Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Adams, Christopher J.' _publ_contact_author_name 'Prof Christopher J Adams' _publ_contact_author_address ; School of Chemistry University of Bristol Bristol BS8 1TS UNITED KINGDOM ; _publ_contact_author_email 'C.J.ADAMS@BRIS.AC.UK' _publ_section_title ; Synthesis and reactions of diemethyltin dithiooxalate ; data_compound2 _database_code_CSD 172699 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H24 N2 O2 Pt S2' _chemical_formula_weight 583.62 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pt' 'Pt' -1.7033 8.3905 '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 14.210(3) _cell_length_b 7.121(2) _cell_length_c 20.478(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2072.1(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 91 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Needle _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.871 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1136 _exptl_absorpt_coefficient_mu 6.990 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.612 _exptl_absorpt_correction_T_max 0.948 _exptl_absorpt_process_details 'SADABS (Sheldrick 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'omega scans with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 8183 _diffrn_reflns_av_R_equivalents 0.0518 _diffrn_reflns_av_sigmaI/netI 0.0565 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 27.49 _reflns_number_total 2566 _reflns_number_gt 1881 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0308P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2566 _refine_ls_number_parameters 157 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0543 _refine_ls_R_factor_gt 0.0303 _refine_ls_wR_factor_ref 0.0672 _refine_ls_wR_factor_gt 0.0610 _refine_ls_goodness_of_fit_ref 0.944 _refine_ls_restrained_S_all 0.944 _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 Pt1 Pt -0.096080(18) 1.2500 1.057082(14) 0.01883(9) Uani 1 2 d S . . N1 N -0.0699(4) 1.2500 0.9597(3) 0.0186(13) Uani 1 2 d S . . C1 C -0.1348(5) 1.2500 0.9120(4) 0.0281(18) Uani 1 2 d S . . H1A H -0.1993 1.2500 0.9242 0.034 Uiso 1 2 calc SR . . C2 C -0.1137(5) 1.2500 0.8467(4) 0.033(2) Uani 1 2 d S . . H2A H -0.1627 1.2500 0.8152 0.040 Uiso 1 2 calc SR . . C3 C -0.0183(5) 1.2500 0.8265(4) 0.0224(16) Uani 1 2 d S . . C4 C 0.0486(5) 1.2500 0.8759(3) 0.0190(15) Uani 1 2 d S . . H4A H 0.1136 1.2500 0.8649 0.023 Uiso 1 2 calc SR . . C5 C 0.0218(4) 1.2500 0.9413(4) 0.0201(14) Uani 1 2 d S . . C6 C 0.0048(5) 1.2500 0.7535(4) 0.0261(17) Uani 1 2 d S . . C7 C -0.0383(4) 1.0740(9) 0.7222(3) 0.0386(15) Uani 1 1 d . . . H7A H -0.0213 1.0695 0.6758 0.058 Uiso 1 1 calc R . . H7B H -0.1069 1.0785 0.7265 0.058 Uiso 1 1 calc R . . H7C H -0.0142 0.9618 0.7442 0.058 Uiso 1 1 calc R . . C8 C 0.1108(5) 1.2500 0.7413(4) 0.0328(19) Uani 1 2 d S . . H8A H 0.1229 1.2500 0.6942 0.049 Uiso 1 2 calc SR . . H8B H 0.1388 1.1376 0.7610 0.049 Uiso 0.50 1 calc PR . . H8C H 0.1388 1.3624 0.7610 0.049 Uiso 0.50 1 calc PR . . N2 N 0.0479(4) 1.2500 1.0563(3) 0.0237(13) Uani 1 2 d S . . C10 C 0.1047(5) 1.2500 1.1086(4) 0.0285(18) Uani 1 2 d S . . H10A H 0.0766 1.2500 1.1507 0.034 Uiso 1 2 calc SR . . C11 C 0.2010(5) 1.2500 1.1048(3) 0.0284(18) Uani 1 2 d S . . H11A H 0.2385 1.2500 1.1432 0.034 Uiso 1 2 calc SR . . C12 C 0.2424(5) 1.2500 1.0435(3) 0.0232(17) Uani 1 2 d S . . C13 C 0.1862(5) 1.2500 0.9905(3) 0.0206(16) Uani 1 2 d S . . H13A H 0.2137 1.2500 0.9483 0.025 Uiso 1 2 calc SR . . C14 C 0.0895(5) 1.2500 0.9964(3) 0.0171(14) Uani 1 2 d S . . C15 C 0.3526(5) 1.2500 1.0400(4) 0.0257(18) Uani 1 2 d S . . C16 C 0.3898(3) 1.0751(9) 1.0752(3) 0.0380(15) Uani 1 1 d . . . H16A H 0.3651 1.0720 1.1198 0.057 Uiso 1 1 calc R . . H16B H 0.4587 1.0792 1.0764 0.057 Uiso 1 1 calc R . . H16C H 0.3694 0.9623 1.0517 0.057 Uiso 1 1 calc R . . C17 C 0.3873(5) 1.2500 0.9684(4) 0.0312(19) Uani 1 2 d S . . H17A H 0.3626 1.3608 0.9458 0.047 Uiso 0.50 1 calc PR . . H17B H 0.3651 1.1361 0.9464 0.047 Uiso 0.50 1 calc PR . . H17C H 0.4562 1.2531 0.9677 0.047 Uiso 1 2 calc SR . . S1 S -0.25423(13) 1.2500 1.04761(10) 0.0318(5) Uani 1 2 d S . . C19 C -0.3020(5) 1.2500 1.1255(4) 0.0259(17) Uani 1 2 d S . . O1 O -0.3856(3) 1.2500 1.1357(3) 0.0402(15) Uani 1 2 d S . . S2 S -0.11355(12) 1.2500 1.16679(10) 0.0304(5) Uani 1 2 d S . . C20 C -0.2325(5) 1.2500 1.1841(4) 0.0328(19) Uani 1 2 d S . . O2 O -0.2637(4) 1.2500 1.2386(3) 0.0560(19) Uani 1 2 d S . . 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 Pt1 0.01776(13) 0.02066(15) 0.01808(13) 0.000 0.00117(14) 0.000 N1 0.012(3) 0.028(3) 0.016(3) 0.000 0.000(2) 0.000 C1 0.015(3) 0.044(5) 0.025(4) 0.000 0.005(3) 0.000 C2 0.031(5) 0.054(6) 0.015(4) 0.000 -0.009(3) 0.000 C3 0.022(4) 0.025(4) 0.020(4) 0.000 0.003(3) 0.000 C4 0.019(4) 0.021(4) 0.017(4) 0.000 -0.001(3) 0.000 C5 0.021(3) 0.019(4) 0.020(3) 0.000 0.000(3) 0.000 C6 0.024(4) 0.033(5) 0.021(4) 0.000 0.004(3) 0.000 C7 0.037(3) 0.053(4) 0.026(3) -0.004(3) 0.002(3) -0.005(3) C8 0.033(5) 0.043(5) 0.022(4) 0.000 0.004(3) 0.000 N2 0.023(3) 0.027(3) 0.022(3) 0.000 -0.006(3) 0.000 C10 0.032(4) 0.033(5) 0.020(4) 0.000 -0.002(3) 0.000 C11 0.027(4) 0.045(5) 0.013(4) 0.000 -0.012(3) 0.000 C12 0.014(3) 0.031(4) 0.025(4) 0.000 -0.003(3) 0.000 C13 0.025(4) 0.023(4) 0.014(3) 0.000 -0.003(3) 0.000 C14 0.016(3) 0.019(4) 0.016(3) 0.000 0.004(3) 0.000 C15 0.014(4) 0.034(5) 0.029(4) 0.000 -0.006(3) 0.000 C16 0.025(3) 0.044(4) 0.046(4) 0.003(3) -0.007(2) 0.006(3) C17 0.016(4) 0.045(5) 0.033(4) 0.000 0.000(3) 0.000 S1 0.0191(9) 0.0509(13) 0.0255(11) 0.000 0.0017(8) 0.000 C19 0.021(4) 0.028(4) 0.029(4) 0.000 0.006(3) 0.000 O1 0.022(3) 0.058(4) 0.040(4) 0.000 0.010(3) 0.000 S2 0.0236(10) 0.0479(13) 0.0195(9) 0.000 0.0028(8) 0.000 C20 0.031(4) 0.037(5) 0.031(5) 0.000 0.000(4) 0.000 O2 0.036(3) 0.111(6) 0.021(3) 0.000 0.009(3) 0.000 _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 Pt1 N1 2.029(5) . ? Pt1 N2 2.045(6) . ? Pt1 S1 2.2556(19) . ? Pt1 S2 2.260(2) . ? N1 C1 1.344(9) . ? N1 C5 1.356(8) . ? C1 C2 1.369(10) . ? C2 C3 1.417(9) . ? C3 C4 1.388(9) . ? C3 C6 1.530(10) . ? C4 C5 1.393(9) . ? C5 C14 1.482(9) . ? C6 C8 1.526(10) . ? C6 C7 1.535(7) . ? C6 C7 1.535(7) 7_585 ? N2 C10 1.341(9) . ? N2 C14 1.363(8) . ? C10 C11 1.371(10) . ? C11 C12 1.386(10) . ? C12 C13 1.346(9) . ? C12 C15 1.567(9) . ? C13 C14 1.379(9) . ? C15 C16 1.533(7) 7_585 ? C15 C16 1.533(7) . ? C15 C17 1.547(10) . ? S1 C19 1.733(8) . ? C19 O1 1.207(8) . ? C19 C20 1.555(10) . ? S2 C20 1.728(8) . ? C20 O2 1.201(9) . ? 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 Pt1 N2 79.0(2) . . ? N1 Pt1 S1 95.63(16) . . ? N2 Pt1 S1 174.64(18) . . ? N1 Pt1 S2 175.75(15) . . ? N2 Pt1 S2 96.74(18) . . ? S1 Pt1 S2 88.63(7) . . ? C1 N1 C5 117.2(6) . . ? C1 N1 Pt1 126.1(5) . . ? C5 N1 Pt1 116.7(5) . . ? N1 C1 C2 124.0(7) . . ? C1 C2 C3 119.7(7) . . ? C4 C3 C2 116.2(7) . . ? C4 C3 C6 124.4(6) . . ? C2 C3 C6 119.4(6) . . ? C3 C4 C5 120.9(6) . . ? N1 C5 C4 122.0(6) . . ? N1 C5 C14 114.4(6) . . ? C4 C5 C14 123.7(6) . . ? C8 C6 C3 111.8(6) . . ? C8 C6 C7 109.0(4) . . ? C3 C6 C7 108.8(4) . . ? C8 C6 C7 109.0(4) . 7_585 ? C3 C6 C7 108.8(4) . 7_585 ? C7 C6 C7 109.4(6) . 7_585 ? C10 N2 C14 117.3(6) . . ? C10 N2 Pt1 126.6(5) . . ? C14 N2 Pt1 116.2(5) . . ? N2 C10 C11 123.7(7) . . ? C10 C11 C12 118.5(7) . . ? C13 C12 C11 118.5(6) . . ? C13 C12 C15 123.8(7) . . ? C11 C12 C15 117.7(6) . . ? C12 C13 C14 121.4(7) . . ? N2 C14 C13 120.7(6) . . ? N2 C14 C5 113.8(6) . . ? C13 C14 C5 125.5(6) . . ? C16 C15 C16 108.7(6) 7_585 . ? C16 C15 C17 109.6(4) 7_585 . ? C16 C15 C17 109.6(4) . . ? C16 C15 C12 108.9(4) 7_585 . ? C16 C15 C12 108.9(4) . . ? C17 C15 C12 111.2(6) . . ? C19 S1 Pt1 108.1(3) . . ? O1 C19 C20 119.4(7) . . ? O1 C19 S1 123.1(6) . . ? C20 C19 S1 117.5(5) . . ? C20 S2 Pt1 108.2(3) . . ? O2 C20 C19 119.0(7) . . ? O2 C20 S2 123.5(7) . . ? C19 C20 S2 117.5(6) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.471 _refine_diff_density_min -1.173 _refine_diff_density_rms 0.164 data_compound5 _database_code_CSD 172700 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36.50 H39 Cl N2 O3.50 P Ru S3' _chemical_formula_weight 825.37 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' '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.182(5) _cell_length_b 11.229(2) _cell_length_c 38.208(10) _cell_angle_alpha 90.00 _cell_angle_beta 101.87(2) _cell_angle_gamma 90.00 _cell_volume 7214(3) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 76 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.520 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3392 _exptl_absorpt_coefficient_mu 0.767 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.784 _exptl_absorpt_correction_T_max 0.894 _exptl_absorpt_process_details 'SADABS (Sheldrick 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'omega scans with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 45958 _diffrn_reflns_av_R_equivalents 0.0879 _diffrn_reflns_av_sigmaI/netI 0.1151 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -49 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 27.49 _reflns_number_total 16462 _reflns_number_gt 9375 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0529P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16462 _refine_ls_number_parameters 865 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1193 _refine_ls_R_factor_gt 0.0530 _refine_ls_wR_factor_ref 0.1263 _refine_ls_wR_factor_gt 0.1055 _refine_ls_goodness_of_fit_ref 0.956 _refine_ls_restrained_S_all 0.956 _refine_ls_shift/su_max 0.003 _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 -0.32644(2) 2.05670(3) 0.300123(9) 0.01847(10) Uani 1 1 d . . . N1 N -0.2280(2) 2.0449(4) 0.34350(9) 0.0218(9) Uani 1 1 d . . . C1 C -0.1759(3) 2.1332(5) 0.35662(12) 0.0267(12) Uani 1 1 d . . . H1A H -0.1828 2.2092 0.3454 0.032 Uiso 1 1 calc R . . C2 C -0.1137(3) 2.1176(5) 0.38536(12) 0.0285(12) Uani 1 1 d . . . H2A H -0.0789 2.1820 0.3935 0.034 Uiso 1 1 calc R . . C3 C -0.1017(3) 2.0082(4) 0.40237(12) 0.0233(11) Uani 1 1 d . . . C4 C -0.1565(3) 1.9182(4) 0.38964(12) 0.0235(11) Uani 1 1 d . . . H4A H -0.1510 1.8422 0.4008 0.028 Uiso 1 1 calc R . . C5 C -0.2179(3) 1.9387(4) 0.36125(11) 0.0197(10) Uani 1 1 d . . . C6 C -0.0336(3) 1.9875(5) 0.43375(13) 0.0363(14) Uani 1 1 d . . . H6A H -0.0350 1.9049 0.4419 0.054 Uiso 1 1 calc R . . H6B H -0.0386 2.0417 0.4533 0.054 Uiso 1 1 calc R . . H6C H 0.0169 2.0023 0.4264 0.054 Uiso 1 1 calc R . . N2 N -0.3332(2) 1.8798(3) 0.31786(9) 0.0180(8) Uani 1 1 d . . . C7 C -0.3893(3) 1.7998(4) 0.30462(13) 0.0258(11) Uani 1 1 d . . . H7A H -0.4280 1.8212 0.2841 0.031 Uiso 1 1 calc R . . C8 C -0.3944(3) 1.6883(4) 0.31902(13) 0.0278(12) Uani 1 1 d . . . H8A H -0.4358 1.6354 0.3085 0.033 Uiso 1 1 calc R . . C9 C -0.3381(3) 1.6535(4) 0.34920(12) 0.0258(11) Uani 1 1 d . . . C10 C -0.2800(3) 1.7360(4) 0.36280(12) 0.0247(11) Uani 1 1 d . . . H10A H -0.2405 1.7160 0.3832 0.030 Uiso 1 1 calc R . . C11 C -0.2781(3) 1.8473(4) 0.34727(11) 0.0194(10) Uani 1 1 d . . . C12 C -0.3400(3) 1.5322(4) 0.36541(14) 0.0354(13) Uani 1 1 d . . . H12A H -0.3848 1.4868 0.3517 0.053 Uiso 1 1 calc R . . H12B H -0.3462 1.5401 0.3902 0.053 Uiso 1 1 calc R . . H12C H -0.2902 1.4904 0.3649 0.053 Uiso 1 1 calc R . . S1 S -0.32381(7) 2.25355(11) 0.28626(3) 0.0242(3) Uani 1 1 d . . . O1 O -0.25811(19) 2.3291(3) 0.30585(9) 0.0318(9) Uani 1 1 d . . . C13 C -0.3294(3) 2.2813(5) 0.23956(12) 0.0329(13) Uani 1 1 d . . . H13A H -0.3278 2.3673 0.2354 0.049 Uiso 1 1 calc R . . H13B H -0.3792 2.2485 0.2257 0.049 Uiso 1 1 calc R . . H13C H -0.2843 2.2431 0.2320 0.049 Uiso 1 1 calc R . . C14 C -0.4124(3) 2.3333(5) 0.28970(14) 0.0333(13) Uani 1 1 d . . . H14A H -0.4067 2.4171 0.2834 0.050 Uiso 1 1 calc R . . H14B H -0.4207 2.3280 0.3143 0.050 Uiso 1 1 calc R . . H14C H -0.4580 2.2985 0.2733 0.050 Uiso 1 1 calc R . . S2 S -0.44936(7) 2.04819(11) 0.25846(3) 0.0242(3) Uani 1 1 d . . . S3 S -0.40301(8) 2.10162(12) 0.34398(3) 0.0275(3) Uani 1 1 d . . . C15 C -0.5241(3) 2.0682(4) 0.28247(13) 0.0261(11) Uani 1 1 d . . . C16 C -0.5026(3) 2.0856(4) 0.32339(13) 0.0293(12) Uani 1 1 d . . . O2 O -0.5944(2) 2.0657(3) 0.26797(9) 0.0392(9) Uani 1 1 d . . . O3 O -0.5565(2) 2.0923(4) 0.33968(10) 0.0465(11) Uani 1 1 d . . . P1 P -0.25013(7) 1.98916(12) 0.25920(3) 0.0213(3) Uani 1 1 d . . . C1A C -0.3023(3) 1.9837(4) 0.21198(12) 0.0255(11) Uani 1 1 d . . . C1B C -0.3694(3) 1.9103(5) 0.20187(13) 0.0280(12) Uani 1 1 d . . . H1BA H -0.3871 1.8630 0.2193 0.034 Uiso 1 1 calc R . . C1C C -0.4102(3) 1.9068(5) 0.16624(14) 0.0346(13) Uani 1 1 d . . . H1CA H -0.4549 1.8557 0.1595 0.041 Uiso 1 1 calc R . . C1D C -0.3863(3) 1.9766(5) 0.14080(14) 0.0385(15) Uani 1 1 d . . . H1DA H -0.4143 1.9739 0.1166 0.046 Uiso 1 1 calc R . . C1E C -0.3211(3) 2.0509(5) 0.15070(13) 0.0380(14) Uani 1 1 d . . . H1EA H -0.3049 2.1003 0.1333 0.046 Uiso 1 1 calc R . . C1F C -0.2793(3) 2.0535(5) 0.18588(13) 0.0321(12) Uani 1 1 d . . . H1FA H -0.2342 2.1040 0.1922 0.039 Uiso 1 1 calc R . . C1G C -0.1557(3) 2.0617(4) 0.25581(12) 0.0254(11) Uani 1 1 d . . . C1H C -0.1315(3) 2.1673(5) 0.27306(13) 0.0295(12) Uani 1 1 d . . . H1HA H -0.1639 2.2039 0.2874 0.035 Uiso 1 1 calc R . . C1I C -0.0600(3) 2.2214(5) 0.26984(14) 0.0392(14) Uani 1 1 d . . . H1IA H -0.0443 2.2945 0.2817 0.047 Uiso 1 1 calc R . . C1J C -0.0125(3) 2.1688(5) 0.24951(14) 0.0389(14) Uani 1 1 d . . . H1JA H 0.0362 2.2051 0.2473 0.047 Uiso 1 1 calc R . . C1K C -0.0359(3) 2.0630(5) 0.23223(14) 0.0376(14) Uani 1 1 d . . . H1KA H -0.0033 2.0272 0.2179 0.045 Uiso 1 1 calc R . . C1L C -0.1061(3) 2.0082(5) 0.23553(14) 0.0340(13) Uani 1 1 d . . . H1LA H -0.1207 1.9342 0.2240 0.041 Uiso 1 1 calc R . . C1M C -0.2123(3) 1.8373(4) 0.27023(12) 0.0235(11) Uani 1 1 d . . . C1N C -0.1456(3) 1.8272(5) 0.29845(12) 0.0290(12) Uani 1 1 d . . . H1NA H -0.1189 1.8970 0.3086 0.035 Uiso 1 1 calc R . . C1O C -0.1183(3) 1.7154(5) 0.31160(14) 0.0335(13) Uani 1 1 d . . . H1OA H -0.0734 1.7094 0.3307 0.040 Uiso 1 1 calc R . . C1P C -0.1563(3) 1.6145(5) 0.29699(15) 0.0398(14) Uani 1 1 d . . . H1PA H -0.1380 1.5386 0.3062 0.048 Uiso 1 1 calc R . . C1Q C -0.2208(3) 1.6224(5) 0.26919(15) 0.0398(14) Uani 1 1 d . . . H1QA H -0.2464 1.5520 0.2589 0.048 Uiso 1 1 calc R . . C1R C -0.2492(3) 1.7342(5) 0.25588(14) 0.0318(12) Uani 1 1 d . . . H1RA H -0.2942 1.7389 0.2368 0.038 Uiso 1 1 calc R . . Ru2 Ru 0.23278(2) 2.26043(3) 0.494983(10) 0.01767(10) Uani 1 1 d . . . N3 N 0.3359(2) 2.2480(3) 0.53642(9) 0.0193(8) Uani 1 1 d . . . C17 C 0.3891(3) 2.3349(4) 0.54825(12) 0.0247(11) Uani 1 1 d . . . H17A H 0.3819 2.4104 0.5368 0.030 Uiso 1 1 calc R . . C18 C 0.4530(3) 2.3195(5) 0.57601(13) 0.0304(12) Uani 1 1 d . . . H18A H 0.4886 2.3839 0.5831 0.037 Uiso 1 1 calc R . . C19 C 0.4665(3) 2.2112(5) 0.59403(13) 0.0312(13) Uani 1 1 d . . . C20 C 0.4102(3) 2.1239(4) 0.58275(12) 0.0262(11) Uani 1 1 d . . . H20A H 0.4153 2.0491 0.5946 0.031 Uiso 1 1 calc R . . C21 C 0.3466(3) 2.1429(4) 0.55460(12) 0.0219(11) Uani 1 1 d . . . C22 C 0.5362(3) 2.1920(5) 0.62368(14) 0.0442(16) Uani 1 1 d . . . H22A H 0.5348 2.1107 0.6329 0.066 Uiso 1 1 calc R . . H22B H 0.5345 2.2490 0.6429 0.066 Uiso 1 1 calc R . . H22C H 0.5853 2.2035 0.6148 0.066 Uiso 1 1 calc R . . N4 N 0.2279(2) 2.0845(3) 0.51369(9) 0.0184(8) Uani 1 1 d . . . C23 C 0.1729(3) 2.0016(4) 0.50031(12) 0.0240(11) Uani 1 1 d . . . H23A H 0.1324 2.0222 0.4803 0.029 Uiso 1 1 calc R . . C24 C 0.1727(3) 1.8881(4) 0.51426(13) 0.0258(11) Uani 1 1 d . . . H24A H 0.1329 1.8327 0.5037 0.031 Uiso 1 1 calc R . . C25 C 0.2303(3) 1.8548(4) 0.54361(12) 0.0231(11) Uani 1 1 d . . . C26 C 0.2869(3) 1.9393(4) 0.55735(12) 0.0233(11) Uani 1 1 d . . . H26A H 0.3273 1.9201 0.5775 0.028 Uiso 1 1 calc R . . C27 C 0.2857(3) 2.0522(4) 0.54213(11) 0.0195(10) Uani 1 1 d . . . C28 C 0.2336(3) 1.7327(4) 0.55948(13) 0.0307(12) Uani 1 1 d . . . H28A H 0.2790 1.7273 0.5797 0.046 Uiso 1 1 calc R . . H28B H 0.2396 1.6737 0.5413 0.046 Uiso 1 1 calc R . . H28C H 0.1843 1.7170 0.5678 0.046 Uiso 1 1 calc R . . S4 S 0.23848(7) 2.45591(10) 0.47963(3) 0.0221(3) Uani 1 1 d . . . O4 O 0.30776(19) 2.5277(3) 0.49823(9) 0.0302(8) Uani 1 1 d . . . C29 C 0.1535(3) 2.5434(4) 0.48338(14) 0.0324(13) Uani 1 1 d . . . H29A H 0.1615 2.6258 0.4764 0.049 Uiso 1 1 calc R . . H29B H 0.1464 2.5419 0.5082 0.049 Uiso 1 1 calc R . . H29C H 0.1061 2.5106 0.4676 0.049 Uiso 1 1 calc R . . C30 C 0.2327(3) 2.4789(5) 0.43285(12) 0.0326(13) Uani 1 1 d . . . H30A H 0.2357 2.5643 0.4281 0.049 Uiso 1 1 calc R . . H30B H 0.1822 2.4471 0.4194 0.049 Uiso 1 1 calc R . . H30C H 0.2769 2.4378 0.4255 0.049 Uiso 1 1 calc R . . S5 S 0.16876(8) 2.31728(12) 0.54240(3) 0.0286(3) Uani 1 1 d . . . S6 S 0.10322(7) 2.25817(11) 0.45865(3) 0.0240(3) Uani 1 1 d . . . C34 C 0.0370(3) 2.2877(4) 0.48597(14) 0.0290(12) Uani 1 1 d . . . O5 O 0.0181(2) 2.3135(4) 0.54535(10) 0.0463(10) Uani 1 1 d . . . O6 O -0.0345(2) 2.2982(4) 0.47395(11) 0.0464(11) Uani 1 1 d . . . P2 P 0.29439(7) 2.18427(11) 0.44930(3) 0.0180(3) Uani 1 1 d . . . C2A C 0.3906(3) 2.2451(4) 0.44399(11) 0.0203(10) Uani 1 1 d . . . C2B C 0.4240(3) 2.3430(4) 0.46379(11) 0.0214(11) Uani 1 1 d . . . H2BA H 0.3962 2.3808 0.4798 0.026 Uiso 1 1 calc R . . C2C C 0.4985(3) 2.3862(4) 0.46030(12) 0.0245(11) Uani 1 1 d . . . H2CA H 0.5207 2.4532 0.4739 0.029 Uiso 1 1 calc R . . C2D C 0.5402(3) 2.3323(5) 0.43717(13) 0.0283(12) Uani 1 1 d . . . H2DA H 0.5914 2.3607 0.4354 0.034 Uiso 1 1 calc R . . C2E C 0.5063(3) 2.2364(5) 0.41666(13) 0.0295(12) Uani 1 1 d . . . H2EA H 0.5334 2.2012 0.4000 0.035 Uiso 1 1 calc R . . C2F C 0.4329(3) 2.1913(4) 0.42034(12) 0.0241(11) Uani 1 1 d . . . H2FA H 0.4112 2.1237 0.4068 0.029 Uiso 1 1 calc R . . C2G C 0.3226(3) 2.0264(4) 0.45447(12) 0.0210(10) Uani 1 1 d . . . C2H C 0.3844(3) 1.9961(4) 0.48283(13) 0.0265(11) Uani 1 1 d . . . H2HA H 0.4103 2.0570 0.4982 0.032 Uiso 1 1 calc R . . C2I C 0.4088(3) 1.8788(5) 0.48901(14) 0.0325(13) Uani 1 1 d . . . H2IA H 0.4514 1.8602 0.5084 0.039 Uiso 1 1 calc R . . C2J C 0.3713(3) 1.7888(5) 0.46709(15) 0.0383(14) Uani 1 1 d . . . H2JA H 0.3863 1.7080 0.4718 0.046 Uiso 1 1 calc R . . C2K C 0.3119(4) 1.8185(5) 0.43834(16) 0.0446(16) Uani 1 1 d . . . H2KA H 0.2878 1.7577 0.4225 0.053 Uiso 1 1 calc R . . C2L C 0.2866(3) 1.9349(4) 0.43208(14) 0.0313(12) Uani 1 1 d . . . H2LA H 0.2444 1.9528 0.4125 0.038 Uiso 1 1 calc R . . C2M C 0.2344(3) 2.1902(4) 0.40345(12) 0.0223(11) Uani 1 1 d . . . C2N C 0.2571(3) 2.2514(5) 0.37604(13) 0.0342(13) Uani 1 1 d . . . H2NA H 0.3071 2.2907 0.3804 0.041 Uiso 1 1 calc R . . C2O C 0.2090(4) 2.2571(5) 0.34227(14) 0.0443(15) Uani 1 1 d . . . H2OA H 0.2268 2.2982 0.3236 0.053 Uiso 1 1 calc R . . C2P C 0.1363(4) 2.2041(6) 0.33565(15) 0.0496(17) Uani 1 1 d . . . H2PA H 0.1030 2.2091 0.3125 0.059 Uiso 1 1 calc R . . C2Q C 0.1106(3) 2.1425(5) 0.36281(15) 0.0417(15) Uani 1 1 d . . . H2QA H 0.0595 2.1065 0.3583 0.050 Uiso 1 1 calc R . . C2R C 0.1597(3) 2.1337(4) 0.39644(13) 0.0281(12) Uani 1 1 d . . . H2RA H 0.1428 2.0896 0.4148 0.034 Uiso 1 1 calc R . . C33 C 0.0679(3) 2.3073(5) 0.52647(14) 0.0309(12) Uani 1 1 d . . . C35 C -0.0349(4) 2.4660(6) 0.39902(16) 0.0563(18) Uani 1 1 d . . . H35A H -0.0249 2.5452 0.4105 0.068 Uiso 1 1 calc R . . H35B H -0.0197 2.4047 0.4178 0.068 Uiso 1 1 calc R . . Cl1 Cl -0.13563(11) 2.45217(17) 0.38002(5) 0.0707(5) Uani 1 1 d . . . Cl2 Cl 0.02317(13) 2.4498(3) 0.36709(6) 0.1042(8) Uani 1 1 d . . . C36 C -0.0847(5) 2.2286(9) 0.6119(2) 0.103(3) Uani 1 1 d . . . H36A H -0.0296 2.2555 0.6143 0.155 Uiso 1 1 calc R . . H36B H -0.1208 2.2888 0.5990 0.155 Uiso 1 1 calc R . . H36C H -0.0920 2.1533 0.5987 0.155 Uiso 1 1 calc R . . C37 C -0.1018(6) 2.2113(12) 0.6472(3) 0.157(6) Uani 1 1 d D . . H37A H -0.0649 2.1506 0.6601 0.188 Uiso 1 1 calc R . . H37B H -0.0918 2.2868 0.6607 0.188 Uiso 1 1 calc R . . O7 O -0.1776(4) 2.1761(6) 0.64645(15) 0.113(2) Uani 1 1 d D . . C38 C -0.1855(4) 2.1345(8) 0.67736(16) 0.071(2) Uani 1 1 d D . . H38A H -0.1876 2.2006 0.6943 0.086 Uiso 1 1 calc R . . H38B H -0.1399 2.0824 0.6876 0.086 Uiso 1 1 calc R . . C39 C -0.2632(4) 2.0634(7) 0.67091(16) 0.064(2) Uani 1 1 d . . . H39A H -0.2728 2.0339 0.6938 0.096 Uiso 1 1 calc R . . H39B H -0.2592 1.9958 0.6551 0.096 Uiso 1 1 calc R . . H39C H -0.3073 2.1149 0.6597 0.096 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0170(2) 0.0223(2) 0.01576(18) -0.00137(16) 0.00251(15) 0.00015(17) N1 0.018(2) 0.028(2) 0.020(2) -0.0047(17) 0.0060(16) -0.0038(18) C1 0.029(3) 0.028(3) 0.023(3) -0.003(2) 0.004(2) -0.007(2) C2 0.022(3) 0.033(3) 0.028(3) -0.005(2) 0.001(2) -0.005(2) C3 0.020(3) 0.029(3) 0.020(2) -0.002(2) 0.003(2) 0.001(2) C4 0.023(3) 0.022(3) 0.024(3) 0.000(2) 0.002(2) -0.003(2) C5 0.020(2) 0.019(3) 0.021(2) -0.001(2) 0.0066(19) 0.002(2) C6 0.029(3) 0.039(3) 0.037(3) -0.001(3) -0.002(2) -0.007(3) N2 0.018(2) 0.022(2) 0.0145(19) -0.0011(16) 0.0052(16) 0.0010(17) C7 0.025(3) 0.025(3) 0.026(3) -0.001(2) 0.001(2) -0.002(2) C8 0.023(3) 0.028(3) 0.032(3) -0.002(2) 0.004(2) -0.003(2) C9 0.026(3) 0.030(3) 0.023(3) -0.001(2) 0.010(2) 0.000(2) C10 0.028(3) 0.024(3) 0.022(2) 0.001(2) 0.004(2) -0.001(2) C11 0.021(3) 0.024(3) 0.014(2) -0.0034(19) 0.0041(19) -0.001(2) C12 0.041(3) 0.026(3) 0.036(3) 0.000(2) 0.002(3) -0.010(3) S1 0.0242(6) 0.0237(7) 0.0242(6) -0.0010(5) 0.0035(5) 0.0020(5) O1 0.028(2) 0.024(2) 0.040(2) -0.0039(16) -0.0019(16) -0.0039(16) C13 0.046(3) 0.026(3) 0.029(3) 0.006(2) 0.012(2) 0.003(3) C14 0.030(3) 0.028(3) 0.042(3) 0.003(2) 0.008(3) 0.011(2) S2 0.0189(6) 0.0327(7) 0.0199(6) -0.0009(5) 0.0014(5) 0.0007(5) S3 0.0261(7) 0.0359(8) 0.0209(6) -0.0015(5) 0.0054(5) 0.0030(6) C15 0.026(3) 0.023(3) 0.029(3) -0.003(2) 0.005(2) 0.005(2) C16 0.032(3) 0.027(3) 0.032(3) -0.008(2) 0.015(2) -0.003(2) O2 0.0191(19) 0.053(3) 0.043(2) -0.0075(19) 0.0025(17) 0.0049(18) O3 0.030(2) 0.067(3) 0.046(2) -0.014(2) 0.0169(19) -0.004(2) P1 0.0199(7) 0.0258(7) 0.0182(6) -0.0010(5) 0.0038(5) -0.0013(5) C1A 0.024(3) 0.029(3) 0.023(3) -0.006(2) 0.005(2) 0.006(2) C1B 0.025(3) 0.031(3) 0.028(3) -0.005(2) 0.007(2) 0.006(2) C1C 0.024(3) 0.046(4) 0.031(3) -0.013(3) -0.001(2) 0.008(3) C1D 0.039(3) 0.050(4) 0.021(3) -0.007(3) -0.007(2) 0.023(3) C1E 0.051(4) 0.037(3) 0.025(3) 0.003(2) 0.005(3) 0.014(3) C1F 0.039(3) 0.033(3) 0.026(3) -0.003(2) 0.010(2) 0.005(3) C1G 0.024(3) 0.030(3) 0.023(2) -0.001(2) 0.009(2) -0.003(2) C1H 0.025(3) 0.036(3) 0.027(3) -0.004(2) 0.006(2) -0.004(2) C1I 0.036(3) 0.041(4) 0.040(3) -0.007(3) 0.007(3) -0.014(3) C1J 0.024(3) 0.057(4) 0.037(3) 0.001(3) 0.010(3) -0.015(3) C1K 0.029(3) 0.051(4) 0.037(3) -0.002(3) 0.016(2) -0.003(3) C1L 0.036(3) 0.031(3) 0.036(3) -0.005(2) 0.009(3) -0.002(3) C1M 0.025(3) 0.028(3) 0.018(2) 0.000(2) 0.006(2) 0.000(2) C1N 0.024(3) 0.038(3) 0.026(3) -0.002(2) 0.007(2) 0.002(2) C1O 0.026(3) 0.044(4) 0.029(3) 0.002(2) 0.003(2) 0.011(3) C1P 0.039(4) 0.030(3) 0.055(4) 0.013(3) 0.022(3) 0.013(3) C1Q 0.038(3) 0.031(3) 0.050(4) -0.003(3) 0.009(3) 0.000(3) C1R 0.027(3) 0.031(3) 0.038(3) -0.002(2) 0.007(2) 0.005(2) Ru2 0.01599(19) 0.0178(2) 0.01922(19) 0.00025(16) 0.00371(15) -0.00143(16) N3 0.018(2) 0.018(2) 0.021(2) -0.0014(16) 0.0030(16) 0.0000(17) C17 0.023(3) 0.026(3) 0.024(3) -0.003(2) 0.002(2) -0.006(2) C18 0.029(3) 0.024(3) 0.036(3) -0.003(2) 0.002(2) -0.011(2) C19 0.028(3) 0.034(3) 0.029(3) 0.000(2) 0.001(2) -0.005(2) C20 0.023(3) 0.025(3) 0.028(3) 0.002(2) -0.001(2) -0.006(2) C21 0.025(3) 0.023(3) 0.019(2) 0.001(2) 0.008(2) -0.001(2) C22 0.035(3) 0.050(4) 0.038(3) 0.009(3) -0.014(3) -0.010(3) N4 0.015(2) 0.019(2) 0.022(2) 0.0020(16) 0.0059(16) -0.0027(16) C23 0.024(3) 0.027(3) 0.018(2) 0.002(2) -0.001(2) 0.000(2) C24 0.021(3) 0.029(3) 0.029(3) -0.003(2) 0.007(2) -0.006(2) C25 0.026(3) 0.019(3) 0.027(3) 0.000(2) 0.012(2) -0.001(2) C26 0.021(3) 0.026(3) 0.024(2) 0.004(2) 0.007(2) 0.001(2) C27 0.015(2) 0.025(3) 0.019(2) -0.001(2) 0.0059(19) -0.003(2) C28 0.029(3) 0.024(3) 0.038(3) 0.004(2) 0.008(2) -0.004(2) S4 0.0207(6) 0.0181(7) 0.0270(6) -0.0001(5) 0.0038(5) -0.0005(5) O4 0.0262(19) 0.0204(19) 0.042(2) -0.0035(15) 0.0011(16) -0.0051(15) C29 0.028(3) 0.023(3) 0.047(3) -0.005(2) 0.009(2) 0.003(2) C30 0.042(3) 0.028(3) 0.030(3) 0.010(2) 0.012(2) 0.004(3) S5 0.0288(7) 0.0346(8) 0.0232(6) -0.0008(6) 0.0073(5) 0.0036(6) S6 0.0186(6) 0.0266(7) 0.0259(6) 0.0011(5) 0.0027(5) -0.0016(5) C34 0.025(3) 0.021(3) 0.041(3) 0.002(2) 0.007(2) -0.005(2) O5 0.041(2) 0.061(3) 0.045(2) 0.001(2) 0.028(2) 0.004(2) O6 0.021(2) 0.056(3) 0.062(3) 0.003(2) 0.0080(19) 0.0015(19) P2 0.0168(6) 0.0177(6) 0.0190(6) 0.0006(5) 0.0025(5) -0.0023(5) C2A 0.022(2) 0.021(3) 0.017(2) 0.002(2) 0.0025(19) -0.002(2) C2B 0.025(3) 0.023(3) 0.018(2) 0.0008(19) 0.007(2) -0.001(2) C2C 0.026(3) 0.021(3) 0.025(3) -0.003(2) 0.001(2) -0.010(2) C2D 0.022(3) 0.031(3) 0.032(3) 0.008(2) 0.006(2) -0.004(2) C2E 0.023(3) 0.040(3) 0.027(3) 0.001(2) 0.009(2) 0.001(2) C2F 0.027(3) 0.022(3) 0.023(3) -0.008(2) 0.005(2) 0.002(2) C2G 0.017(2) 0.021(3) 0.026(3) 0.000(2) 0.009(2) -0.001(2) C2H 0.028(3) 0.026(3) 0.027(3) 0.000(2) 0.008(2) -0.001(2) C2I 0.040(3) 0.026(3) 0.032(3) 0.006(2) 0.009(2) 0.006(3) C2J 0.043(4) 0.022(3) 0.050(4) 0.008(3) 0.010(3) 0.009(3) C2K 0.056(4) 0.015(3) 0.061(4) -0.009(3) 0.006(3) -0.009(3) C2L 0.034(3) 0.021(3) 0.036(3) 0.002(2) 0.001(2) -0.001(2) C2M 0.023(3) 0.021(3) 0.022(2) 0.000(2) 0.002(2) 0.000(2) C2N 0.036(3) 0.033(3) 0.031(3) 0.006(2) 0.003(2) -0.005(3) C2O 0.048(4) 0.053(4) 0.029(3) 0.008(3) 0.001(3) -0.006(3) C2P 0.050(4) 0.065(5) 0.025(3) 0.002(3) -0.012(3) 0.008(3) C2Q 0.029(3) 0.049(4) 0.043(3) -0.011(3) -0.002(3) -0.008(3) C2R 0.025(3) 0.031(3) 0.027(3) -0.006(2) 0.004(2) 0.001(2) C33 0.028(3) 0.026(3) 0.043(3) 0.003(2) 0.018(3) 0.003(2) C35 0.071(5) 0.048(4) 0.045(4) 0.005(3) 0.002(3) 0.002(4) Cl1 0.0617(12) 0.0757(13) 0.0697(12) 0.0225(10) 0.0020(9) -0.0063(10) Cl2 0.0748(15) 0.157(2) 0.0813(15) 0.0066(15) 0.0168(12) 0.0368(15) C36 0.082(6) 0.119(8) 0.112(8) 0.001(6) 0.027(6) -0.024(6) C37 0.143(10) 0.228(14) 0.101(8) -0.044(8) 0.031(7) -0.136(10) O7 0.091(5) 0.176(7) 0.070(4) -0.030(4) 0.010(3) -0.065(5) C38 0.043(4) 0.145(8) 0.028(4) -0.026(4) 0.013(3) 0.002(4) C39 0.068(5) 0.085(5) 0.039(4) -0.015(4) 0.010(3) 0.012(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N2 2.110(4) . ? Ru1 N1 2.115(4) . ? Ru1 S1 2.2757(14) . ? Ru1 P1 2.3629(14) . ? Ru1 S2 2.3707(14) . ? Ru1 S3 2.3875(14) . ? N1 C1 1.362(6) . ? N1 C5 1.365(6) . ? C1 C2 1.377(6) . ? C2 C3 1.385(7) . ? C3 C4 1.399(6) . ? C3 C6 1.511(6) . ? C4 C5 1.368(6) . ? C5 C11 1.478(6) . ? N2 C7 1.339(6) . ? N2 C11 1.361(5) . ? C7 C8 1.377(7) . ? C8 C9 1.399(6) . ? C9 C10 1.383(6) . ? C9 C12 1.500(7) . ? C10 C11 1.387(6) . ? S1 O1 1.486(3) . ? S1 C14 1.794(5) . ? S1 C13 1.794(5) . ? S2 C15 1.740(5) . ? S3 C16 1.739(5) . ? C15 O2 1.221(5) . ? C15 C16 1.543(7) . ? C16 O3 1.220(6) . ? P1 C1M 1.843(5) . ? P1 C1A 1.843(5) . ? P1 C1G 1.843(5) . ? C1A C1F 1.389(7) . ? C1A C1B 1.405(7) . ? C1B C1C 1.398(7) . ? C1C C1D 1.376(8) . ? C1D C1E 1.386(8) . ? C1E C1F 1.388(7) . ? C1G C1H 1.378(7) . ? C1G C1L 1.401(7) . ? C1H C1I 1.399(7) . ? C1I C1J 1.370(7) . ? C1J C1K 1.379(8) . ? C1K C1L 1.382(7) . ? C1M C1R 1.378(7) . ? C1M C1N 1.407(6) . ? C1N C1O 1.397(7) . ? C1O C1P 1.368(7) . ? C1P C1Q 1.371(7) . ? C1Q C1R 1.403(7) . ? Ru2 N4 2.108(4) . ? Ru2 N3 2.124(4) . ? Ru2 S4 2.2795(13) . ? Ru2 S6 2.3690(14) . ? Ru2 P2 2.3789(14) . ? Ru2 S5 2.3917(14) . ? N3 C17 1.349(6) . ? N3 C21 1.363(6) . ? C17 C18 1.371(6) . ? C18 C19 1.394(7) . ? C19 C20 1.383(7) . ? C19 C22 1.485(7) . ? C20 C21 1.383(6) . ? C21 C27 1.469(6) . ? N4 C23 1.350(6) . ? N4 C27 1.362(5) . ? C23 C24 1.382(7) . ? C24 C25 1.386(6) . ? C25 C26 1.383(6) . ? C25 C28 1.496(6) . ? C26 C27 1.393(6) . ? S4 O4 1.491(3) . ? S4 C30 1.788(5) . ? S4 C29 1.790(5) . ? S5 C33 1.719(5) . ? S6 C34 1.726(5) . ? C34 O6 1.226(6) . ? C34 C33 1.545(7) . ? O5 C33 1.229(6) . ? P2 C2G 1.838(5) . ? P2 C2A 1.838(5) . ? P2 C2M 1.842(5) . ? C2A C2B 1.390(6) . ? C2A C2F 1.407(6) . ? C2B C2C 1.400(6) . ? C2C C2D 1.386(7) . ? C2D C2E 1.388(7) . ? C2E C2F 1.393(7) . ? C2G C2H 1.394(6) . ? C2G C2L 1.397(6) . ? C2H C2I 1.388(7) . ? C2I C2J 1.385(7) . ? C2J C2K 1.378(7) . ? C2K C2L 1.383(7) . ? C2M C2N 1.375(7) . ? C2M C2R 1.407(6) . ? C2N C2O 1.384(7) . ? C2O C2P 1.360(8) . ? C2P C2Q 1.392(8) . ? C2Q C2R 1.388(7) . ? C35 Cl2 1.737(7) . ? C35 Cl1 1.740(6) . ? C36 C37 1.449(11) . ? C37 O7 1.355(9) . ? O7 C38 1.303(8) . ? C38 C39 1.532(9) . ? 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 N2 Ru1 N1 77.10(14) . . ? N2 Ru1 S1 173.94(10) . . ? N1 Ru1 S1 101.10(11) . . ? N2 Ru1 P1 89.13(10) . . ? N1 Ru1 P1 92.03(11) . . ? S1 Ru1 P1 96.74(5) . . ? N2 Ru1 S2 94.45(10) . . ? N1 Ru1 S2 169.14(11) . . ? S1 Ru1 S2 86.58(4) . . ? P1 Ru1 S2 94.69(5) . . ? N2 Ru1 S3 84.21(10) . . ? N1 Ru1 S3 86.01(11) . . ? S1 Ru1 S3 89.90(5) . . ? P1 Ru1 S3 173.32(5) . . ? S2 Ru1 S3 86.35(5) . . ? C1 N1 C5 116.5(4) . . ? C1 N1 Ru1 127.0(3) . . ? C5 N1 Ru1 116.4(3) . . ? N1 C1 C2 123.0(5) . . ? C1 C2 C3 120.3(5) . . ? C2 C3 C4 116.9(4) . . ? C2 C3 C6 121.7(4) . . ? C4 C3 C6 121.3(4) . . ? C5 C4 C3 120.5(4) . . ? N1 C5 C4 122.7(4) . . ? N1 C5 C11 114.7(4) . . ? C4 C5 C11 122.6(4) . . ? C7 N2 C11 117.2(4) . . ? C7 N2 Ru1 126.4(3) . . ? C11 N2 Ru1 116.3(3) . . ? N2 C7 C8 124.0(4) . . ? C7 C8 C9 119.6(5) . . ? C10 C9 C8 116.5(5) . . ? C10 C9 C12 121.9(4) . . ? C8 C9 C12 121.6(4) . . ? C9 C10 C11 121.4(4) . . ? N2 C11 C10 121.4(4) . . ? N2 C11 C5 115.4(4) . . ? C10 C11 C5 123.2(4) . . ? O1 S1 C14 104.2(2) . . ? O1 S1 C13 106.4(2) . . ? C14 S1 C13 96.5(2) . . ? O1 S1 Ru1 119.15(14) . . ? C14 S1 Ru1 114.23(18) . . ? C13 S1 Ru1 113.61(18) . . ? C15 S2 Ru1 107.04(16) . . ? C16 S3 Ru1 107.07(17) . . ? O2 C15 C16 118.1(4) . . ? O2 C15 S2 121.7(4) . . ? C16 C15 S2 120.1(4) . . ? O3 C16 C15 118.4(5) . . ? O3 C16 S3 122.8(4) . . ? C15 C16 S3 118.7(4) . . ? C1M P1 C1A 105.7(2) . . ? C1M P1 C1G 98.7(2) . . ? C1A P1 C1G 101.8(2) . . ? C1M P1 Ru1 111.31(16) . . ? C1A P1 Ru1 115.73(16) . . ? C1G P1 Ru1 121.37(16) . . ? C1F C1A C1B 118.2(4) . . ? C1F C1A P1 122.1(4) . . ? C1B C1A P1 119.7(4) . . ? C1C C1B C1A 120.2(5) . . ? C1D C1C C1B 120.6(5) . . ? C1C C1D C1E 119.5(5) . . ? C1D C1E C1F 120.4(5) . . ? C1E C1F C1A 121.1(5) . . ? C1H C1G C1L 118.4(5) . . ? C1H C1G P1 122.0(4) . . ? C1L C1G P1 119.6(4) . . ? C1G C1H C1I 121.1(5) . . ? C1J C1I C1H 120.0(5) . . ? C1I C1J C1K 119.6(5) . . ? C1J C1K C1L 120.9(5) . . ? C1K C1L C1G 120.1(5) . . ? C1R C1M C1N 118.2(5) . . ? C1R C1M P1 125.1(4) . . ? C1N C1M P1 116.3(4) . . ? C1O C1N C1M 120.5(5) . . ? C1P C1O C1N 120.1(5) . . ? C1O C1P C1Q 120.3(5) . . ? C1P C1Q C1R 120.2(5) . . ? C1M C1R C1Q 120.7(5) . . ? N4 Ru2 N3 76.79(14) . . ? N4 Ru2 S4 175.12(10) . . ? N3 Ru2 S4 100.46(11) . . ? N4 Ru2 S6 95.17(10) . . ? N3 Ru2 S6 167.27(10) . . ? S4 Ru2 S6 86.82(4) . . ? N4 Ru2 P2 88.10(11) . . ? N3 Ru2 P2 95.41(10) . . ? S4 Ru2 P2 96.21(5) . . ? S6 Ru2 P2 94.16(5) . . ? N4 Ru2 S5 86.35(11) . . ? N3 Ru2 S5 84.04(11) . . ? S4 Ru2 S5 89.36(5) . . ? S6 Ru2 S5 85.62(5) . . ? P2 Ru2 S5 174.41(5) . . ? C17 N3 C21 116.4(4) . . ? C17 N3 Ru2 127.3(3) . . ? C21 N3 Ru2 116.2(3) . . ? N3 C17 C18 123.2(5) . . ? C17 C18 C19 121.2(5) . . ? C20 C19 C18 115.4(4) . . ? C20 C19 C22 122.5(5) . . ? C18 C19 C22 122.0(5) . . ? C19 C20 C21 121.6(5) . . ? N3 C21 C20 122.2(4) . . ? N3 C21 C27 115.1(4) . . ? C20 C21 C27 122.8(4) . . ? C23 N4 C27 117.2(4) . . ? C23 N4 Ru2 126.3(3) . . ? C27 N4 Ru2 116.5(3) . . ? N4 C23 C24 123.2(4) . . ? C23 C24 C25 120.1(4) . . ? C26 C25 C24 116.9(4) . . ? C26 C25 C28 120.7(4) . . ? C24 C25 C28 122.4(4) . . ? C25 C26 C27 121.1(4) . . ? N4 C27 C26 121.5(4) . . ? N4 C27 C21 115.3(4) . . ? C26 C27 C21 123.2(4) . . ? O4 S4 C30 105.9(2) . . ? O4 S4 C29 104.4(2) . . ? C30 S4 C29 97.0(2) . . ? O4 S4 Ru2 118.05(14) . . ? C30 S4 Ru2 113.56(18) . . ? C29 S4 Ru2 115.42(18) . . ? C33 S5 Ru2 107.58(19) . . ? C34 S6 Ru2 107.46(18) . . ? O6 C34 C33 118.1(5) . . ? O6 C34 S6 121.8(4) . . ? C33 C34 S6 120.0(4) . . ? C2G P2 C2A 98.5(2) . . ? C2G P2 C2M 102.7(2) . . ? C2A P2 C2M 102.8(2) . . ? C2G P2 Ru2 114.54(15) . . ? C2A P2 Ru2 119.56(15) . . ? C2M P2 Ru2 116.01(16) . . ? C2B C2A C2F 118.6(4) . . ? C2B C2A P2 121.0(4) . . ? C2F C2A P2 120.4(4) . . ? C2A C2B C2C 120.4(4) . . ? C2D C2C C2B 120.8(4) . . ? C2C C2D C2E 119.1(5) . . ? C2D C2E C2F 120.6(5) . . ? C2E C2F C2A 120.4(4) . . ? C2H C2G C2L 117.9(4) . . ? C2H C2G P2 117.4(4) . . ? C2L C2G P2 124.7(4) . . ? C2I C2H C2G 121.2(5) . . ? C2J C2I C2H 120.2(5) . . ? C2K C2J C2I 118.8(5) . . ? C2J C2K C2L 121.5(5) . . ? C2K C2L C2G 120.3(5) . . ? C2N C2M C2R 118.1(4) . . ? C2N C2M P2 123.5(4) . . ? C2R C2M P2 118.4(4) . . ? C2M C2N C2O 121.6(5) . . ? C2P C2O C2N 120.2(6) . . ? C2O C2P C2Q 119.9(5) . . ? C2R C2Q C2P 120.0(5) . . ? C2Q C2R C2M 120.1(5) . . ? O5 C33 C34 117.4(5) . . ? O5 C33 S5 124.1(4) . . ? C34 C33 S5 118.5(4) . . ? Cl2 C35 Cl1 111.3(3) . . ? O7 C37 C36 113.5(8) . . ? C38 O7 C37 111.4(7) . . ? O7 C38 C39 106.9(5) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.831 _refine_diff_density_min -0.939 _refine_diff_density_rms 0.114