . ? C20 C25 1.394(4) . ? C21 C22 1.386(4) . ? C22 C23 1.374(6) . ? C23 C24 1.369(6) . ? C24 C25 1.399(5) . ? S1 O1 1.479(2) . ? S1 C26 1.785(4) . ? S1 C27 1.793(3) . ? S2 O2 1.477(2) . ? S2 C29 1.784(3) . ? S2 C28 1.789(3) . ? 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 O3 Ru1 N1 90.16(8) . . ? O3 Ru1 S1 87.22(6) . . ? N1 Ru1 S1 88.87(6) . . ? O3 Ru1 S2 87.41(6) . . ? N1 Ru1 S2 173.31(6) . . ? S1 Ru1 S2 97.23(3) . . ? O3 Ru1 P1 173.18(6) . . ? N1 Ru1 P1 83.12(6) . . ? S1 Ru1 P1 93.84(2) . . ? S2 Ru1 P1 99.14(2) . . ? O3 Ru1 Cl1 83.11(6) . . ? N1 Ru1 Cl1 85.20(6) . . ? S1 Ru1 Cl1 168.62(3) . . ? S2 Ru1 Cl1 88.32(2) . . ? P1 Ru1 Cl1 95.07(2) . . ? C1 N1 C8 117.5(2) . . ? C1 N1 Ru1 121.7(2) . . ? C8 N1 Ru1 119.8(2) . . ? N1 C1 C2 129.1(3) . . ? C3 C2 C7 119.4(3) . . ? C3 C2 C1 124.9(2) . . ? C7 C2 C1 115.7(3) . . ? O3 C3 C4 118.0(3) . . ? O3 C3 C2 125.7(3) . . ? C4 C3 C2 116.3(3) . . ? C3 O3 Ru1 124.7(2) . . ? C5 C4 C3 122.5(4) . . ? C4 C5 C6 121.4(3) . . ? C7 C6 C5 118.4(3) . . ? C6 C7 C2 122.0(3) . . ? C9 C8 C13 118.5(3) . . ? C9 C8 N1 117.5(2) . . ? C13 C8 N1 124.1(2) . . ? C9 P1 C20 102.92(12) . . ? C9 P1 C14 101.88(12) . . ? C20 P1 C14 101.51(13) . . ? C9 P1 Ru1 101.31(9) . . ? C20 P1 Ru1 117.37(9) . . ? C14 P1 Ru1 128.13(9) . . ? C8 C9 C10 119.9(2) . . ? C8 C9 P1 117.3(2) . . ? C10 C9 P1 122.6(2) . . ? C11 C10 C9 120.7(3) . . ? C10 C11 C12 119.2(3) . . ? C13 C12 C11 121.2(3) . . ? C12 C13 C8 120.4(3) . . ? C15 C14 C19 118.2(3) . . ? C15 C14 P1 120.1(2) . . ? C19 C14 P1 121.5(2) . . ? C14 C15 C16 121.2(3) . . ? C17 C16 C15 119.3(3) . . ? C18 C17 C16 120.7(3) . . ? C17 C18 C19 119.8(3) . . ? C14 C19 C18 120.7(3) . . ? C21 C20 C25 118.5(3) . . ? C21 C20 P1 121.9(2) . . ? C25 C20 P1 119.5(2) . . ? C22 C21 C20 121.1(3) . . ? C23 C22 C21 119.8(4) . . ? C24 C23 C22 120.3(3) . . ? C23 C24 C25 120.5(4) . . ? C20 C25 C24 119.8(3) . . ? O1 S1 C26 106.4(2) . . ? O1 S1 C27 105.9(2) . . ? C26 S1 C27 96.8(2) . . ? O1 S1 Ru1 115.61(9) . . ? C26 S1 Ru1 110.02(13) . . ? C27 S1 Ru1 119.82(12) . . ? O2 S2 C29 105.2(2) . . ? O2 S2 C28 106.7(2) . . ? C29 S2 C28 98.7(2) . . ? O2 S2 Ru1 121.73(10) . . ? C29 S2 Ru1 111.87(11) . . ? C28 S2 Ru1 110.09(13) . . ? _refine_diff_density_max 0.575 _refine_diff_density_min -0.645 _refine_diff_density_rms 0.083 #---END data_9 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common - _chemical_formula_moiety 'C56 H50 N2 O4 P2 Ru.[O H2].[C H2 Cl2]0.2' _chemical_formula_structural 'C56.20 H54.40 Cl0.40 N2 O4 P2 Ru' _chemical_formula_analytical 'C56.20 H54.40 Cl0.40 N2 O4 P2 Ru' _chemical_formula_sum 'C56.20 H54.40 Cl0.40 N2 O4 P2 Ru' _chemical_formula_weight 999.01 _chemical_melting_point - _chemical_compound_source - 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' 'Ru' 'Ru' -1.2594 0.8363 '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' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P3(1)21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' 'y, x, -z' 'x-y, -y, -z+2/3' '-x, -x+y, -z+1/3' _cell_length_a 19.90540(10) _cell_length_b 19.90540(10) _cell_length_c 12.04170(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4132.00(5) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 38 _cell_measurement_theta_min 12 _cell_measurement_theta_max 166 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max .08 _exptl_crystal_size_mid .15 _exptl_crystal_size_min .3 _exptl_crystal_density_meas - _exptl_crystal_density_diffrn 1.204 _exptl_crystal_density_method - _exptl_crystal_F_000 1555 _exptl_absorpt_coefficient_mu 0.405 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.857257 _exptl_absorpt_correction_T_max 1.000000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device SMART _diffrn_measurement_method CCD _diffrn_standards_number - _diffrn_standards_interval_count - _diffrn_standards_interval_time - _diffrn_standards_decay_% - _diffrn_reflns_number 18400 _diffrn_reflns_av_R_equivalents 0.0483 _diffrn_reflns_av_sigmaI/netI 0.0381 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.18 _diffrn_reflns_theta_max 23.27 _reflns_number_total 3970 _reflns_number_observed 3389 _reflns_observed_criterion >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART/SAINT _computing_data_reduction SAINT _computing_structure_solution SHELXTL _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement on F^2^ for ALL reflections except for 50 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1154P)^2^+2.8384P] 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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0036(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(6) _refine_ls_number_reflns 3920 _refine_ls_number_parameters 296 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0698 _refine_ls_R_factor_obs 0.0493 _refine_ls_wR_factor_all 0.1934 _refine_ls_wR_factor_obs 0.1281 _refine_ls_goodness_of_fit_all 0.882 _refine_ls_goodness_of_fit_obs 0.854 _refine_ls_restrained_S_all 1.206 _refine_ls_restrained_S_obs 0.854 _refine_ls_shift/esd_max 0.116 _refine_ls_shift/esd_mean 0.011 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ru1 Ru 1.43936(3) 0.0000 1.8333 0.0454(2) Uani 1 d S . O1 O 1.3215(2) -0.0565(3) 1.7716(3) 0.0595(10) Uani 1 d . . C1 C 1.3214(4) -0.0510(4) 1.6534(5) 0.062(2) Uani 1 d . . H1A H 1.3357(4) -0.0880(4) 1.6236(5) 0.074 Uiso 1 calc R . C2 C 1.3859(4) 0.0319(4) 1.6173(5) 0.063(2) Uani 1 d . . H2A H 1.3952(4) 0.0308(4) 1.5376(5) 0.075 Uiso 1 calc R . N3 N 1.4577(3) 0.0487(3) 1.6775(4) 0.0513(11) Uani 1 d . . C3 C 1.5208(4) 0.0913(4) 1.6209(5) 0.058(2) Uani 1 d . . H3A H 1.5136(4) 0.1026(4) 1.5484(5) 0.069 Uiso 1 calc R . C4 C 1.2418(5) -0.0741(4) 1.6088(7) 0.079(2) Uani 1 d . . C5 C 1.1799(5) -0.1021(8) 1.6735(10) 0.135(5) Uani 1 d . . H5A H 1.1850(5) -0.1037(8) 1.7501(10) 0.163 Uiso 1 calc R . C6 C 1.1088(7) -0.1287(11) 1.6268(17) 0.203(9) Uani 1 d . . H6A H 1.0653(7) -0.1544(11) 1.6721(17) 0.243 Uiso 1 calc R . C7 C 1.0984(7) -0.1201(8) 1.5228(15) 0.152(5) Uani 1 d . . H7A H 1.0498(7) -0.1322(8) 1.4964(15) 0.183 Uiso 1 calc R . C8 C 1.1580(8) -0.0941(8) 1.4556(9) 0.117(4) Uani 1 d . . H8A H 1.1502(8) -0.0926(8) 1.3797(9) 0.140 Uiso 1 calc R . C9 C 1.2311(6) -0.0693(6) 1.4942(8) 0.103(3) Uani 1 d . . H9A H 1.2731(6) -0.0496(6) 1.4457(8) 0.124 Uiso 1 calc R . C10 C 1.3680(5) 0.0967(4) 1.6389(6) 0.074(2) Uani 1 d . . H10A H 1.4107(5) 0.1451(4) 1.6141(6) 0.112 Uiso 1 calc R . H10B H 1.3602(5) 0.0996(4) 1.7171(6) 0.112 Uiso 1 calc R . H10C H 1.3219(5) 0.0862(4) 1.5993(6) 0.112 Uiso 1 calc R . P1 P 1.56095(9) 0.09082(9) 1.88246(12) 0.0479(4) Uani 1 d . . C11 C 1.5731(4) 0.1848(4) 1.9292(5) 0.059(2) Uani 1 d . . C12 C 1.5243(5) 0.2098(4) 1.8952(6) 0.074(2) Uani 1 d . . H12A H 1.4810(5) 0.1764(4) 1.8534(6) 0.089 Uiso 1 calc R . C13 C 1.5362(6) 0.2825(5) 1.9199(8) 0.086(2) Uani 1 d . . H13A H 1.5011(6) 0.2974(5) 1.8958(8) 0.103 Uiso 1 calc R . C14 C 1.6003(7) 0.3329(5) 1.9803(7) 0.097(3) Uani 1 d . . H14A H 1.6091(7) 0.3821(5) 1.9976(7) 0.116 Uiso 1 calc R . C15 C 1.6516(7) 0.3096(5) 2.0151(7) 0.095(3) Uani 1 d . . H15A H 1.6952(7) 0.3435(5) 2.0560(7) 0.114 Uiso 1 calc R . C16 C 1.6390(6) 0.2369(4) 1.9899(6) 0.082(2) Uani 1 d . . H16A H 1.6743(6) 0.2221(4) 2.0133(6) 0.098 Uiso 1 calc R . C17 C 1.6294(4) 0.1276(4) 1.7660(5) 0.0554(15) Uani 1 d . . C18 C 1.6007(4) 0.1235(4) 1.6558(5) 0.056(2) Uani 1 d . . C19 C 1.6549(4) 0.1582(4) 1.5698(6) 0.073(2) Uani 1 d . . H19A H 1.6375(4) 0.1548(4) 1.4972(6) 0.088 Uiso 1 calc R . C20 C 1.7318(5) 0.1964(6) 1.5906(7) 0.096(3) Uani 1 d . . H20A H 1.7667(5) 0.2198(6) 1.5325(7) 0.115 Uiso 1 calc R . C21 C 1.7589(5) 0.2009(6) 1.6961(8) 0.095(3) Uani 1 d . . H21A H 1.8121(5) 0.2267(6) 1.7093(8) 0.114 Uiso 1 calc R . C22 C 1.7075(4) 0.1672(4) 1.7834(6) 0.073(2) Uani 1 d . . H22A H 1.7265(4) 0.1716(4) 1.8552(6) 0.088 Uiso 1 calc R . C23 C 1.6085(4) 0.0675(4) 1.9934(5) 0.056(2) Uani 1 d . . C24 C 1.5835(4) 0.0692(4) 2.1014(5) 0.066(2) Uani 1 d . . H24A H 1.5491(4) 0.0872(4) 2.1141(5) 0.080 Uiso 1 calc R . C25 C 1.6106(6) 0.0434(5) 2.1916(6) 0.080(2) Uani 1 d . . H25A H 1.5933(6) 0.0433(5) 2.2633(6) 0.096 Uiso 1 calc R . C26 C 1.6621(6) 0.0187(6) 2.1722(7) 0.101(3) Uani 1 d . . H26A H 1.6795(6) 0.0013(6) 2.2313(7) 0.121 Uiso 1 calc R . C27 C 1.6891(6) 0.0189(6) 2.0653(8) 0.100(3) Uani 1 d . . H27A H 1.7257(6) 0.0036(6) 2.0540(8) 0.120 Uiso 1 calc R . C28 C 1.6614(5) 0.0420(5) 1.9756(6) 0.076(2) Uani 1 d . . H28A H 1.6781(5) 0.0404(5) 1.9040(6) 0.092 Uiso 1 calc R . O30 O 1.4603 0.0671 1.3270 0.084 Uani 1 d . . H30A H 1.4791 0.0658 1.4020 0.101 Uiso 1 d . . H30B H 1.4244 0.0873 1.3318 0.101 Uiso 1 d . . C50 C 1.1202(42) 0.1202(42) 1.5000 0.108(21) Uiso 0.20 d SP . Cl1 Cl 1.1611(13) 0.2304(13) 1.4996(18) 0.086(6) Uiso 0.10 d P . Cl2 Cl 1.0752(27) 0.0658(27) 1.4429(34) 0.166(14) Uiso 0.10 d P . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0508(3) 0.0462(4) 0.0377(3) 0.0036(3) 0.00181(15) 0.0231(2) O1 0.054(2) 0.064(3) 0.056(2) 0.007(2) 0.000(2) 0.026(2) C1 0.061(4) 0.066(4) 0.055(4) -0.003(3) -0.012(3) 0.029(4) C2 0.073(4) 0.069(4) 0.046(3) 0.007(3) -0.009(3) 0.036(4) N3 0.056(3) 0.058(3) 0.043(3) 0.004(2) -0.002(2) 0.031(2) C3 0.069(4) 0.062(4) 0.046(3) 0.007(3) -0.001(3) 0.035(4) C4 0.083(5) 0.069(4) 0.086(5) -0.007(4) -0.012(5) 0.038(4) C5 0.065(6) 0.187(13) 0.114(8) 0.036(8) -0.004(5) 0.032(7) C6 0.065(7) 0.243(19) 0.196(16) 0.052(13) -0.040(9) -0.002(9) C7 0.077(8) 0.172(13) 0.172(14) -0.010(11) -0.066(9) 0.036(8) C8 0.111(8) 0.165(11) 0.093(7) -0.046(7) -0.052(7) 0.083(8) C9 0.115(8) 0.131(8) 0.084(6) -0.030(5) -0.037(5) 0.076(7) C10 0.078(5) 0.063(4) 0.081(5) 0.010(4) -0.015(4) 0.034(4) P1 0.0541(9) 0.0484(8) 0.0362(8) 0.0022(6) -0.0001(6) 0.0219(7) C11 0.076(4) 0.057(4) 0.038(3) 0.001(3) 0.000(3) 0.029(3) C12 0.077(5) 0.068(5) 0.074(5) 0.007(4) 0.007(4) 0.035(4) C13 0.110(7) 0.069(5) 0.094(6) 0.019(5) 0.027(5) 0.057(5) C14 0.145(9) 0.049(4) 0.075(5) -0.001(4) 0.035(6) 0.032(6) C15 0.130(8) 0.061(5) 0.082(6) -0.007(4) -0.001(5) 0.039(5) C16 0.119(7) 0.051(4) 0.060(4) -0.007(3) -0.011(4) 0.031(4) C17 0.058(4) 0.053(4) 0.051(4) 0.005(3) 0.009(3) 0.025(3) C18 0.063(4) 0.054(4) 0.048(4) 0.014(3) 0.007(3) 0.026(3) C19 0.074(5) 0.084(5) 0.051(4) 0.017(4) 0.015(3) 0.033(4) C20 0.076(6) 0.111(7) 0.071(6) 0.024(5) 0.027(5) 0.025(5) C21 0.055(4) 0.111(7) 0.079(6) 0.004(5) 0.005(4) 0.012(5) C22 0.054(4) 0.078(5) 0.065(4) -0.001(4) 0.000(4) 0.015(4) C23 0.059(4) 0.057(4) 0.043(3) 0.003(3) -0.009(3) 0.023(3) C24 0.089(5) 0.057(4) 0.043(3) 0.001(3) -0.005(3) 0.029(4) C25 0.113(7) 0.078(5) 0.049(4) 0.003(4) -0.014(4) 0.047(5) C26 0.128(8) 0.112(7) 0.065(6) 0.011(5) -0.034(5) 0.063(7) C27 0.102(7) 0.144(9) 0.082(7) 0.003(6) -0.023(5) 0.082(7) C28 0.087(5) 0.099(6) 0.057(4) 0.003(4) -0.009(4) 0.057(5) O30 0.143 0.126 0.028 -0.001 0.004 0.101 _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 N3 2.059(5) . ? Ru1 N3 2.059(5) 5_558 ? Ru1 O1 2.164(4) 5_558 ? Ru1 O1 2.164(4) . ? Ru1 P1 2.258(2) . ? Ru1 P1 2.259(2) 5_558 ? O1 C1 1.427(7) . ? C1 C4 1.511(11) . ? C1 C2 1.563(10) . ? C2 N3 1.484(8) . ? C2 C10 1.523(10) . ? N3 C3 1.303(8) . ? C3 C18 1.447(10) . ? C4 C5 1.322(13) . ? C4 C9 1.407(12) . ? C5 C6 1.36(2) . ? C6 C7 1.29(2) . ? C7 C8 1.31(2) . ? C8 C9 1.364(14) . ? P1 C23 1.826(6) . ? P1 C17 1.834(6) . ? P1 C11 1.850(7) . ? C11 C12 1.357(10) . ? C11 C16 1.404(11) . ? C12 C13 1.378(11) . ? C13 C14 1.372(14) . ? C14 C15 1.381(15) . ? C15 C16 1.374(11) . ? C17 C22 1.362(10) . ? C17 C18 1.430(9) . ? C18 C19 1.403(9) . ? C19 C20 1.350(12) . ? C20 C21 1.365(12) . ? C21 C22 1.385(11) . ? C23 C28 1.396(10) . ? C23 C24 1.398(9) . ? C24 C25 1.418(10) . ? C25 C26 1.360(13) . ? C26 C27 1.394(13) . ? C27 C28 1.392(11) . ? C50 Cl2 1.22(6) . ? C50 Cl2 1.22(6) 4_648 ? C50 Cl1 1.92(7) . ? C50 Cl1 1.92(7) 4_648 ? Cl1 Cl1 2.39(5) 4_648 ? Cl2 Cl2 1.41(8) 4_648 ? 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 N3 Ru1 N3 173.4(3) . 5_558 ? N3 Ru1 O1 94.7(2) . 5_558 ? N3 Ru1 O1 79.8(2) 5_558 5_558 ? N3 Ru1 O1 79.8(2) . . ? N3 Ru1 O1 94.7(2) 5_558 . ? O1 Ru1 O1 69.0(3) 5_558 . ? N3 Ru1 P1 89.71(15) . . ? N3 Ru1 P1 94.73(15) 5_558 . ? O1 Ru1 P1 98.70(15) 5_558 . ? O1 Ru1 P1 162.82(14) . . ? N3 Ru1 P1 94.73(15) . 5_558 ? N3 Ru1 P1 89.71(14) 5_558 5_558 ? O1 Ru1 P1 162.82(14) 5_558 5_558 ? O1 Ru1 P1 98.71(15) . 5_558 ? P1 Ru1 P1 95.65(8) . 5_558 ? C1 O1 Ru1 110.2(3) . . ? O1 C1 C4 111.9(6) . . ? O1 C1 C2 109.0(5) . . ? C4 C1 C2 113.9(6) . . ? N3 C2 C10 109.4(5) . . ? N3 C2 C1 107.0(5) . . ? C10 C2 C1 115.5(6) . . ? C3 N3 C2 113.4(5) . . ? C3 N3 Ru1 132.1(4) . . ? C2 N3 Ru1 114.5(4) . . ? N3 C3 C18 128.6(6) . . ? C5 C4 C9 117.8(9) . . ? C5 C4 C1 122.2(8) . . ? C9 C4 C1 120.0(8) . . ? C6 C5 C4 119.3(13) . . ? C7 C6 C5 123.5(14) . . ? C8 C7 C6 118.5(12) . . ? C7 C8 C9 121.6(11) . . ? C4 C9 C8 118.7(11) . . ? C23 P1 C17 106.6(3) . . ? C23 P1 C11 102.2(3) . . ? C17 P1 C11 97.7(3) . . ? C23 P1 Ru1 118.2(2) . . ? C17 P1 Ru1 113.8(2) . . ? C11 P1 Ru1 115.8(2) . . ? C12 C11 C16 117.6(7) . . ? C12 C11 P1 121.6(6) . . ? C16 C11 P1 120.4(6) . . ? C11 C12 C13 122.8(8) . . ? C14 C13 C12 119.4(9) . . ? C13 C14 C15 119.3(8) . . ? C16 C15 C14 120.7(9) . . ? C15 C16 C11 120.2(9) . . ? C22 C17 C18 118.9(6) . . ? C22 C17 P1 121.2(5) . . ? C18 C17 P1 119.4(5) . . ? C19 C18 C17 118.0(6) . . ? C19 C18 C3 114.0(6) . . ? C17 C18 C3 127.9(6) . . ? C20 C19 C18 121.1(7) . . ? C19 C20 C21 120.6(7) . . ? C22 C21 C20 120.1(8) . . ? C21 C22 C17 121.1(8) . . ? C28 C23 C24 119.6(6) . . ? C28 C23 P1 124.1(5) . . ? C24 C23 P1 116.0(5) . . ? C25 C24 C23 119.9(8) . . ? C26 C25 C24 119.5(8) . . ? C25 C26 C27 121.1(8) . . ? C28 C27 C26 120.1(8) . . ? C23 C28 C27 119.8(8) . . ? Cl2 C50 Cl2 70.9(59) . 4_648 ? Cl2 C50 Cl1 136.2(22) . . ? Cl2 C50 Cl1 124.0(22) 4_648 . ? Cl2 C50 Cl1 123.6(22) . 4_648 ? Cl2 C50 Cl1 135.8(22) 4_648 4_648 ? Cl1 C50 Cl1 77.0(33) . 4_648 ? C50 Cl1 Cl1 51.6(17) . 4_648 ? C50 Cl2 Cl2 54.5(30) . 4_648 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Ru1 O1 C1 18.4(4) . . . . ? N3 Ru1 O1 C1 -165.4(4) 5_558 . . . ? O1 Ru1 O1 C1 117.5(5) 5_558 . . . ? P1 Ru1 O1 C1 71.4(6) . . . . ? P1 Ru1 O1 C1 -74.9(4) 5_558 . . . ? Ru1 O1 C1 C4 -167.8(5) . . . . ? Ru1 O1 C1 C2 -40.9(6) . . . . ? O1 C1 C2 N3 48.1(7) . . . . ? C4 C1 C2 N3 173.9(6) . . . . ? O1 C1 C2 C10 -73.9(7) . . . . ? C4 C1 C2 C10 51.8(8) . . . . ? C10 C2 N3 C3 -87.5(7) . . . . ? C1 C2 N3 C3 146.7(6) . . . . ? C10 C2 N3 Ru1 92.9(6) . . . . ? C1 C2 N3 Ru1 -32.9(6) . . . . ? N3 Ru1 N3 C3 156.0(6) 5_558 . . . ? O1 Ru1 N3 C3 122.4(6) 5_558 . . . ? O1 Ru1 N3 C3 -169.9(6) . . . . ? P1 Ru1 N3 C3 23.7(6) . . . . ? P1 Ru1 N3 C3 -71.9(6) 5_558 . . . ? N3 Ru1 N3 C2 -24.5(4) 5_558 . . . ? O1 Ru1 N3 C2 -58.1(4) 5_558 . . . ? O1 Ru1 N3 C2 9.5(4) . . . . ? P1 Ru1 N3 C2 -156.8(4) . . . . ? P1 Ru1 N3 C2 107.6(4) 5_558 . . . ? C2 N3 C3 C18 175.0(6) . . . . ? Ru1 N3 C3 C18 -5.5(10) . . . . ? O1 C1 C4 C5 -5.5(13) . . . . ? C2 C1 C4 C5 -129.7(10) . . . . ? O1 C1 C4 C9 177.4(7) . . . . ? C2 C1 C4 C9 53.2(10) . . . . ? C9 C4 C5 C6 3.4(20) . . . . ? C1 C4 C5 C6 -173.8(13) . . . . ? C4 C5 C6 C7 -8.3(30) . . . . ? C5 C6 C7 C8 9.6(30) . . . . ? C6 C7 C8 C9 -6.3(25) . . . . ? C5 C4 C9 C8 -0.5(15) . . . . ? C1 C4 C9 C8 176.8(9) . . . . ? C7 C8 C9 C4 1.9(19) . . . . ? N3 Ru1 P1 C23 -154.6(3) . . . . ? N3 Ru1 P1 C23 30.3(3) 5_558 . . . ? O1 Ru1 P1 C23 110.7(3) 5_558 . . . ? O1 Ru1 P1 C23 153.5(5) . . . . ? P1 Ru1 P1 C23 -59.9(2) 5_558 . . . ? N3 Ru1 P1 C17 -28.4(3) . . . . ? N3 Ru1 P1 C17 156.5(3) 5_558 . . . ? O1 Ru1 P1 C17 -123.1(3) 5_558 . . . ? O1 Ru1 P1 C17 -80.3(5) . . . . ? P1 Ru1 P1 C17 66.3(2) 5_558 . . . ? N3 Ru1 P1 C11 83.7(3) . . . . ? N3 Ru1 P1 C11 -91.4(3) 5_558 . . . ? O1 Ru1 P1 C11 -11.1(2) 5_558 . . . ? O1 Ru1 P1 C11 31.8(5) . . . . ? P1 Ru1 P1 C11 178.4(2) 5_558 . . . ? C23 P1 C11 C12 -155.8(6) . . . . ? C17 P1 C11 C12 95.3(6) . . . . ? Ru1 P1 C11 C12 -25.9(6) . . . . ? C23 P1 C11 C16 32.2(6) . . . . ? C17 P1 C11 C16 -76.7(6) . . . . ? Ru1 P1 C11 C16 162.1(5) . . . . ? C16 C11 C12 C13 -1.4(11) . . . . ? P1 C11 C12 C13 -173.6(6) . . . . ? C11 C12 C13 C14 0.8(12) . . . . ? C12 C13 C14 C15 0.0(13) . . . . ? C13 C14 C15 C16 -0.1(14) . . . . ? C14 C15 C16 C11 -0.6(13) . . . . ? C12 C11 C16 C15 1.3(11) . . . . ? P1 C11 C16 C15 173.6(7) . . . . ? C23 P1 C17 C22 -31.4(7) . . . . ? C11 P1 C17 C22 73.8(6) . . . . ? Ru1 P1 C17 C22 -163.5(5) . . . . ? C23 P1 C17 C18 156.8(5) . . . . ? C11 P1 C17 C18 -97.9(6) . . . . ? Ru1 P1 C17 C18 24.7(6) . . . . ? C22 C17 C18 C19 2.5(10) . . . . ? P1 C17 C18 C19 174.5(5) . . . . ? C22 C17 C18 C3 -173.5(7) . . . . ? P1 C17 C18 C3 -1.6(9) . . . . ? N3 C3 C18 C19 171.9(7) . . . . ? N3 C3 C18 C17 -11.9(11) . . . . ? C17 C18 C19 C20 -2.1(11) . . . . ? C3 C18 C19 C20 174.6(8) . . . . ? C18 C19 C20 C21 1.3(14) . . . . ? C19 C20 C21 C22 -0.9(16) . . . . ? C20 C21 C22 C17 1.5(14) . . . . ? C18 C17 C22 C21 -2.3(12) . . . . ? P1 C17 C22 C21 -174.1(7) . . . . ? C17 P1 C23 C28 -31.3(7) . . . . ? C11 P1 C23 C28 -133.3(6) . . . . ? Ru1 P1 C23 C28 98.3(6) . . . . ? C17 P1 C23 C24 154.7(5) . . . . ? C11 P1 C23 C24 52.8(6) . . . . ? Ru1 P1 C23 C24 -75.7(5) . . . . ? C28 C23 C24 C25 -1.4(10) . . . . ? P1 C23 C24 C25 172.8(6) . . . . ? C23 C24 C25 C26 1.3(12) . . . . ? C24 C25 C26 C27 0.5(14) . . . . ? C25 C26 C27 C28 -2.3(16) . . . . ? C24 C23 C28 C27 -0.4(12) . . . . ? P1 C23 C28 C27 -174.1(7) . . . . ? C26 C27 C28 C23 2.2(14) . . . . ? Cl2 C50 Cl1 Cl1 -125.4(50) . . . 4_648 ? Cl2 C50 Cl1 Cl1 137.0(36) 4_648 . . 4_648 ? Cl1 C50 Cl1 Cl1 0.0 4_648 . . 4_648 ? Cl2 C50 Cl2 Cl2 0.000(3) 4_648 . . 4_648 ? Cl1 C50 Cl2 Cl2 -119.6(46) . . . 4_648 ? Cl1 C50 Cl2 Cl2 132.8(33) 4_648 . . 4_648 ? _refine_diff_density_max 0.894 _refine_diff_density_min -0.290 _refine_diff_density_rms 0.068 #---END data_10 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common - _chemical_formula_moiety 'C44 H35 Cl3 N2 O P2 Ru' _chemical_formula_structural 'C44 H35 Cl3 N2 O P2 Ru' _chemical_formula_analytical 'C44 H35 Cl3 N2 O P2 Ru' _chemical_formula_sum 'C44 H35 Cl3 N2 O P2 Ru' _chemical_formula_weight 877.10 _chemical_melting_point - _chemical_compound_source - 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.4070(6) _cell_length_b 15.4418(5) _cell_length_c 20.7336(9) _cell_angle_alpha 90.00 _cell_angle_beta 97.4800(10) _cell_angle_gamma 90.00 _cell_volume 4255.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 28 _cell_measurement_theta_min 12 _cell_measurement_theta_max 166 _exptl_crystal_description black _exptl_crystal_colour block _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas - _exptl_crystal_density_diffrn 1.369 _exptl_crystal_density_method - _exptl_crystal_F_000 1784 _exptl_absorpt_coefficient_mu 0.667 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min .608297 _exptl_absorpt_correction_T_max 1.000000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'SMART' _diffrn_measurement_method 'CCD' _diffrn_standards_number - _diffrn_standards_interval_count - _diffrn_standards_interval_time - _diffrn_standards_decay_% - _diffrn_reflns_number 25719 _diffrn_reflns_av_R_equivalents 0.2295 _diffrn_reflns_av_sigmaI/netI 0.3914 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 28.35 _reflns_number_total 9965 _reflns_number_observed 2799 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART' _computing_cell_refinement 'SMART/SAINT' _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXTL' _computing_structure_refinement 'SHELXTL' _computing_molecular_graphics 'SHELXTL' _computing_publication_material 'SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 50 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1721P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0042(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 9915 _refine_ls_number_parameters 506 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.3303 _refine_ls_R_factor_obs 0.1032 _refine_ls_wR_factor_all 0.3947 _refine_ls_wR_factor_obs 0.2259 _refine_ls_goodness_of_fit_all 0.926 _refine_ls_goodness_of_fit_obs 1.068 _refine_ls_restrained_S_all 0.986 _refine_ls_restrained_S_obs 1.068 _refine_ls_shift/esd_max -0.118 _refine_ls_shift/esd_mean 0.008 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ru1 Ru 0.40781(8) 0.80911(7) 0.02629(5) 0.0506(5) Uani 1 d . . Cl1 Cl 0.5037(3) 0.8744(2) -0.0558(2) 0.0633(10) Uani 1 d . . N1 N 0.3690(9) 0.7086(7) -0.0366(5) 0.057(3) Uani 1 d . . C1 C 0.4310(12) 0.6502(10) -0.0482(8) 0.071(4) Uani 1 d . . H1A H 0.4099(12) 0.6133(10) -0.0828(8) 0.086 Uiso 1 calc R . C2 C 0.5333(11) 0.6338(9) -0.0131(8) 0.066(4) Uani 1 d . . C3 C 0.5816(11) 0.6824(10) 0.0387(8) 0.068(4) Uani 1 d . . O3 O 0.5449(6) 0.7514(6) 0.0621(5) 0.060(3) Uani 1 d . . C4 C 0.6783(12) 0.6528(12) 0.0679(10) 0.090(6) Uani 1 d . . H4A H 0.7101(12) 0.6812(12) 0.1045(10) 0.108 Uiso 1 calc R . C5 C 0.7233(14) 0.5862(14) 0.0442(12) 0.110(8) Uani 1 d . . H5A H 0.7867(14) 0.5700(14) 0.0641(12) 0.131 Uiso 1 calc R . C6 C 0.6812(16) 0.5413(13) -0.0074(14) 0.125(9) Uani 1 d . . H6A H 0.7160(16) 0.4954(13) -0.0230(14) 0.150 Uiso 1 calc R . C7 C 0.5823(14) 0.5634(11) -0.0390(9) 0.088(5) Uani 1 d . . H7A H 0.5521(14) 0.5327(11) -0.0749(9) 0.106 Uiso 1 calc R . C8 C 0.2696(12) 0.7077(10) -0.0770(7) 0.066(4) Uani 1 d . . P1 P 0.2645(3) 0.8687(2) -0.0221(2) 0.0541(10) Uani 1 d . . C9 C 0.2138(11) 0.7822(9) -0.0759(7) 0.056(4) Uani 1 d . . C10 C 0.1228(11) 0.7858(10) -0.1179(7) 0.073(4) Uani 1 d . . H10A H 0.0850(11) 0.8365(10) -0.1203(7) 0.088 Uiso 1 calc R . C11 C 0.0879(15) 0.7148(13) -0.1560(7) 0.093(6) Uani 1 d . . H11A H 0.0280(15) 0.7181(13) -0.1842(7) 0.112 Uiso 1 calc R . C12 C 0.1433(15) 0.6407(13) -0.1512(9) 0.103(6) Uani 1 d . . H12A H 0.1181(15) 0.5913(13) -0.1733(9) 0.124 Uiso 1 calc R . C13 C 0.2351(14) 0.6380(11) -0.1145(8) 0.085(5) Uani 1 d . . H13A H 0.2747(14) 0.5886(11) -0.1149(8) 0.102 Uiso 1 calc R . C14 C 0.2672(10) 0.9592(10) -0.0781(7) 0.063(4) Uani 1 d . . C15 C 0.2709(14) 0.9484(12) -0.1447(9) 0.096(6) Uani 1 d . . H15A H 0.2713(14) 0.8919(12) -0.1601(9) 0.115 Uiso 1 calc R . C16 C 0.2740(18) 1.0121(16) -0.1888(11) 0.128(10) Uani 1 d . . H16A H 0.2756(18) 1.0001(16) -0.2326(11) 0.153 Uiso 1 calc R . C17 C 0.2746(14) 1.0910(21) -0.1673(13) 0.130(11) Uani 1 d . . H17A H 0.2759(14) 1.1357(21) -0.1972(13) 0.156 Uiso 1 calc R . C18 C 0.2733(13) 1.1134(10) -0.1014(14) 0.109(8) Uani 1 d . . H18A H 0.2739(13) 1.1707(10) -0.0876(14) 0.130 Uiso 1 calc R . C19 C 0.2712(11) 1.0456(10) -0.0588(10) 0.084(5) Uani 1 d . . H19A H 0.2725(11) 1.0580(10) -0.0148(10) 0.101 Uiso 1 calc R . C20 C 0.1666(11) 0.9035(9) 0.0229(7) 0.062(4) Uani 1 d . . C21 C 0.1883(11) 0.9628(10) 0.0721(8) 0.073(5) Uani 1 d . . H21A H 0.2537(11) 0.9840(10) 0.0795(8) 0.087 Uiso 1 calc R . C22 C 0.1189(16) 0.9944(13) 0.1124(9) 0.099(6) Uani 1 d . . H22A H 0.1373(16) 1.0333(13) 0.1461(9) 0.119 Uiso 1 calc R . C23 C 0.0202(17) 0.9628(15) 0.0978(10) 0.111(8) Uani 1 d . . H23A H -0.0290(17) 0.9830(15) 0.1218(10) 0.133 Uiso 1 calc R . C24 C -0.0067(15) 0.9026(13) 0.0491(10) 0.096(6) Uani 1 d . . H24A H -0.0723(15) 0.8823(13) 0.0405(10) 0.116 Uiso 1 calc R . C25 C 0.0671(12) 0.8741(11) 0.0141(8) 0.077(5) Uani 1 d . . H25A H 0.0497(12) 0.8323(11) -0.0177(8) 0.093 Uiso 1 calc R . N31 N 0.4653(8) 0.9115(6) 0.0901(5) 0.055(3) Uani 1 d . . C38 C 0.4278(10) 0.9164(9) 0.1517(7) 0.057(4) Uani 1 d . . C39 C 0.3725(10) 0.8493(9) 0.1715(6) 0.052(3) Uani 1 d . . C40 C 0.3439(10) 0.8494(10) 0.2345(8) 0.069(4) Uani 1 d . . H40A H 0.3110(10) 0.8018(10) 0.2493(8) 0.082 Uiso 1 calc R . C41 C 0.3657(13) 0.9232(11) 0.2757(7) 0.076(5) Uani 1 d . . H41A H 0.3448(13) 0.9251(11) 0.3167(7) 0.091 Uiso 1 calc R . C42 C 0.4179(12) 0.9909(11) 0.2537(8) 0.078(5) Uani 1 d . . H42A H 0.4318(12) 1.0394(11) 0.2799(8) 0.093 Uiso 1 calc R . C43 C 0.4505(10) 0.9881(10) 0.1929(7) 0.063(4) Uani 1 d . . H43A H 0.4876(10) 1.0339(10) 0.1792(7) 0.076 Uiso 1 calc R . P2 P 0.3435(3) 0.7607(2) 0.1147(2) 0.0544(10) Uani 1 d . . C44 C 0.4035(11) 0.6694(10) 0.1599(7) 0.062(4) Uani 1 d . . C45 C 0.3542(14) 0.5938(11) 0.1727(8) 0.087(5) Uani 1 d . . H45A H 0.2862(14) 0.5879(11) 0.1573(8) 0.104 Uiso 1 calc R . C46 C 0.4048(18) 0.5249(11) 0.2088(9) 0.111(7) Uani 1 d . . H46A H 0.3711(18) 0.4747(11) 0.2180(9) 0.133 Uiso 1 calc R . C47 C 0.5059(16) 0.5355(13) 0.2297(9) 0.099(6) Uani 1 d . . H47A H 0.5411(16) 0.4895(13) 0.2507(9) 0.119 Uiso 1 calc R . C48 C 0.5558(14) 0.6087(14) 0.2212(8) 0.097(6) Uani 1 d . . H48A H 0.6229(14) 0.6147(14) 0.2386(8) 0.117 Uiso 1 calc R . C49 C 0.5043(13) 0.6765(10) 0.1853(7) 0.080(5) Uani 1 d . . H49A H 0.5388(13) 0.7272(10) 0.1785(7) 0.096 Uiso 1 calc R . C50 C 0.2122(12) 0.7312(10) 0.1111(8) 0.071(4) Uani 1 d . . C51 C 0.1759(12) 0.6706(10) 0.0638(8) 0.076(5) Uani 1 d . . H51A H 0.2190(12) 0.6506(10) 0.0354(8) 0.091 Uiso 1 calc R . C52 C 0.0816(15) 0.6400(15) 0.0575(11) 0.122(8) Uani 1 d . . H52A H 0.0628(15) 0.5973(15) 0.0267(11) 0.146 Uiso 1 calc R . C53 C 0.0141(17) 0.6690(16) 0.0942(13) 0.122(9) Uani 1 d . . H53A H -0.0516(17) 0.6482(16) 0.0881(13) 0.147 Uiso 1 calc R . C54 C 0.0435(16) 0.7309(17) 0.1418(13) 0.134(9) Uani 1 d . . H54A H -0.0026(16) 0.7509(17) 0.1682(13) 0.161 Uiso 1 calc R . C55 C 0.1454(12) 0.7646(11) 0.1507(8) 0.074(5) Uani 1 d . . H55A H 0.1653(12) 0.8069(11) 0.1816(8) 0.089 Uiso 1 calc R . C60 C 0.2183(18) 0.7408(17) 0.4078(12) 0.052(7) Uani 0.50 d P . H60A H 0.1840(18) 0.7962(17) 0.4065(12) 0.063 Uiso 0.50 calc PR . H60B H 0.1900(18) 0.7037(17) 0.4386(12) 0.063 Uiso 0.50 calc PR . Cl2 Cl 0.3434(6) 0.7549(6) 0.4315(5) 0.098(3) Uani 0.50 d P . Cl3 Cl 0.2006(8) 0.6921(8) 0.3287(4) 0.126(4) Uani 0.50 d P . C70 C 0.5790(35) 0.2170(23) 0.2075(15) 0.117(15) Uani 0.50 d P . H70A H 0.5174(35) 0.1833(23) 0.2020(15) 0.140 Uiso 0.50 calc PR . H70B H 0.6102(35) 0.2102(23) 0.1682(15) 0.140 Uiso 0.50 calc PR . Cl4 Cl 0.6576(8) 0.1738(8) 0.2706(5) 0.128(4) Uani 0.50 d P . Cl5 Cl 0.5485(12) 0.3205(7) 0.2142(5) 0.142(5) Uani 0.50 d P . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0369(6) 0.0632(8) 0.0473(7) 0.0013(6) -0.0110(5) 0.0013(6) Cl1 0.056(2) 0.077(2) 0.055(2) 0.003(2) 0.002(2) -0.004(2) N1 0.067(8) 0.050(7) 0.053(8) 0.004(6) -0.001(6) 0.011(6) C1 0.072(12) 0.074(10) 0.067(11) 0.001(9) 0.006(9) -0.008(10) C2 0.050(9) 0.058(9) 0.088(12) -0.011(9) 0.001(9) -0.003(8) C3 0.052(9) 0.074(11) 0.076(11) -0.007(9) 0.004(8) 0.001(9) O3 0.039(5) 0.066(6) 0.073(7) 0.005(5) -0.005(5) 0.007(5) C4 0.056(11) 0.084(12) 0.126(16) 0.006(11) -0.010(11) 0.029(10) C5 0.053(11) 0.087(14) 0.175(23) -0.002(14) -0.038(13) 0.001(11) C6 0.072(15) 0.084(15) 0.227(29) 0.011(16) 0.044(18) 0.025(12) C7 0.083(14) 0.074(11) 0.103(15) -0.007(10) -0.001(12) -0.002(10) C8 0.059(10) 0.079(11) 0.052(9) -0.005(8) -0.017(7) -0.014(9) P1 0.038(2) 0.068(2) 0.051(2) 0.008(2) -0.014(2) 0.001(2) C9 0.051(9) 0.065(10) 0.051(9) 0.003(7) -0.001(7) -0.006(8) C10 0.053(9) 0.087(11) 0.069(10) 0.000(9) -0.030(8) -0.003(8) C11 0.092(14) 0.123(15) 0.050(10) 0.005(10) -0.042(9) -0.036(12) C12 0.089(14) 0.093(14) 0.112(16) -0.013(12) -0.044(12) -0.015(12) C13 0.097(14) 0.078(11) 0.073(12) -0.027(10) -0.011(10) -0.012(11) C14 0.038(8) 0.086(12) 0.058(10) 0.022(9) -0.018(7) -0.011(8) C15 0.111(15) 0.092(13) 0.078(14) 0.009(11) -0.013(11) -0.038(11) C16 0.168(23) 0.113(17) 0.085(16) 0.023(16) -0.047(14) -0.068(17) C17 0.054(12) 0.206(30) 0.119(21) 0.102(21) -0.027(13) -0.017(15) C18 0.082(14) 0.037(9) 0.205(25) 0.046(14) 0.010(16) 0.002(9) C19 0.051(10) 0.067(11) 0.131(16) 0.012(11) -0.005(10) -0.006(9) C20 0.048(9) 0.072(10) 0.060(10) 0.004(8) -0.011(8) 0.017(8) C21 0.042(9) 0.100(13) 0.072(11) 0.026(10) -0.008(9) 0.027(9) C22 0.082(14) 0.140(17) 0.074(13) 0.013(11) 0.006(12) 0.043(13) C23 0.097(17) 0.174(22) 0.067(14) 0.042(14) 0.029(13) 0.080(16) C24 0.082(14) 0.129(16) 0.083(14) 0.022(12) 0.029(13) 0.029(12) C25 0.052(10) 0.101(12) 0.076(12) 0.010(10) -0.001(9) 0.022(10) N31 0.060(7) 0.056(7) 0.044(7) -0.009(5) -0.010(6) -0.003(6) C38 0.046(8) 0.065(9) 0.053(10) 0.001(8) -0.015(7) -0.008(8) C39 0.043(8) 0.071(9) 0.039(9) 0.005(7) -0.009(7) 0.012(7) C40 0.046(9) 0.083(11) 0.072(12) 0.015(9) -0.008(8) -0.001(8) C41 0.088(13) 0.092(12) 0.044(9) 0.003(9) -0.004(9) -0.012(11) C42 0.081(12) 0.081(12) 0.064(11) -0.020(9) -0.016(9) -0.005(10) C43 0.057(10) 0.085(11) 0.044(9) 0.000(8) -0.007(7) -0.009(8) P2 0.040(2) 0.065(2) 0.054(2) 0.006(2) -0.011(2) 0.000(2) C44 0.061(10) 0.073(10) 0.047(9) 0.010(7) -0.013(7) -0.004(8) C45 0.079(13) 0.094(13) 0.080(12) 0.017(10) -0.014(10) 0.016(11) C46 0.141(20) 0.074(12) 0.110(16) 0.025(11) -0.015(15) -0.017(14) C47 0.102(16) 0.096(15) 0.089(14) 0.041(11) -0.026(12) 0.007(13) C48 0.078(13) 0.120(16) 0.083(13) 0.021(12) -0.034(10) 0.011(12) C49 0.078(12) 0.087(12) 0.066(11) 0.020(9) -0.022(9) 0.004(10) C50 0.067(11) 0.067(10) 0.076(12) 0.025(9) -0.007(10) -0.008(9) C51 0.051(10) 0.087(12) 0.085(12) 0.009(10) -0.007(9) -0.019(9) C52 0.058(13) 0.157(20) 0.139(20) 0.050(16) -0.028(13) -0.048(14) C53 0.052(13) 0.153(21) 0.153(23) 0.025(17) -0.022(14) -0.036(14) C54 0.068(15) 0.187(25) 0.144(22) 0.082(19) 0.006(15) 0.003(15) C55 0.049(10) 0.108(13) 0.067(11) 0.016(9) 0.012(9) 0.013(10) C60 0.036(15) 0.067(17) 0.051(17) -0.006(14) -0.006(13) -0.017(14) Cl2 0.045(5) 0.132(8) 0.113(8) -0.006(6) -0.013(5) 0.013(5) Cl3 0.113(8) 0.204(11) 0.063(6) 0.002(7) 0.016(6) -0.093(8) C70 0.180(44) 0.118(30) 0.042(20) -0.039(19) -0.025(23) 0.042(28) Cl4 0.095(7) 0.215(12) 0.069(6) -0.031(7) -0.002(5) 0.046(8) Cl5 0.223(15) 0.111(8) 0.092(8) 0.005(7) 0.017(9) -0.007(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N1 2.050(11) . ? Ru1 O3 2.090(9) . ? Ru1 N31 2.140(10) . ? Ru1 P1 2.245(4) . ? Ru1 P2 2.253(4) . ? Ru1 Cl1 2.478(4) . ? N1 C1 1.27(2) . ? N1 C8 1.48(2) . ? C1 C2 1.49(2) . ? C2 C3 1.40(2) . ? C2 C7 1.41(2) . ? C3 O3 1.29(2) . ? C3 C4 1.43(2) . ? C4 C5 1.32(2) . ? C5 C6 1.34(3) . ? C6 C7 1.44(3) . ? C8 C9 1.38(2) . ? C8 C13 1.37(2) . ? P1 C20 1.789(15) . ? P1 C9 1.815(14) . ? P1 C14 1.821(14) . ? C9 C10 1.41(2) . ? C10 C11 1.40(2) . ? C11 C12 1.36(2) . ? C12 C13 1.36(2) . ? C14 C19 1.39(2) . ? C14 C15 1.40(2) . ? C15 C16 1.35(2) . ? C16 C17 1.30(3) . ? C17 C18 1.41(3) . ? C18 C19 1.37(2) . ? C20 C25 1.40(2) . ? C20 C21 1.37(2) . ? C21 C22 1.41(2) . ? C22 C23 1.41(3) . ? C23 C24 1.38(3) . ? C24 C25 1.37(2) . ? N31 C38 1.44(2) . ? C38 C39 1.37(2) . ? C38 C43 1.41(2) . ? C39 C40 1.41(2) . ? C39 P2 1.814(14) . ? C40 C41 1.43(2) . ? C41 C42 1.37(2) . ? C42 C43 1.39(2) . ? P2 C50 1.81(2) . ? P2 C44 1.820(15) . ? C44 C45 1.38(2) . ? C44 C49 1.39(2) . ? C45 C46 1.42(2) . ? C46 C47 1.38(3) . ? C47 C48 1.34(2) . ? C48 C49 1.41(2) . ? C50 C55 1.39(2) . ? C50 C51 1.40(2) . ? C51 C52 1.34(2) . ? C52 C53 1.33(3) . ? C53 C54 1.39(3) . ? C54 C55 1.45(3) . ? C60 Cl2 1.70(2) . ? C60 Cl3 1.79(3) . ? C70 Cl4 1.71(4) . ? C70 Cl5 1.66(3) . ? 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 N1 Ru1 O3 92.4(4) . . ? N1 Ru1 N31 173.6(5) . . ? O3 Ru1 N31 82.3(4) . . ? N1 Ru1 P1 84.0(4) . . ? O3 Ru1 P1 174.4(3) . . ? N31 Ru1 P1 101.0(3) . . ? N1 Ru1 P2 100.0(3) . . ? O3 Ru1 P2 88.9(3) . . ? N31 Ru1 P2 83.5(3) . . ? P1 Ru1 P2 95.96(13) . . ? N1 Ru1 Cl1 89.0(3) . . ? O3 Ru1 Cl1 84.7(3) . . ? N31 Ru1 Cl1 86.9(3) . . ? P1 Ru1 Cl1 90.95(13) . . ? P2 Ru1 Cl1 169.15(13) . . ? C1 N1 C8 116.6(13) . . ? C1 N1 Ru1 122.7(11) . . ? C8 N1 Ru1 120.3(9) . . ? N1 C1 C2 127.7(15) . . ? C3 C2 C7 120.9(15) . . ? C3 C2 C1 126.2(14) . . ? C7 C2 C1 112.9(15) . . ? O3 C3 C2 124.7(14) . . ? O3 C3 C4 118.1(15) . . ? C2 C3 C4 117.2(15) . . ? C3 O3 Ru1 125.3(9) . . ? C5 C4 C3 121.6(18) . . ? C4 C5 C6 122.4(19) . . ? C5 C6 C7 120.6(18) . . ? C6 C7 C2 117.1(17) . . ? C9 C8 C13 121.5(15) . . ? C9 C8 N1 115.7(13) . . ? C13 C8 N1 122.8(15) . . ? C20 P1 C9 107.5(7) . . ? C20 P1 C14 100.3(7) . . ? C9 P1 C14 102.0(7) . . ? C20 P1 Ru1 122.3(5) . . ? C9 P1 Ru1 101.7(5) . . ? C14 P1 Ru1 120.8(4) . . ? C8 C9 C10 117.0(13) . . ? C8 C9 P1 117.7(11) . . ? C10 C9 P1 125.3(12) . . ? C11 C10 C9 121.3(15) . . ? C12 C11 C10 118.6(16) . . ? C11 C12 C13 120.8(17) . . ? C12 C13 C8 120.4(17) . . ? C19 C14 C15 113.1(15) . . ? C19 C14 P1 123.7(13) . . ? C15 C14 P1 123.1(14) . . ? C16 C15 C14 126.3(19) . . ? C17 C16 C15 116.9(23) . . ? C16 C17 C18 124.2(22) . . ? C19 C18 C17 116.1(19) . . ? C18 C19 C14 123.3(19) . . ? C25 C20 C21 114.8(14) . . ? C25 C20 P1 126.0(13) . . ? C21 C20 P1 119.2(12) . . ? C20 C21 C22 125.2(16) . . ? C23 C22 C21 115.2(19) . . ? C24 C23 C22 122.5(18) . . ? C23 C24 C25 117.6(20) . . ? C20 C25 C24 124.6(17) . . ? C38 N31 Ru1 116.8(8) . . ? C39 C38 C43 119.9(13) . . ? C39 C38 N31 119.5(13) . . ? C43 C38 N31 120.6(13) . . ? C38 C39 C40 120.0(14) . . ? C38 C39 P2 117.2(11) . . ? C40 C39 P2 122.7(12) . . ? C39 C40 C41 119.7(14) . . ? C42 C41 C40 118.8(14) . . ? C41 C42 C43 120.9(15) . . ? C42 C43 C38 120.5(14) . . ? C50 P2 C44 100.9(7) . . ? C50 P2 C39 110.0(7) . . ? C44 P2 C39 102.0(6) . . ? C50 P2 Ru1 121.5(5) . . ? C44 P2 Ru1 119.0(5) . . ? C39 P2 Ru1 101.8(5) . . ? C45 C44 C49 117.3(14) . . ? C45 C44 P2 124.2(12) . . ? C49 C44 P2 118.5(12) . . ? C44 C45 C46 121.7(17) . . ? C47 C46 C45 117.4(17) . . ? C48 C47 C46 123.2(18) . . ? C47 C48 C49 118.5(17) . . ? C44 C49 C48 121.7(16) . . ? C55 C50 C51 118.1(15) . . ? C55 C50 P2 125.5(14) . . ? C51 C50 P2 116.4(13) . . ? C52 C51 C50 122.8(19) . . ? C51 C52 C53 122.0(23) . . ? C52 C53 C54 118.9(21) . . ? C53 C54 C55 120.7(22) . . ? C50 C55 C54 117.5(19) . . ? Cl2 C60 Cl3 109.1(14) . . ? Cl4 C70 Cl5 116.5(19) . . ? _refine_diff_density_max 1.082 _refine_diff_density_min -1.546 _refine_diff_density_rms 0.146 #---END data_11 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common - _chemical_formula_moiety 'C28 H26 Cl5 N O2 P Ru S' _chemical_formula_structural 'C28 H26 Cl5 N O2 P Ru S' _chemical_formula_analytical 'C28 H26 Cl5 N O2 P Ru S' _chemical_formula_sum 'C28 H26 Cl5 N O2 P Ru S' _chemical_formula_weight 749.85 _chemical_melting_point - _chemical_compound_source - 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7225(2) _cell_length_b 10.4699(2) _cell_length_c 16.2582(4) _cell_angle_alpha 107.8590(10) _cell_angle_beta 90.1360(10) _cell_angle_gamma 98.5150(10) _cell_volume 1555.86(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 34 _cell_measurement_theta_min 12 _cell_measurement_theta_max 166 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max .1 _exptl_crystal_size_mid .1 _exptl_crystal_size_min .15 _exptl_crystal_density_meas - _exptl_crystal_density_diffrn 1.601 _exptl_crystal_density_method - _exptl_crystal_F_000 754 _exptl_absorpt_coefficient_mu 1.079 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.600600 _exptl_absorpt_correction_T_max 1.00000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device SMART _diffrn_measurement_method CCD _diffrn_standards_number - _diffrn_standards_interval_count - _diffrn_standards_interval_time - _diffrn_standards_decay_% - _diffrn_reflns_number 7899 _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_av_sigmaI/netI 0.0776 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 23.26 _reflns_number_total 4406 _reflns_number_observed 3248 _reflns_observed_criterion >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART/SAINT _computing_data_reduction SAINT _computing_structure_solution SHELXTL _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement on F^2^ for ALL reflections except for 51 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0592P)^2^+7.0747P] 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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0004(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4355 _refine_ls_number_parameters 353 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1034 _refine_ls_R_factor_obs 0.0685 _refine_ls_wR_factor_all 0.1843 _refine_ls_wR_factor_obs 0.1522 _refine_ls_goodness_of_fit_all 1.093 _refine_ls_goodness_of_fit_obs 1.161 _refine_ls_restrained_S_all 1.199 _refine_ls_restrained_S_obs 1.161 _refine_ls_shift/esd_max -0.083 _refine_ls_shift/esd_mean 0.002 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ru1 Ru 0.61255(7) 0.52485(8) 0.72671(4) 0.0372(3) Uani 1 d . . Cl1 Cl 0.3787(2) 0.5484(3) 0.6844(2) 0.0558(7) Uani 1 d . . Cl2 Cl 0.6644(3) 0.7648(3) 0.7714(2) 0.0544(6) Uani 1 d . . P1 P 0.8462(2) 0.5269(3) 0.75695(14) 0.0406(6) Uani 1 d . . C1 C 0.9393(9) 0.6174(10) 0.8606(6) 0.048(2) Uani 1 d . . C2 C 1.0347(10) 0.5592(12) 0.8934(6) 0.062(3) Uani 1 d . . H2A H 1.0538(10) 0.4737(12) 0.8622(6) 0.074 Uiso 1 calc R . C3 C 1.1038(12) 0.6295(14) 0.9745(7) 0.076(3) Uani 1 d . . H3A H 1.1694(12) 0.5902(14) 0.9961(7) 0.092 Uiso 1 calc R . C4 C 1.0768(14) 0.7508(16) 1.0207(8) 0.088(4) Uani 1 d . . H4A H 1.1259(14) 0.7979(16) 1.0729(8) 0.106 Uiso 1 calc R . C5 C 0.9760(18) 0.8059(16) 0.9907(9) 0.123(6) Uani 1 d . . H5A H 0.9521(18) 0.8879(16) 1.0247(9) 0.147 Uiso 1 calc R . C6 C 0.9092(15) 0.7405(14) 0.9102(8) 0.103(5) Uani 1 d . . H6A H 0.8432(15) 0.7807(14) 0.8896(8) 0.123 Uiso 1 calc R . C7 C 0.8993(9) 0.3604(9) 0.7269(5) 0.043(2) Uani 1 d . . C8 C 0.8203(10) 0.2587(10) 0.7534(6) 0.055(3) Uani 1 d . . H8A H 0.7403(10) 0.2759(10) 0.7834(6) 0.066 Uiso 1 calc R . C9 C 0.8616(12) 0.1315(11) 0.7348(7) 0.067(3) Uani 1 d . . H9A H 0.8113(12) 0.0649(11) 0.7545(7) 0.081 Uiso 1 calc R . C10 C 0.9749(15) 0.1045(14) 0.6881(8) 0.083(4) Uani 1 d . . H10A H 1.0004(15) 0.0184(14) 0.6735(8) 0.100 Uiso 1 calc R . C11 C 1.0512(14) 0.2046(16) 0.6627(8) 0.093(4) Uani 1 d . . H11A H 1.1298(14) 0.1857(16) 0.6315(8) 0.111 Uiso 1 calc R . C12 C 1.0166(11) 0.3306(12) 0.6812(7) 0.065(3) Uani 1 d . . H12A H 1.0714(11) 0.3969(12) 0.6634(7) 0.078 Uiso 1 calc R . C13 C 0.9212(9) 0.6071(9) 0.6783(6) 0.043(2) Uani 1 d . . C14 C 0.8293(8) 0.5906(9) 0.6067(5) 0.040(2) Uani 1 d . . C15 C 0.8705(10) 0.6448(10) 0.5422(5) 0.052(3) Uani 1 d . . H15A H 0.8093(10) 0.6360(10) 0.4961(5) 0.062 Uiso 1 calc R . C16 C 1.0066(11) 0.7137(11) 0.5475(7) 0.062(3) Uani 1 d . . H16A H 1.0367(11) 0.7506(11) 0.5042(7) 0.074 Uiso 1 calc R . C17 C 1.0951(11) 0.7268(11) 0.6155(6) 0.061(3) Uani 1 d . . H17A H 1.1852(11) 0.7729(11) 0.6178(6) 0.073 Uiso 1 calc R . N19 N 0.6936(7) 0.5132(7) 0.6077(4) 0.040(2) Uani 1 d . . C20 C 0.6409(9) 0.4229(10) 0.5358(6) 0.045(2) Uani 1 d . . H20A H 0.6768(9) 0.4301(10) 0.4842(6) 0.054 Uiso 1 calc R . C21 C 0.5312(9) 0.3133(10) 0.5315(5) 0.045(2) Uani 1 d . . O22 O 0.5536(6) 0.3273(6) 0.6831(4) 0.047(2) Uani 1 d . . C22 C 0.4995(9) 0.2656(9) 0.6030(6) 0.044(2) Uani 1 d . . C23 C 0.4086(11) 0.1439(11) 0.5887(7) 0.061(3) Uani 1 d . . H23A H 0.3896(11) 0.1090(11) 0.6343(7) 0.073 Uiso 1 calc R . C24 C 0.3460(11) 0.0741(11) 0.5073(8) 0.072(3) Uani 1 d . . H24A H 0.2821(11) -0.0044(11) 0.5000(8) 0.086 Uiso 1 calc R . C25 C 0.3770(11) 0.1194(12) 0.4363(7) 0.065(3) Uani 1 d . . H25A H 0.3356(11) 0.0714(12) 0.3818(7) 0.078 Uiso 1 calc R . C26 C 0.4692(10) 0.2356(11) 0.4488(6) 0.056(3) Uani 1 d . . H26A H 0.4924(10) 0.2651(11) 0.4015(6) 0.068 Uiso 1 calc R . S1 S 0.5388(2) 0.5099(3) 0.85897(14) 0.0459(6) Uani 1 d . . O1 O 0.6345(7) 0.4625(8) 0.9099(4) 0.063(2) Uani 1 d . . C27 C 0.3754(11) 0.3981(12) 0.8449(7) 0.068(3) Uani 1 d . . H27A H 0.3866(11) 0.3090(12) 0.8087(7) 0.101 Uiso 1 calc R . H27B H 0.3070(11) 0.4320(12) 0.8181(7) 0.101 Uiso 1 calc R . H27C H 0.3453(11) 0.3935(12) 0.9002(7) 0.101 Uiso 1 calc R . C18 C 1.0547(9) 0.6735(10) 0.6810(6) 0.053(3) Uani 1 d . . H18A H 1.1173(9) 0.6824(10) 0.7266(6) 0.063 Uiso 1 calc R . C28 C 0.4901(15) 0.6633(12) 0.9264(7) 0.089(4) Uani 1 d . . H28A H 0.5696(15) 0.7339(12) 0.9396(7) 0.133 Uiso 1 calc R . H28B H 0.4562(15) 0.6501(12) 0.9791(7) 0.133 Uiso 1 calc R . H28C H 0.4182(15) 0.6889(12) 0.8969(7) 0.133 Uiso 1 calc R . C30 C 0.6012(16) 1.0363(14) 1.1661(9) 0.100(4) Uani 1 d . . H30A H 0.5729(16) 1.1218(14) 1.2011(9) 0.120 Uiso 1 calc R . Cl3 Cl 0.4641(5) 0.9072(5) 1.1385(4) 0.171(2) Uani 1 d . . Cl4 Cl 0.7341(8) 0.9887(6) 1.2211(4) 0.216(3) Uani 1 d . . Cl5 Cl 0.6803(7) 1.0527(7) 1.0744(5) 0.211(3) Uani 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 0.0281(4) 0.0534(5) 0.0332(4) 0.0152(4) -0.0001(3) 0.0122(3) Cl1 0.0376(13) 0.086(2) 0.0564(15) 0.0334(14) 0.0020(11) 0.0235(13) Cl2 0.061(2) 0.054(2) 0.0508(14) 0.0180(12) 0.0017(12) 0.0157(12) P1 0.0339(13) 0.056(2) 0.0345(13) 0.0155(12) -0.0033(10) 0.0100(11) C1 0.043(6) 0.064(7) 0.035(5) 0.019(5) -0.006(4) 0.001(5) C2 0.059(7) 0.085(8) 0.043(6) 0.016(6) -0.008(5) 0.023(6) C3 0.064(8) 0.101(10) 0.060(7) 0.024(7) -0.030(6) 0.004(7) C4 0.086(10) 0.117(12) 0.047(7) 0.014(8) -0.029(6) -0.006(9) C5 0.157(15) 0.106(12) 0.080(10) -0.023(9) -0.039(10) 0.052(11) C6 0.130(12) 0.088(10) 0.073(9) -0.010(8) -0.057(8) 0.040(9) C7 0.034(5) 0.056(6) 0.035(5) 0.009(5) -0.008(4) 0.010(5) C8 0.044(6) 0.054(7) 0.063(6) 0.013(5) -0.010(5) 0.010(5) C9 0.071(8) 0.056(7) 0.074(8) 0.019(6) -0.021(6) 0.009(6) C10 0.093(10) 0.085(10) 0.069(8) 0.002(7) -0.007(7) 0.053(9) C11 0.080(10) 0.123(13) 0.085(9) 0.025(9) 0.021(7) 0.064(10) C12 0.053(7) 0.084(8) 0.067(7) 0.028(6) 0.015(5) 0.031(6) C13 0.037(5) 0.050(6) 0.043(5) 0.013(5) 0.004(4) 0.011(4) C14 0.029(5) 0.055(6) 0.037(5) 0.014(4) 0.001(4) 0.011(4) C15 0.061(7) 0.069(7) 0.031(5) 0.020(5) 0.005(4) 0.017(6) C16 0.055(7) 0.077(8) 0.059(7) 0.030(6) 0.018(5) 0.010(6) C17 0.047(6) 0.074(8) 0.055(6) 0.015(6) 0.007(5) 0.001(5) N19 0.039(4) 0.054(5) 0.029(4) 0.013(4) -0.002(3) 0.018(4) C20 0.037(5) 0.065(7) 0.035(5) 0.017(5) -0.002(4) 0.016(5) C21 0.031(5) 0.062(6) 0.039(5) 0.011(5) -0.006(4) 0.011(5) O22 0.047(4) 0.057(4) 0.039(4) 0.016(3) -0.001(3) 0.015(3) C22 0.034(5) 0.046(6) 0.052(6) 0.013(5) 0.000(4) 0.013(4) C23 0.056(7) 0.069(7) 0.057(7) 0.017(6) 0.004(5) 0.016(6) C24 0.045(7) 0.059(7) 0.092(9) -0.001(7) -0.009(6) 0.001(5) C25 0.045(6) 0.078(8) 0.059(7) 0.006(6) -0.015(5) 0.002(6) C26 0.052(6) 0.076(8) 0.044(6) 0.015(6) -0.002(5) 0.023(6) S1 0.0486(15) 0.058(2) 0.0370(12) 0.0185(12) 0.0069(10) 0.0198(12) O1 0.054(4) 0.104(6) 0.050(4) 0.045(4) 0.000(3) 0.021(4) C27 0.061(7) 0.088(8) 0.061(7) 0.038(6) 0.011(5) 0.003(6) C18 0.037(6) 0.067(7) 0.047(6) 0.015(5) -0.012(4) -0.006(5) C28 0.141(12) 0.075(8) 0.058(7) 0.019(6) 0.045(7) 0.045(8) C30 0.122(12) 0.075(9) 0.103(11) 0.033(8) 0.005(9) 0.011(8) Cl3 0.104(4) 0.122(4) 0.250(6) 0.007(4) 0.023(4) 0.014(3) Cl4 0.265(8) 0.169(5) 0.204(6) 0.084(5) -0.130(6) -0.050(5) Cl5 0.232(7) 0.251(7) 0.250(7) 0.179(6) 0.131(6) 0.131(6) _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 O22 1.964(6) . ? Ru1 N19 2.066(7) . ? Ru1 S1 2.311(2) . ? Ru1 P1 2.318(2) . ? Ru1 Cl2 2.366(3) . ? Ru1 Cl1 2.443(2) . ? P1 C7 1.813(9) . ? P1 C1 1.821(9) . ? P1 C13 1.831(9) . ? C1 C2 1.371(12) . ? C1 C6 1.369(15) . ? C2 C3 1.409(14) . ? C3 C4 1.33(2) . ? C4 C5 1.37(2) . ? C5 C6 1.39(2) . ? C7 C12 1.384(13) . ? C7 C8 1.396(13) . ? C8 C9 1.393(13) . ? C9 C10 1.35(2) . ? C10 C11 1.36(2) . ? C11 C12 1.35(2) . ? C13 C18 1.372(12) . ? C13 C14 1.418(11) . ? C14 C15 1.371(11) . ? C14 N19 1.445(11) . ? C15 C16 1.399(13) . ? C16 C17 1.359(13) . ? C17 C18 1.380(13) . ? N19 C20 1.304(11) . ? C20 C21 1.431(12) . ? C21 C22 1.417(12) . ? C21 C26 1.419(12) . ? O22 C22 1.330(10) . ? C22 C23 1.394(13) . ? C23 C24 1.387(14) . ? C24 C25 1.395(15) . ? C25 C26 1.360(14) . ? S1 O1 1.478(6) . ? S1 C28 1.775(11) . ? S1 C27 1.798(11) . ? C30 Cl5 1.722(14) . ? C30 Cl3 1.702(15) . ? C30 Cl4 1.782(15) . ? 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 O22 Ru1 N19 87.9(3) . . ? O22 Ru1 S1 86.1(2) . . ? N19 Ru1 S1 171.2(2) . . ? O22 Ru1 P1 98.5(2) . . ? N19 Ru1 P1 79.0(2) . . ? S1 Ru1 P1 95.57(8) . . ? O22 Ru1 Cl2 174.4(2) . . ? N19 Ru1 Cl2 91.0(2) . . ? S1 Ru1 Cl2 95.61(9) . . ? P1 Ru1 Cl2 86.65(9) . . ? O22 Ru1 Cl1 87.4(2) . . ? N19 Ru1 Cl1 95.1(2) . . ? S1 Ru1 Cl1 90.99(8) . . ? P1 Ru1 Cl1 171.42(9) . . ? Cl2 Ru1 Cl1 87.22(9) . . ? C7 P1 C1 104.1(4) . . ? C7 P1 C13 105.6(4) . . ? C1 P1 C13 107.0(4) . . ? C7 P1 Ru1 114.6(3) . . ? C1 P1 Ru1 125.0(3) . . ? C13 P1 Ru1 98.8(3) . . ? C2 C1 C6 118.4(9) . . ? C2 C1 P1 120.5(8) . . ? C6 C1 P1 120.9(7) . . ? C1 C2 C3 119.8(11) . . ? C4 C3 C2 121.2(11) . . ? C3 C4 C5 119.4(12) . . ? C4 C5 C6 120.5(13) . . ? C1 C6 C5 120.6(11) . . ? C12 C7 C8 118.5(9) . . ? C12 C7 P1 123.2(8) . . ? C8 C7 P1 118.3(7) . . ? C9 C8 C7 119.9(10) . . ? C10 C9 C8 120.2(12) . . ? C9 C10 C11 119.4(12) . . ? C12 C11 C10 122.2(12) . . ? C11 C12 C7 119.8(11) . . ? C18 C13 C14 119.3(8) . . ? C18 C13 P1 126.7(7) . . ? C14 C13 P1 113.9(7) . . ? C15 C14 C13 120.8(8) . . ? C15 C14 N19 124.2(7) . . ? C13 C14 N19 115.0(7) . . ? C14 C15 C16 118.5(9) . . ? C17 C16 C15 120.4(9) . . ? C16 C17 C18 121.7(10) . . ? C20 N19 C14 118.1(7) . . ? C20 N19 Ru1 123.1(6) . . ? C14 N19 Ru1 117.7(5) . . ? N19 C20 C21 124.0(8) . . ? C22 C21 C26 118.8(9) . . ? C22 C21 C20 122.5(8) . . ? C26 C21 C20 117.7(8) . . ? C22 O22 Ru1 121.8(5) . . ? O22 C22 C23 117.3(8) . . ? O22 C22 C21 124.4(8) . . ? C23 C22 C21 118.3(9) . . ? C24 C23 C22 120.9(10) . . ? C23 C24 C25 121.3(11) . . ? C26 C25 C24 118.3(10) . . ? C25 C26 C21 122.3(9) . . ? O1 S1 C28 108.4(5) . . ? O1 S1 C27 107.0(5) . . ? C28 S1 C27 100.3(6) . . ? O1 S1 Ru1 116.5(3) . . ? C28 S1 Ru1 113.0(4) . . ? C27 S1 Ru1 110.2(3) . . ? C13 C18 C17 119.3(9) . . ? Cl5 C30 Cl3 109.9(9) . . ? Cl5 C30 Cl4 102.7(8) . . ? Cl3 C30 Cl4 108.9(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O22 Ru1 P1 C7 3.6(4) . . . . ? N19 Ru1 P1 C7 -82.6(4) . . . . ? S1 Ru1 P1 C7 90.5(3) . . . . ? Cl2 Ru1 P1 C7 -174.2(3) . . . . ? Cl1 Ru1 P1 C7 -129.7(7) . . . . ? O22 Ru1 P1 C1 -126.7(4) . . . . ? N19 Ru1 P1 C1 147.1(4) . . . . ? S1 Ru1 P1 C1 -39.8(4) . . . . ? Cl2 Ru1 P1 C1 55.5(4) . . . . ? Cl1 Ru1 P1 C1 100.0(7) . . . . ? O22 Ru1 P1 C13 115.3(3) . . . . ? N19 Ru1 P1 C13 29.1(4) . . . . ? S1 Ru1 P1 C13 -157.8(3) . . . . ? Cl2 Ru1 P1 C13 -62.5(3) . . . . ? Cl1 Ru1 P1 C13 -18.0(7) . . . . ? C7 P1 C1 C2 5.6(9) . . . . ? C13 P1 C1 C2 -105.9(8) . . . . ? Ru1 P1 C1 C2 139.9(7) . . . . ? C7 P1 C1 C6 -169.9(10) . . . . ? C13 P1 C1 C6 78.6(11) . . . . ? Ru1 P1 C1 C6 -35.6(11) . . . . ? C6 C1 C2 C3 -3.0(17) . . . . ? P1 C1 C2 C3 -178.7(8) . . . . ? C1 C2 C3 C4 1.0(18) . . . . ? C2 C3 C4 C5 2.8(21) . . . . ? C3 C4 C5 C6 -4.5(25) . . . . ? C2 C1 C6 C5 1.4(21) . . . . ? P1 C1 C6 C5 177.0(12) . . . . ? C4 C5 C6 C1 2.4(26) . . . . ? C1 P1 C7 C12 -87.8(8) . . . . ? C13 P1 C7 C12 24.7(9) . . . . ? Ru1 P1 C7 C12 132.3(7) . . . . ? C1 P1 C7 C8 90.2(7) . . . . ? C13 P1 C7 C8 -157.3(7) . . . . ? Ru1 P1 C7 C8 -49.7(7) . . . . ? C12 C7 C8 C9 1.0(13) . . . . ? P1 C7 C8 C9 -177.1(7) . . . . ? C7 C8 C9 C10 -2.7(15) . . . . ? C8 C9 C10 C11 2.7(17) . . . . ? C9 C10 C11 C12 -1.1(20) . . . . ? C10 C11 C12 C7 -0.6(19) . . . . ? C8 C7 C12 C11 0.6(15) . . . . ? P1 C7 C12 C11 178.6(9) . . . . ? C7 P1 C13 C18 -82.6(9) . . . . ? C1 P1 C13 C18 27.9(10) . . . . ? Ru1 P1 C13 C18 158.7(8) . . . . ? C7 P1 C13 C14 94.5(7) . . . . ? C1 P1 C13 C14 -155.1(7) . . . . ? Ru1 P1 C13 C14 -24.2(7) . . . . ? C18 C13 C14 C15 -2.7(13) . . . . ? P1 C13 C14 C15 -179.9(7) . . . . ? C18 C13 C14 N19 176.9(8) . . . . ? P1 C13 C14 N19 -0.4(10) . . . . ? C13 C14 C15 C16 1.7(14) . . . . ? N19 C14 C15 C16 -177.8(8) . . . . ? C14 C15 C16 C17 -0.4(15) . . . . ? C15 C16 C17 C18 0.0(16) . . . . ? C15 C14 N19 C20 42.9(12) . . . . ? C13 C14 N19 C20 -136.6(8) . . . . ? C15 C14 N19 Ru1 -148.8(7) . . . . ? C13 C14 N19 Ru1 31.7(9) . . . . ? O22 Ru1 N19 C20 30.9(6) . . . . ? S1 Ru1 N19 C20 77.8(16) . . . . ? P1 Ru1 N19 C20 130.0(6) . . . . ? Cl2 Ru1 N19 C20 -143.6(6) . . . . ? Cl1 Ru1 N19 C20 -56.3(6) . . . . ? O22 Ru1 N19 C14 -136.7(6) . . . . ? S1 Ru1 N19 C14 -89.8(16) . . . . ? P1 Ru1 N19 C14 -37.6(5) . . . . ? Cl2 Ru1 N19 C14 48.8(5) . . . . ? Cl1 Ru1 N19 C14 136.1(5) . . . . ? C14 N19 C20 C21 160.7(7) . . . . ? Ru1 N19 C20 C21 -6.8(11) . . . . ? N19 C20 C21 C22 -20.9(13) . . . . ? N19 C20 C21 C26 170.3(8) . . . . ? N19 Ru1 O22 C22 -40.9(6) . . . . ? S1 Ru1 O22 C22 145.5(6) . . . . ? P1 Ru1 O22 C22 -119.5(6) . . . . ? Cl2 Ru1 O22 C22 37.5(22) . . . . ? Cl1 Ru1 O22 C22 54.3(6) . . . . ? Ru1 O22 C22 C23 -152.9(6) . . . . ? Ru1 O22 C22 C21 28.9(11) . . . . ? C26 C21 C22 O22 178.2(8) . . . . ? C20 C21 C22 O22 9.5(13) . . . . ? C26 C21 C22 C23 0.0(12) . . . . ? C20 C21 C22 C23 -168.6(8) . . . . ? O22 C22 C23 C24 179.0(8) . . . . ? C21 C22 C23 C24 -2.7(14) . . . . ? C22 C23 C24 C25 3.2(16) . . . . ? C23 C24 C25 C26 -0.9(16) . . . . ? C24 C25 C26 C21 -1.8(15) . . . . ? C22 C21 C26 C25 2.3(14) . . . . ? C20 C21 C26 C25 171.5(9) . . . . ? O22 Ru1 S1 O1 79.3(4) . . . . ? N19 Ru1 S1 O1 32.2(15) . . . . ? P1 Ru1 S1 O1 -18.9(4) . . . . ? Cl2 Ru1 S1 O1 -106.1(4) . . . . ? Cl1 Ru1 S1 O1 166.6(4) . . . . ? O22 Ru1 S1 C28 -154.2(6) . . . . ? N19 Ru1 S1 C28 158.8(15) . . . . ? P1 Ru1 S1 C28 107.6(5) . . . . ? Cl2 Ru1 S1 C28 20.4(5) . . . . ? Cl1 Ru1 S1 C28 -66.9(5) . . . . ? O22 Ru1 S1 C27 -42.8(4) . . . . ? N19 Ru1 S1 C27 -89.9(15) . . . . ? P1 Ru1 S1 C27 -141.0(4) . . . . ? Cl2 Ru1 S1 C27 131.8(4) . . . . ? Cl1 Ru1 S1 C27 44.5(4) . . . . ? C14 C13 C18 C17 2.2(14) . . . . ? P1 C13 C18 C17 179.1(7) . . . . ? C16 C17 C18 C13 -1.0(16) . . . . ? _refine_diff_density_max 1.097 _refine_diff_density_min -0.833 _refine_diff_density_rms 0.114 #---END