# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 182/1449 data_la9805 _audit_creation_method SHELXL _chemical_name_systematic ; (Ph4As)2[Ru(S2C2(CN)2]3 ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C60 H40 As2 N6 Ru S6' _chemical_formula_weight 1288.25 _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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'As' 'As' 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, z' 'x, -y, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, -z' '-x, y, -z-1/2' 'x-1/2, y-1/2, -z-1/2' _cell_length_a 20.399(2) _cell_length_b 15.674(2) _cell_length_c 18.020(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5761.8(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15 _cell_measurement_theta_max 16 _exptl_crystal_description block-shaped _exptl_crystal_colour black _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.485 _exptl_crystal_density_method ? _exptl_crystal_F_000 2592 _exptl_absorpt_coefficient_mu 1.673 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8070 _exptl_absorpt_correction_T_max 1.0000 _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 'Enraf-Nonius CAD4' _diffrn_measurement_method '\w/2\q' _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 5068 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0508 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 24.98 _reflns_number_total 5068 _reflns_number_observed 2984 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4-ARGUS (Enraf-Nonius, 1994)' _computing_cell_refinement 'CAD4-ARGUS (Enraf-Nonius, 1994)' _computing_data_reduction ; CHI90s (Boyle, 1996), XCAD4 (Harms, 1996), SHELXTL-v5 (Siemens, 1994) ; _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXTL-v5 (Siemens, 1994)' _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^)+(0.0536P)^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 'Idealized with riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5068 _refine_ls_number_parameters 339 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0898 _refine_ls_R_factor_obs 0.0471 _refine_ls_wR_factor_all 0.1124 _refine_ls_wR_factor_obs 0.0999 _refine_ls_goodness_of_fit_all 0.984 _refine_ls_goodness_of_fit_obs 1.167 _refine_ls_restrained_S_all 0.984 _refine_ls_restrained_S_obs 1.167 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ru Ru 0.5000 0.17104(3) 0.2500 0.0656(2) Uani 1 d S . S1 S 0.44461(6) 0.18408(8) 0.13673(7) 0.0745(4) Uani 1 d . . C1 C 0.3911(2) 0.2672(3) 0.1513(3) 0.0647(13) Uani 1 d . . C2 C 0.3539(3) 0.2951(3) 0.0887(3) 0.078(2) Uani 1 d . . N1 N 0.3240(3) 0.3162(3) 0.0392(3) 0.101(2) Uani 1 d . . S2 S 0.42533(6) 0.27188(8) 0.29676(7) 0.0712(4) Uani 1 d . . C3 C 0.3820(2) 0.3036(3) 0.2196(3) 0.0635(12) Uani 1 d . . C4 C 0.3346(3) 0.3695(3) 0.2287(3) 0.083(2) Uani 1 d . . N2 N 0.2964(3) 0.4214(3) 0.2342(3) 0.126(2) Uani 1 d . . S3 S 0.55749(7) 0.06229(9) 0.18995(8) 0.0846(4) Uani 1 d . . C5 C 0.5234(2) -0.0308(3) 0.2236(3) 0.086(2) Uani 1 d . . C6 C 0.5471(3) -0.1092(4) 0.1917(4) 0.130(3) Uani 1 d . . N3 N 0.5657(4) -0.1704(4) 0.1653(5) 0.192(4) Uani 1 d . . As As 0.36617(2) 0.67153(3) 0.09854(3) 0.0613(2) Uani 1 d . . C11 C 0.4452(2) 0.6066(3) 0.1055(3) 0.0624(12) Uani 1 d . . C12 C 0.4442(3) 0.5338(4) 0.1450(4) 0.109(2) Uani 1 d . . H12 H 0.4066(3) 0.5189(4) 0.1712(4) 0.131 Uiso 1 calc R . C13 C 0.4986(3) 0.4807(4) 0.1471(4) 0.122(2) Uani 1 d . . H13 H 0.4972(3) 0.4304(4) 0.1744(4) 0.146 Uiso 1 calc R . C14 C 0.5531(3) 0.5017(4) 0.1098(4) 0.096(2) Uani 1 d . . H14 H 0.5893(3) 0.4656(4) 0.1104(4) 0.115 Uiso 1 calc R . C15 C 0.5552(3) 0.5744(5) 0.0719(4) 0.119(2) Uani 1 d . . H15 H 0.5932(3) 0.5897(5) 0.0468(4) 0.143 Uiso 1 calc R . C16 C 0.5003(3) 0.6280(4) 0.0697(3) 0.101(2) Uani 1 d . . H16 H 0.5021(3) 0.6789(4) 0.0432(3) 0.121 Uiso 1 calc R . C21 C 0.3182(2) 0.6584(3) 0.1879(2) 0.0606(12) Uani 1 d . . C22 C 0.3476(3) 0.6719(3) 0.2549(3) 0.085(2) Uani 1 d . . H22 H 0.3921(3) 0.6843(3) 0.2571(3) 0.102 Uiso 1 calc R . C23 C 0.3111(4) 0.6671(4) 0.3201(3) 0.097(2) Uani 1 d . . H23 H 0.3308(4) 0.6765(4) 0.3659(3) 0.116 Uiso 1 calc R . C24 C 0.2461(4) 0.6485(3) 0.3156(4) 0.092(2) Uani 1 d . . H24 H 0.2214(4) 0.6457(3) 0.3589(4) 0.111 Uiso 1 calc R . C25 C 0.2164(3) 0.6338(3) 0.2487(4) 0.085(2) Uani 1 d . . H25 H 0.1721(3) 0.6202(3) 0.2467(4) 0.102 Uiso 1 calc R . C26 C 0.2524(2) 0.6393(3) 0.1849(3) 0.0667(13) Uani 1 d . . H26 H 0.2323(2) 0.6301(3) 0.1392(3) 0.080 Uiso 1 calc R . C31 C 0.3812(2) 0.7905(3) 0.0828(3) 0.0635(12) Uani 1 d . . C32 C 0.3551(3) 0.8470(3) 0.1306(3) 0.0792(15) Uani 1 d . . H32 H 0.3300(3) 0.8277(3) 0.1702(3) 0.095 Uiso 1 calc R . C33 C 0.3653(3) 0.9342(4) 0.1212(3) 0.097(2) Uani 1 d . . H33 H 0.3484(3) 0.9728(4) 0.1553(3) 0.117 Uiso 1 calc R . C34 C 0.3997(3) 0.9620(4) 0.0626(4) 0.105(2) Uani 1 d . . H34 H 0.4059(3) 1.0203(4) 0.0559(4) 0.126 Uiso 1 calc R . C35 C 0.4251(3) 0.9073(4) 0.0139(4) 0.114(2) Uani 1 d . . H35 H 0.4496(3) 0.9275(4) -0.0260(4) 0.137 Uiso 1 calc R . C36 C 0.4149(3) 0.8188(3) 0.0227(3) 0.099(2) Uani 1 d . . H36 H 0.4311(3) 0.7804(3) -0.0122(3) 0.119 Uiso 1 calc R . C41 C 0.3145(2) 0.6244(3) 0.0213(3) 0.0638(12) Uani 1 d . . C42 C 0.3016(3) 0.5393(3) 0.0220(3) 0.0785(14) Uani 1 d . . H42 H 0.3203(3) 0.5048(3) 0.0582(3) 0.094 Uiso 1 calc R . C43 C 0.2614(3) 0.5042(3) -0.0301(3) 0.092(2) Uani 1 d . . H43 H 0.2524(3) 0.4461(3) -0.0287(3) 0.111 Uiso 1 calc R . C44 C 0.2343(3) 0.5533(4) -0.0841(3) 0.108(2) Uani 1 d . . H44 H 0.2075(3) 0.5292(4) -0.1203(3) 0.129 Uiso 1 calc R . C45 C 0.2473(4) 0.6386(4) -0.0843(4) 0.132(3) Uani 1 d . . H45 H 0.2283(4) 0.6729(4) -0.1205(4) 0.158 Uiso 1 calc R . C46 C 0.2874(3) 0.6746(3) -0.0326(3) 0.103(2) Uani 1 d . . H46 H 0.2962(3) 0.7327(3) -0.0340(3) 0.124 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 Ru 0.0653(3) 0.0550(3) 0.0765(4) 0.000 -0.0128(3) 0.000 S1 0.0759(8) 0.0720(9) 0.0755(9) -0.0113(7) -0.0154(7) 0.0129(7) C1 0.062(3) 0.049(3) 0.084(4) 0.006(3) -0.008(3) -0.004(2) C2 0.087(4) 0.065(3) 0.083(4) 0.012(3) -0.006(3) 0.003(3) N1 0.116(4) 0.087(3) 0.099(4) 0.023(3) -0.021(3) 0.009(3) S2 0.0776(8) 0.0602(7) 0.0756(9) -0.0084(7) -0.0042(7) -0.0029(6) C3 0.064(3) 0.040(2) 0.087(4) 0.007(2) -0.003(3) -0.002(2) C4 0.097(4) 0.049(3) 0.102(4) 0.006(3) 0.003(3) 0.008(3) N2 0.151(5) 0.092(4) 0.136(5) 0.006(3) 0.008(4) 0.053(4) S3 0.0810(9) 0.0715(9) 0.1012(11) -0.0085(8) -0.0175(8) 0.0171(7) C5 0.091(4) 0.056(3) 0.112(6) -0.009(3) -0.047(3) 0.008(3) C6 0.134(6) 0.076(4) 0.181(8) -0.019(5) -0.069(5) 0.027(4) N3 0.202(7) 0.094(5) 0.280(10) -0.052(5) -0.073(7) 0.063(5) As 0.0673(3) 0.0529(3) 0.0638(3) 0.0008(2) 0.0082(2) 0.0039(3) C11 0.062(3) 0.051(3) 0.074(3) 0.001(2) 0.008(3) 0.001(2) C12 0.078(4) 0.094(4) 0.156(6) 0.039(4) 0.036(4) 0.018(3) C13 0.096(4) 0.103(5) 0.167(7) 0.051(5) 0.024(5) 0.034(4) C14 0.081(4) 0.090(4) 0.117(5) 0.008(4) -0.006(4) 0.024(4) C15 0.070(4) 0.131(6) 0.157(6) 0.027(5) 0.028(4) 0.017(4) C16 0.081(4) 0.093(4) 0.129(5) 0.038(4) 0.013(4) -0.005(4) C21 0.074(3) 0.048(3) 0.060(3) -0.002(2) 0.006(3) 0.009(2) C22 0.088(4) 0.089(4) 0.078(4) -0.005(3) -0.004(3) 0.000(3) C23 0.133(6) 0.099(5) 0.059(4) -0.002(3) 0.004(4) 0.020(4) C24 0.128(5) 0.071(4) 0.078(4) 0.012(3) 0.041(4) 0.021(4) C25 0.086(4) 0.066(3) 0.104(5) 0.012(3) 0.034(4) 0.017(3) C26 0.073(3) 0.062(3) 0.066(3) -0.003(2) 0.007(3) 0.005(3) C31 0.075(3) 0.053(3) 0.063(3) 0.002(2) 0.004(3) -0.001(2) C32 0.094(4) 0.061(3) 0.083(4) 0.001(3) 0.004(3) 0.008(3) C33 0.141(6) 0.068(4) 0.083(4) -0.002(3) -0.015(4) 0.018(4) C34 0.144(6) 0.058(4) 0.113(6) 0.007(4) -0.026(5) -0.010(4) C35 0.152(6) 0.077(4) 0.113(5) 0.025(4) 0.018(5) -0.023(4) C36 0.126(5) 0.070(4) 0.101(4) 0.005(3) 0.029(4) -0.002(3) C41 0.076(3) 0.054(3) 0.061(3) -0.001(2) 0.006(2) 0.009(2) C42 0.104(4) 0.065(3) 0.066(3) -0.002(3) -0.009(3) 0.010(3) C43 0.134(5) 0.063(3) 0.080(4) -0.010(3) -0.012(4) 0.005(4) C44 0.145(6) 0.084(4) 0.094(5) -0.017(4) -0.042(4) 0.008(4) C45 0.206(8) 0.079(4) 0.110(5) 0.008(4) -0.065(6) 0.013(5) C46 0.163(6) 0.055(3) 0.092(4) 0.001(3) -0.039(4) 0.001(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 Ru S3 2.3349(14) 7_656 ? Ru S3 2.3349(14) . ? Ru S1 2.3419(13) . ? Ru S1 2.3419(13) 7_656 ? Ru S2 2.3512(13) 7_656 ? Ru S2 2.3512(13) . ? S1 C1 1.720(5) . ? C1 C3 1.369(6) . ? C1 C2 1.427(7) . ? C2 N1 1.130(6) . ? S2 C3 1.722(5) . ? C3 C4 1.424(7) . ? C4 N2 1.131(6) . ? S3 C5 1.725(5) . ? C5 C5 1.349(11) 7_656 ? C5 C6 1.441(8) . ? C6 N3 1.135(7) . ? As C21 1.895(4) . ? As C41 1.897(5) . ? As C11 1.911(4) . ? As C31 1.911(5) . ? C11 C16 1.338(6) . ? C11 C12 1.346(7) . ? C12 C13 1.387(7) . ? C12 H12 0.93 . ? C13 C14 1.341(7) . ? C13 H13 0.93 . ? C14 C15 1.330(7) . ? C14 H14 0.93 . ? C15 C16 1.401(7) . ? C15 H15 0.93 . ? C16 H16 0.93 . ? C21 C22 1.365(6) . ? C21 C26 1.377(6) . ? C22 C23 1.392(7) . ? C22 H22 0.93 . ? C23 C24 1.359(8) . ? C23 H23 0.93 . ? C24 C25 1.369(8) . ? C24 H24 0.93 . ? C25 C26 1.368(6) . ? C25 H25 0.93 . ? C26 H26 0.93 . ? C31 C32 1.345(6) . ? C31 C36 1.357(6) . ? C32 C33 1.392(7) . ? C32 H32 0.93 . ? C33 C34 1.341(8) . ? C33 H33 0.93 . ? C34 C35 1.331(8) . ? C34 H34 0.93 . ? C35 C36 1.413(7) . ? C35 H35 0.93 . ? C36 H36 0.93 . ? C41 C42 1.360(6) . ? C41 C46 1.366(6) . ? C42 C43 1.362(6) . ? C42 H42 0.93 . ? C43 C44 1.358(7) . ? C43 H43 0.93 . ? C44 C45 1.362(8) . ? C44 H44 0.93 . ? C45 C46 1.363(8) . ? C45 H45 0.93 . ? C46 H46 0.93 . ? 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 S3 Ru S3 86.22(8) 7_656 . ? S3 Ru S1 103.02(5) 7_656 . ? S3 Ru S1 84.38(5) . . ? S3 Ru S1 84.38(5) 7_656 7_656 ? S3 Ru S1 103.02(5) . 7_656 ? S1 Ru S1 169.99(7) . 7_656 ? S3 Ru S2 169.18(4) 7_656 7_656 ? S3 Ru S2 89.96(5) . 7_656 ? S1 Ru S2 86.65(5) . 7_656 ? S1 Ru S2 86.63(5) 7_656 7_656 ? S3 Ru S2 89.96(5) 7_656 . ? S3 Ru S2 169.18(4) . . ? S1 Ru S2 86.63(5) . . ? S1 Ru S2 86.65(5) 7_656 . ? S2 Ru S2 95.53(6) 7_656 . ? C1 S1 Ru 103.9(2) . . ? C3 C1 C2 120.7(4) . . ? C3 C1 S1 122.6(4) . . ? C2 C1 S1 116.7(4) . . ? N1 C2 C1 179.0(6) . . ? C3 S2 Ru 103.7(2) . . ? C1 C3 C4 119.9(5) . . ? C1 C3 S2 122.4(4) . . ? C4 C3 S2 117.7(4) . . ? N2 C4 C3 178.3(7) . . ? C5 S3 Ru 104.6(2) . . ? C5 C5 C6 121.3(4) 7_656 . ? C5 C5 S3 122.2(2) 7_656 . ? C6 C5 S3 116.5(5) . . ? N3 C6 C5 178.8(9) . . ? C21 As C41 107.1(2) . . ? C21 As C11 108.8(2) . . ? C41 As C11 108.0(2) . . ? C21 As C31 108.3(2) . . ? C41 As C31 111.1(2) . . ? C11 As C31 113.2(2) . . ? C16 C11 C12 118.7(5) . . ? C16 C11 As 122.9(4) . . ? C12 C11 As 118.3(4) . . ? C11 C12 C13 120.7(5) . . ? C11 C12 H12 119.6(3) . . ? C13 C12 H12 119.6(4) . . ? C14 C13 C12 120.2(6) . . ? C14 C13 H13 119.9(4) . . ? C12 C13 H13 119.9(4) . . ? C15 C14 C13 119.6(6) . . ? C15 C14 H14 120.2(4) . . ? C13 C14 H14 120.2(4) . . ? C14 C15 C16 120.2(6) . . ? C14 C15 H15 119.9(4) . . ? C16 C15 H15 119.9(4) . . ? C11 C16 C15 120.5(5) . . ? C11 C16 H16 119.8(3) . . ? C15 C16 H16 119.8(4) . . ? C22 C21 C26 119.7(5) . . ? C22 C21 As 120.6(4) . . ? C26 C21 As 119.6(4) . . ? C21 C22 C23 120.3(5) . . ? C21 C22 H22 119.9(3) . . ? C23 C22 H22 119.9(4) . . ? C24 C23 C22 118.9(6) . . ? C24 C23 H23 120.6(4) . . ? C22 C23 H23 120.6(4) . . ? C23 C24 C25 121.3(5) . . ? C23 C24 H24 119.4(4) . . ? C25 C24 H24 119.4(4) . . ? C26 C25 C24 119.5(5) . . ? C26 C25 H25 120.2(4) . . ? C24 C25 H25 120.2(4) . . ? C25 C26 C21 120.2(5) . . ? C25 C26 H26 119.9(4) . . ? C21 C26 H26 119.9(3) . . ? C32 C31 C36 119.7(5) . . ? C32 C31 As 119.0(4) . . ? C36 C31 As 121.2(4) . . ? C31 C32 C33 120.6(5) . . ? C31 C32 H32 119.7(3) . . ? C33 C32 H32 119.7(4) . . ? C34 C33 C32 119.5(6) . . ? C34 C33 H33 120.2(4) . . ? C32 C33 H33 120.2(4) . . ? C35 C34 C33 120.9(6) . . ? C35 C34 H34 119.6(4) . . ? C33 C34 H34 119.6(4) . . ? C34 C35 C36 120.1(6) . . ? C34 C35 H35 120.0(4) . . ? C36 C35 H35 120.0(4) . . ? C31 C36 C35 119.0(5) . . ? C31 C36 H36 120.5(3) . . ? C35 C36 H36 120.5(4) . . ? C42 C41 C46 119.6(5) . . ? C42 C41 As 118.9(4) . . ? C46 C41 As 121.5(4) . . ? C41 C42 C43 120.3(5) . . ? C41 C42 H42 119.8(3) . . ? C43 C42 H42 119.8(3) . . ? C44 C43 C42 120.7(5) . . ? C44 C43 H43 119.7(3) . . ? C42 C43 H43 119.7(3) . . ? C43 C44 C45 118.6(6) . . ? C43 C44 H44 120.7(3) . . ? C45 C44 H44 120.7(4) . . ? C44 C45 C46 121.4(6) . . ? C44 C45 H45 119.3(4) . . ? C46 C45 H45 119.3(4) . . ? C45 C46 C41 119.4(5) . . ? C45 C46 H46 120.3(4) . . ? C41 C46 H46 120.3(3) . . ? _refine_diff_density_max 0.283 _refine_diff_density_min -0.411 _refine_diff_density_rms 0.057 data_la9804 _audit_creation_method SHELXL _chemical_name_systematic ; (Et4N)2[Ru(mnd)2].0.5H2O ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C32 H41 N10 O0.50 Ru S6' _chemical_formula_weight 867.18 _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' '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' _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 13.1816(15) _cell_length_b 27.145(5) _cell_length_c 12.767(3) _cell_angle_alpha 90.00 _cell_angle_beta 111.319(10) _cell_angle_gamma 90.00 _cell_volume 4255.6(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 14 _exptl_crystal_description plate-like _exptl_crystal_colour brown _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.353 _exptl_crystal_density_method ? _exptl_crystal_F_000 1788 _exptl_absorpt_coefficient_mu 0.699 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4206 _exptl_absorpt_correction_T_max 1.0000 _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 'Enraf-Nonius CAD4' _diffrn_measurement_method '\w/2\q' _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 7790 _diffrn_reflns_av_R_equivalents 0.0585 _diffrn_reflns_av_sigmaI/netI 0.0626 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7448 _reflns_number_observed 4794 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4-ARGUS (Enraf-Nonius, 1994)' _computing_cell_refinement 'CAD4-ARGUS (Enraf-Nonius, 1994)' _computing_data_reduction ; Chi90s (Boyle, 1996), Xcad4 (Harms, 1996), SHELXTL_V5 (Siemens, 1994) ; _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ; ORTEP-III (Farrugia, Burnett, Johnson, 1996) ; _computing_publication_material 'SHELXTL_V5 (Siemens, 1994)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 4 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^)+(0.1167P)^2^+3.2582P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment ; Ethyl hydrogen atoms were refined with idealized riding models and those of water were refines isotropically with bond length restraints. ; _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7444 _refine_ls_number_parameters 506 _refine_ls_number_restraints 372 _refine_ls_R_factor_all 0.1077 _refine_ls_R_factor_obs 0.0705 _refine_ls_wR_factor_all 0.2184 _refine_ls_wR_factor_obs 0.1907 _refine_ls_goodness_of_fit_all 1.065 _refine_ls_goodness_of_fit_obs 1.195 _refine_ls_restrained_S_all 1.076 _refine_ls_restrained_S_obs 1.178 _refine_ls_shift/esd_max -0.005 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ru Ru 0.66745(5) 0.78033(2) 0.37648(5) 0.0524(2) Uani 1 d . . S1 S 0.7911(2) 0.71466(8) 0.4246(2) 0.0668(5) Uani 1 d . . S2 S 0.54206(14) 0.72961(7) 0.41054(14) 0.0539(4) Uani 1 d . . S3 S 0.5886(2) 0.75891(8) 0.18731(15) 0.0653(5) Uani 1 d . . S4 S 0.5426(2) 0.84590(7) 0.3393(2) 0.0634(5) Uani 1 d . . S5 S 0.7412(2) 0.80679(7) 0.56153(15) 0.0603(5) Uani 1 d . . S6 S 0.7997(2) 0.82674(8) 0.3385(2) 0.0695(5) Uani 1 d . . C1 C 0.7218(6) 0.6718(3) 0.4677(6) 0.060(2) Uani 1 d . . C2 C 0.7849(7) 0.6270(4) 0.5169(8) 0.086(3) Uani 1 d . . N1 N 0.8354(7) 0.5941(3) 0.5574(8) 0.114(3) Uani 1 d . . C3 C 0.6158(6) 0.6751(3) 0.4629(6) 0.060(2) Uani 1 d . . C4 C 0.5629(7) 0.6365(3) 0.4971(7) 0.077(2) Uani 1 d . . N2 N 0.5170(7) 0.6067(3) 0.5233(8) 0.113(3) Uani 1 d . . C5 C 0.4583(5) 0.7104(3) 0.2763(6) 0.056(2) Uani 1 d . . C6 C 0.3645(7) 0.6826(3) 0.2661(7) 0.076(2) Uani 1 d . . N3 N 0.2875(7) 0.6607(4) 0.2615(8) 0.114(3) Uani 1 d . . C7 C 0.4802(6) 0.7233(3) 0.1832(6) 0.059(2) Uani 1 d . . C8 C 0.4082(7) 0.7085(3) 0.0751(6) 0.073(2) Uani 1 d . . N4 N 0.3498(7) 0.6976(4) -0.0120(7) 0.106(3) Uani 1 d . . C9 C 0.5696(6) 0.8693(3) 0.4704(6) 0.060(2) Uani 1 d . . C10 C 0.4965(8) 0.9080(4) 0.4777(7) 0.081(2) Uani 1 d . . N5 N 0.4368(8) 0.9383(4) 0.4816(9) 0.131(4) Uani 1 d . . C11 C 0.6509(6) 0.8553(3) 0.5656(6) 0.063(2) Uani 1 d . . C12 C 0.6680(8) 0.8781(4) 0.6694(7) 0.087(3) Uani 1 d . . N6 N 0.6792(10) 0.8959(4) 0.7538(7) 0.148(4) Uani 1 d . . C13 C 0.8575(6) 0.8407(3) 0.5650(6) 0.066(2) Uani 1 d . . C14 C 0.9272(8) 0.8587(4) 0.6719(9) 0.095(3) Uani 1 d . . N7 N 0.9825(9) 0.8730(4) 0.7570(8) 0.147(4) Uani 1 d . . C15 C 0.8764(6) 0.8477(3) 0.4672(8) 0.071(2) Uani 1 d . . C16 C 0.9706(8) 0.8762(3) 0.4736(9) 0.088(3) Uani 1 d . . N8 N 1.0451(7) 0.8969(4) 0.4739(9) 0.123(3) Uani 1 d . . O O 0.0237(37) 0.0086(20) 0.0415(35) 0.344(22) Uiso 0.50 d PD . H1 H 0.0237(37) 0.0086(20) 0.0415(35) 0.413 Uiso 0.50 d P . H2 H -0.0244(208) 0.0403(117) 0.0559(209) 0.413 Uiso 0.50 d PD . N9 N 0.7156(6) 0.0031(2) 0.2766(6) 0.080(2) Uani 1 d DU . C21 C 0.8103(11) 0.0372(5) 0.2992(12) 0.104(5) Uani 0.733(9) d PDU 1 H21A H 0.8208(11) 0.0552(5) 0.3679(12) 0.125 Uiso 0.733(9) calc PR 1 H21B H 0.7931(11) 0.0610(5) 0.2384(12) 0.125 Uiso 0.733(9) calc PR 1 C22 C 0.9173(15) 0.0113(10) 0.3106(22) 0.129(7) Uani 0.733(9) d PDU 1 H22A H 0.9774(15) 0.0290(10) 0.3628(22) 0.193 Uiso 0.733(9) calc PR 1 H22B H 0.9248(15) 0.0102(10) 0.2386(22) 0.193 Uiso 0.733(9) calc PR 1 H22C H 0.9165(15) -0.0217(10) 0.3375(22) 0.193 Uiso 0.733(9) calc PR 1 C23 C 0.6148(10) 0.0348(5) 0.2706(11) 0.105(5) Uani 0.733(9) d PDU 1 H23A H 0.6337(10) 0.0541(5) 0.3389(11) 0.126 Uiso 0.733(9) calc PR 1 H23B H 0.5989(10) 0.0576(5) 0.2082(11) 0.126 Uiso 0.733(9) calc PR 1 C24 C 0.5128(11) 0.0057(8) 0.2562(15) 0.115(6) Uani 0.733(9) d PDU 1 H24A H 0.4519(11) 0.0203(8) 0.1978(15) 0.172 Uiso 0.733(9) calc PR 1 H24B H 0.4998(11) 0.0059(8) 0.3255(15) 0.172 Uiso 0.733(9) calc PR 1 H24C H 0.5219(11) -0.0277(8) 0.2362(15) 0.172 Uiso 0.733(9) calc PR 1 C25 C 0.7368(10) -0.0344(5) 0.3723(11) 0.096(4) Uani 0.733(9) d PDU 1 H25A H 0.6714(10) -0.0540(5) 0.3574(11) 0.116 Uiso 0.733(9) calc PR 1 H25B H 0.7942(10) -0.0565(5) 0.3711(11) 0.116 Uiso 0.733(9) calc PR 1 C26 C 0.7683(32) -0.0131(12) 0.4872(18) 0.146(12) Uani 0.733(9) d PDU 1 H26A H 0.7779(32) -0.0392(12) 0.5408(18) 0.220 Uiso 0.733(9) calc PR 1 H26B H 0.7121(32) 0.0087(12) 0.4900(18) 0.220 Uiso 0.733(9) calc PR 1 H26C H 0.8352(32) 0.0048(12) 0.5050(18) 0.220 Uiso 0.733(9) calc PR 1 C27 C 0.6928(12) -0.0252(5) 0.1729(10) 0.109(5) Uani 0.733(9) d PDU 1 H27A H 0.6316(12) -0.0469(5) 0.1639(10) 0.131 Uiso 0.733(9) calc PR 1 H27B H 0.7553(12) -0.0460(5) 0.1817(10) 0.131 Uiso 0.733(9) calc PR 1 C28 C 0.6673(18) 0.0043(7) 0.0658(13) 0.125(6) Uani 0.733(9) d PDU 1 H28A H 0.6598(18) -0.0176(7) 0.0044(13) 0.188 Uiso 0.733(9) calc PR 1 H28B H 0.7254(18) 0.0271(7) 0.0744(13) 0.188 Uiso 0.733(9) calc PR 1 H28C H 0.6005(18) 0.0221(7) 0.0507(13) 0.188 Uiso 0.733(9) calc PR 1 C21A C 0.6162(20) -0.0301(11) 0.2510(27) 0.094(10) Uiso 0.267(9) d PDU 2 H21C H 0.6163(20) -0.0542(11) 0.1950(27) 0.113 Uiso 0.267(9) calc PR 2 H21D H 0.6214(20) -0.0477(11) 0.3188(27) 0.113 Uiso 0.267(9) calc PR 2 C22A C 0.5104(41) -0.0020(25) 0.2087(53) 0.143(23) Uiso 0.267(9) d PDU 2 H22D H 0.4649(41) -0.0126(25) 0.2485(53) 0.215 Uiso 0.267(9) calc PR 2 H22E H 0.4740(41) -0.0081(25) 0.1297(53) 0.215 Uiso 0.267(9) calc PR 2 H22F H 0.5248(41) 0.0326(25) 0.2208(53) 0.215 Uiso 0.267(9) calc PR 2 C23A C 0.7425(27) 0.0247(11) 0.3936(18) 0.098(10) Uiso 0.267(9) d PDU 2 H23C H 0.8098(27) 0.0430(11) 0.4112(18) 0.118 Uiso 0.267(9) calc PR 2 H23D H 0.6861(27) 0.0485(11) 0.3885(18) 0.118 Uiso 0.267(9) calc PR 2 C24A C 0.7553(73) -0.0079(23) 0.4940(43) 0.087(16) Uiso 0.267(9) d PDU 2 H24D H 0.6851(73) -0.0140(23) 0.4980(43) 0.131 Uiso 0.267(9) calc PR 2 H24E H 0.8010(73) 0.0083(23) 0.5615(43) 0.131 Uiso 0.267(9) calc PR 2 H24F H 0.7879(73) -0.0386(23) 0.4860(43) 0.131 Uiso 0.267(9) calc PR 2 C25A C 0.6969(30) 0.0416(11) 0.1904(24) 0.116(12) Uiso 0.267(9) d PDU 2 H25C H 0.7492(30) 0.0678(11) 0.2218(24) 0.139 Uiso 0.267(9) calc PR 2 H25D H 0.6250(30) 0.0553(11) 0.1751(24) 0.139 Uiso 0.267(9) calc PR 2 C26A C 0.7045(59) 0.0263(25) 0.0805(42) 0.143(24) Uiso 0.267(9) d PDU 2 H26D H 0.7735(59) 0.0364(25) 0.0785(42) 0.215 Uiso 0.267(9) calc PR 2 H26E H 0.6469(59) 0.0416(25) 0.0198(42) 0.215 Uiso 0.267(9) calc PR 2 H26F H 0.6979(59) -0.0089(25) 0.0731(42) 0.215 Uiso 0.267(9) calc PR 2 C27A C 0.8102(21) -0.0294(11) 0.2787(29) 0.102(11) Uiso 0.267(9) d PDU 2 H27C H 0.8336(21) -0.0492(11) 0.3466(29) 0.122 Uiso 0.267(9) calc PR 2 H27D H 0.7860(21) -0.0517(11) 0.2149(29) 0.122 Uiso 0.267(9) calc PR 2 C28A C 0.9047(58) 0.0003(35) 0.2746(77) 0.173(35) Uiso 0.267(9) d PDU 2 H28D H 0.9496(58) -0.0199(35) 0.2474(77) 0.259 Uiso 0.267(9) calc PR 2 H28E H 0.9468(58) 0.0120(35) 0.3487(77) 0.259 Uiso 0.267(9) calc PR 2 H28F H 0.8781(58) 0.0279(35) 0.2251(77) 0.259 Uiso 0.267(9) calc PR 2 N10 N 0.8435(6) 0.1683(4) 0.8697(7) 0.109(3) Uani 1 d DU . C31 C 0.9238(12) 0.1849(7) 0.9789(15) 0.118(6) Uani 0.662(12) d PDU 3 H31A H 0.9964(12) 0.1824(7) 0.9766(15) 0.142 Uiso 0.662(12) calc PR 3 H31B H 0.9204(12) 0.1631(7) 1.0377(15) 0.142 Uiso 0.662(12) calc PR 3 C32 C 0.9053(21) 0.2373(10) 1.0083(30) 0.249(19) Uani 0.662(12) d PDU 3 H32A H 0.9729(21) 0.2550(10) 1.0319(30) 0.373 Uiso 0.662(12) calc PR 3 H32B H 0.8775(21) 0.2370(10) 1.0681(30) 0.373 Uiso 0.662(12) calc PR 3 H32C H 0.8537(21) 0.2531(10) 0.9435(30) 0.373 Uiso 0.662(12) calc PR 3 C33 C 0.8722(19) 0.1169(9) 0.8579(23) 0.193(10) Uani 0.662(12) d PDU 3 H33A H 0.8569(19) 0.0961(9) 0.9123(23) 0.232 Uiso 0.662(12) calc PR 3 H33B H 0.9489(19) 0.1141(9) 0.8696(23) 0.232 Uiso 0.662(12) calc PR 3 C34 C 0.8002(18) 0.1013(11) 0.7352(21) 0.331(15) Uani 0.662(12) d PDU 3 H34A H 0.7429(18) 0.0799(11) 0.7372(21) 0.496 Uiso 0.662(12) calc PR 3 H34B H 0.8445(18) 0.0843(11) 0.7014(21) 0.496 Uiso 0.662(12) calc PR 3 H34C H 0.7691(18) 0.1301(11) 0.6918(21) 0.496 Uiso 0.662(12) calc PR 3 C35 C 0.8477(22) 0.2049(12) 0.7787(24) 0.203(10) Uani 0.662(12) d PDU 3 H35A H 0.7907(22) 0.1969(12) 0.7076(24) 0.244 Uiso 0.662(12) calc PR 3 H35B H 0.8343(22) 0.2380(12) 0.7994(24) 0.244 Uiso 0.662(12) calc PR 3 C36 C 0.9584(21) 0.2034(14) 0.7648(23) 0.325(13) Uani 0.662(12) d PDU 3 H36A H 1.0131(21) 0.2172(14) 0.8303(23) 0.488 Uiso 0.662(12) calc PR 3 H36B H 0.9546(21) 0.2222(14) 0.6997(23) 0.488 Uiso 0.662(12) calc PR 3 H36C H 0.9768(21) 0.1699(14) 0.7556(23) 0.488 Uiso 0.662(12) calc PR 3 C37 C 0.7333(14) 0.1725(11) 0.8688(20) 0.169(9) Uani 0.662(12) d PDU 3 H37A H 0.6809(14) 0.1604(11) 0.7983(20) 0.202 Uiso 0.662(12) calc PR 3 H37B H 0.7161(14) 0.2064(11) 0.8791(20) 0.202 Uiso 0.662(12) calc PR 3 C38 C 0.7326(21) 0.1416(13) 0.9638(26) 0.341(14) Uani 0.662(12) d PDU 3 H38A H 0.6659(21) 0.1232(13) 0.9418(26) 0.511 Uiso 0.662(12) calc PR 3 H38B H 0.7383(21) 0.1623(13) 1.0267(26) 0.511 Uiso 0.662(12) calc PR 3 H38C H 0.7932(21) 0.1192(13) 0.9846(26) 0.511 Uiso 0.662(12) calc PR 3 C31A C 0.9352(38) 0.1597(18) 0.8322(49) 0.200(14) Uiso 0.338(12) d PDU 4 H31C H 0.9202(38) 0.1304(18) 0.7855(49) 0.240 Uiso 0.338(12) calc PR 4 H31D H 1.0002(38) 0.1534(18) 0.8976(49) 0.240 Uiso 0.338(12) calc PR 4 C32A C 0.9584(21) 0.2034(14) 0.7648(23) 0.325(13) Uani 0.34 d PDU 4 H32D H 0.9837(37) 0.1908(11) 0.7084(45) 0.488 Uiso 0.338(12) calc PR 4 H32E H 1.0131(37) 0.2244(11) 0.8151(45) 0.488 Uiso 0.338(12) calc PR 4 H32F H 0.8927(37) 0.2219(11) 0.7294(45) 0.488 Uiso 0.338(12) calc PR 4 C33A C 0.8066(37) 0.2218(11) 0.8420(45) 0.154(13) Uiso 0.338(12) d PDU 4 H33C H 0.7640(37) 0.2253(11) 0.7624(45) 0.185 Uiso 0.338(12) calc PR 4 H33D H 0.7623(37) 0.2321(11) 0.8844(45) 0.185 Uiso 0.338(12) calc PR 4 C34A C 0.9090(45) 0.2526(23) 0.8740(63) 0.223(27) Uiso 0.338(12) d PDU 4 H34D H 0.9013(45) 0.2812(23) 0.9148(63) 0.334 Uiso 0.338(12) calc PR 4 H34E H 0.9206(45) 0.2628(23) 0.8072(63) 0.334 Uiso 0.338(12) calc PR 4 H34F H 0.9700(45) 0.2335(23) 0.9203(63) 0.334 Uiso 0.338(12) calc PR 4 C35A C 0.8553(30) 0.1400(20) 0.9754(33) 0.177(14) Uiso 0.338(12) d PDU 4 H35C H 0.9025(30) 0.1566(20) 1.0426(33) 0.212 Uiso 0.338(12) calc PR 4 H35D H 0.8808(30) 0.1066(20) 0.9736(33) 0.212 Uiso 0.338(12) calc PR 4 C36A C 0.7326(21) 0.1416(13) 0.9638(26) 0.341(14) Uani 0.34 d PDU 4 H36D H 0.7283(30) 0.1415(15) 1.0373(36) 0.511 Uiso 0.338(12) calc PR 4 H36E H 0.6954(30) 0.1132(15) 0.9227(36) 0.511 Uiso 0.338(12) calc PR 4 H36F H 0.6992(30) 0.1710(15) 0.9245(36) 0.511 Uiso 0.338(12) calc PR 4 C37A C 0.7572(30) 0.1411(15) 0.7803(36) 0.163(12) Uiso 0.338(12) d PDU 4 H37C H 0.7052(30) 0.1281(15) 0.8109(36) 0.196 Uiso 0.338(12) calc PR 4 H37D H 0.7187(30) 0.1637(15) 0.7201(36) 0.196 Uiso 0.338(12) calc PR 4 C38A C 0.8002(18) 0.1013(11) 0.7352(21) 0.331(15) Uani 0.34 d PDU 4 H38D H 0.7534(3984) 0.0953(3984) 0.6587(120) 0.496 Uiso 0.338(12) calc PR 4 H38E H 0.8042(3984) 0.0721(3984) 0.7790(120) 0.496 Uiso 0.338(12) calc PR 4 H38F H 0.8717(3984) 0.1097(3984) 0.7377(120) 0.496 Uiso 0.338(12) calc PR 4 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 Ru 0.0532(3) 0.0536(4) 0.0504(3) -0.0005(3) 0.0190(2) -0.0069(3) S1 0.0547(11) 0.0650(13) 0.0813(13) 0.0059(10) 0.0255(10) -0.0012(9) S2 0.0554(10) 0.0563(11) 0.0529(9) 0.0005(8) 0.0230(8) -0.0023(8) S3 0.0678(12) 0.0812(14) 0.0498(9) -0.0057(9) 0.0247(9) -0.0071(10) S4 0.0662(12) 0.0617(12) 0.0583(10) 0.0012(9) 0.0179(9) 0.0023(9) S5 0.0625(11) 0.0586(12) 0.0553(10) 0.0017(8) 0.0159(8) -0.0053(9) S6 0.0681(12) 0.0721(14) 0.0739(12) 0.0022(10) 0.0325(10) -0.0156(10) C1 0.067(5) 0.051(4) 0.056(4) 0.006(3) 0.016(3) 0.000(4) C2 0.066(5) 0.072(6) 0.106(7) 0.006(5) 0.014(5) -0.005(5) N1 0.083(5) 0.097(6) 0.154(8) 0.061(6) 0.033(5) 0.030(5) C3 0.063(5) 0.053(4) 0.058(4) 0.006(3) 0.017(3) -0.008(3) C4 0.064(5) 0.073(6) 0.089(6) 0.015(5) 0.021(4) -0.001(4) N2 0.095(6) 0.098(6) 0.142(8) 0.053(6) 0.040(5) -0.013(5) C5 0.051(4) 0.050(4) 0.069(4) -0.006(3) 0.025(3) -0.003(3) C6 0.062(5) 0.077(6) 0.085(6) -0.008(5) 0.022(4) -0.011(5) N3 0.083(6) 0.116(7) 0.144(8) -0.004(6) 0.043(5) -0.030(5) C7 0.060(4) 0.061(5) 0.057(4) -0.006(3) 0.021(3) 0.004(4) C8 0.067(5) 0.095(6) 0.053(4) -0.016(4) 0.018(4) -0.001(4) N4 0.087(6) 0.143(8) 0.075(5) -0.022(5) 0.014(4) -0.017(5) C9 0.061(4) 0.056(5) 0.065(4) -0.002(3) 0.026(4) 0.002(4) C10 0.088(6) 0.075(6) 0.079(6) 0.003(5) 0.032(5) -0.003(5) N5 0.128(8) 0.142(9) 0.135(8) -0.013(7) 0.063(7) 0.045(7) C11 0.078(5) 0.052(4) 0.062(4) -0.004(3) 0.028(4) -0.006(4) C12 0.119(8) 0.079(6) 0.068(5) 0.001(5) 0.040(5) 0.019(5) N6 0.234(13) 0.131(9) 0.069(5) -0.009(6) 0.042(7) 0.043(9) C13 0.053(4) 0.064(5) 0.070(5) 0.002(4) 0.010(4) -0.011(4) C14 0.093(7) 0.080(7) 0.093(7) -0.005(5) 0.012(6) -0.025(5) N7 0.145(9) 0.172(10) 0.092(6) -0.030(7) 0.003(6) -0.073(8) C15 0.050(4) 0.059(5) 0.098(6) 0.004(4) 0.019(4) -0.008(4) C16 0.076(6) 0.071(6) 0.111(7) -0.006(5) 0.027(5) -0.024(5) N8 0.094(6) 0.114(8) 0.157(9) -0.006(6) 0.041(6) -0.041(6) N9 0.088(5) 0.057(4) 0.086(5) -0.007(3) 0.022(4) 0.000(4) C21 0.126(11) 0.066(8) 0.119(11) -0.003(7) 0.042(9) -0.029(8) C22 0.088(11) 0.177(21) 0.127(16) -0.021(14) 0.046(11) -0.009(11) C23 0.117(11) 0.089(10) 0.100(9) -0.019(7) 0.028(8) 0.053(9) C24 0.066(9) 0.162(16) 0.106(12) -0.024(12) 0.018(8) 0.015(9) C25 0.084(8) 0.076(8) 0.122(11) 0.017(8) 0.029(8) 0.014(7) C26 0.137(19) 0.220(25) 0.084(11) -0.008(12) 0.042(11) 0.050(16) C27 0.107(10) 0.102(11) 0.105(10) -0.025(8) 0.021(8) 0.017(8) C28 0.164(18) 0.122(16) 0.078(9) 0.001(9) 0.030(10) -0.003(14) N10 0.067(5) 0.162(9) 0.088(5) 0.013(6) 0.017(4) 0.021(5) C31 0.071(9) 0.127(14) 0.133(13) -0.026(11) 0.008(9) 0.000(9) C32 0.172(23) 0.219(29) 0.310(39) -0.193(29) 0.034(24) -0.004(21) C33 0.124(15) 0.196(19) 0.237(20) -0.097(17) 0.040(15) 0.002(15) C34 0.201(19) 0.395(31) 0.272(24) -0.129(23) -0.063(18) 0.027(22) C35 0.162(18) 0.279(22) 0.176(19) 0.037(19) 0.069(16) 0.050(18) C36 0.302(26) 0.470(33) 0.247(24) 0.075(24) 0.151(21) -0.029(27) C37 0.085(12) 0.223(22) 0.167(18) -0.023(17) 0.009(12) 0.027(14) C38 0.208(21) 0.493(35) 0.357(29) 0.100(28) 0.145(20) -0.051(23) C32A 0.302(26) 0.470(33) 0.247(24) 0.075(24) 0.151(21) -0.029(27) C36A 0.208(21) 0.493(35) 0.357(29) 0.100(28) 0.145(20) -0.051(23) C38A 0.201(19) 0.395(31) 0.272(24) -0.129(23) -0.063(18) 0.027(22) _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 Ru S2 2.311(2) . ? Ru S5 2.318(2) . ? Ru S3 2.329(2) . ? Ru S6 2.341(2) . ? Ru S1 2.341(2) . ? Ru S4 2.352(2) . ? S1 C1 1.690(8) . ? S2 C5 1.747(7) . ? S2 C3 1.763(7) . ? S3 C7 1.710(8) . ? S4 C9 1.702(7) . ? S5 C13 1.775(8) . ? S5 C11 1.788(8) . ? S6 C15 1.685(9) . ? C1 C3 1.379(10) . ? C1 C2 1.477(12) . ? C2 N1 1.122(11) . ? C3 C4 1.412(11) . ? C4 N2 1.132(10) . ? C5 C7 1.368(10) . ? C5 C6 1.414(11) . ? C6 N3 1.158(11) . ? C7 C8 1.420(10) . ? C8 N4 1.138(10) . ? C9 C11 1.350(10) . ? C9 C10 1.451(12) . ? C10 N5 1.152(12) . ? C11 C12 1.404(11) . ? C12 N6 1.142(11) . ? C13 C15 1.373(11) . ? C13 C14 1.426(12) . ? C14 N7 1.135(11) . ? C15 C16 1.439(12) . ? C16 N8 1.131(11) . ? O O 1.12(7) 3 ? N9 C27 1.464(13) . ? N9 C25A 1.47(2) . ? N9 C21 1.497(13) . ? N9 C27A 1.52(2) . ? N9 C23A 1.52(2) . ? N9 C21A 1.52(2) . ? N9 C25 1.535(13) . ? N9 C23 1.562(12) . ? C21 C22 1.54(2) . ? C23 C24 1.51(2) . ? C25 C26 1.49(2) . ? C27 C28 1.51(2) . ? C21A C22A 1.51(3) . ? C23A C24A 1.52(3) . ? C25A C26A 1.50(3) . ? C27A C28A 1.50(3) . ? N10 C37 1.45(2) . ? N10 C33 1.47(2) . ? N10 C31A 1.47(3) . ? N10 C31 1.48(2) . ? N10 C37A 1.48(3) . ? N10 C35A 1.51(3) . ? N10 C33A 1.53(3) . ? N10 C35 1.54(2) . ? C31 C32 1.51(2) . ? C33 C34 1.57(2) . ? C35 C36 1.53(2) . ? C37 C38 1.48(2) . ? C31A C32A 1.56(3) . ? C33A C34A 1.51(3) . ? C35A C36A 1.57(3) . ? C37A C38A 1.43(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 S2 Ru S5 93.23(7) . . ? S2 Ru S3 88.08(7) . . ? S5 Ru S3 176.23(8) . . ? S2 Ru S6 175.96(8) . . ? S5 Ru S6 88.66(7) . . ? S3 Ru S6 90.26(7) . . ? S2 Ru S1 88.51(7) . . ? S5 Ru S1 88.54(7) . . ? S3 Ru S1 95.03(8) . . ? S6 Ru S1 87.96(8) . . ? S2 Ru S4 89.60(7) . . ? S5 Ru S4 88.54(7) . . ? S3 Ru S4 87.93(7) . . ? S6 Ru S4 94.02(8) . . ? S1 Ru S4 176.43(7) . . ? C1 S1 Ru 101.7(3) . . ? C5 S2 C3 100.7(3) . . ? C5 S2 Ru 103.5(2) . . ? C3 S2 Ru 103.8(3) . . ? C7 S3 Ru 103.0(2) . . ? C9 S4 Ru 101.7(3) . . ? C13 S5 C11 101.3(4) . . ? C13 S5 Ru 103.0(3) . . ? C11 S5 Ru 102.8(3) . . ? C15 S6 Ru 102.0(3) . . ? C3 C1 C2 118.5(7) . . ? C3 C1 S1 126.8(6) . . ? C2 C1 S1 114.6(6) . . ? N1 C2 C1 177.5(10) . . ? C1 C3 C4 122.9(7) . . ? C1 C3 S2 118.8(5) . . ? C4 C3 S2 118.3(6) . . ? N2 C4 C3 177.4(10) . . ? C7 C5 C6 120.7(7) . . ? C7 C5 S2 121.2(5) . . ? C6 C5 S2 118.0(6) . . ? N3 C6 C5 177.3(10) . . ? C5 C7 C8 119.6(7) . . ? C5 C7 S3 123.8(6) . . ? C8 C7 S3 116.5(6) . . ? N4 C8 C7 178.6(11) . . ? C11 C9 C10 118.3(7) . . ? C11 C9 S4 126.5(6) . . ? C10 C9 S4 115.2(6) . . ? N5 C10 C9 178.6(11) . . ? C9 C11 C12 121.9(8) . . ? C9 C11 S5 120.0(6) . . ? C12 C11 S5 118.1(6) . . ? N6 C12 C11 178.0(13) . . ? C15 C13 C14 123.8(8) . . ? C15 C13 S5 119.4(6) . . ? C14 C13 S5 116.9(7) . . ? N7 C14 C13 179.9(13) . . ? C13 C15 C16 117.5(8) . . ? C13 C15 S6 126.7(6) . . ? C16 C15 S6 115.8(7) . . ? N8 C16 C15 176.2(12) . . ? C27 N9 C21 112.5(9) . . ? C25A N9 C27A 109.8(16) . . ? C25A N9 C23A 112.1(16) . . ? C27A N9 C23A 108.0(15) . . ? C25A N9 C21A 111.2(16) . . ? C27A N9 C21A 107.3(15) . . ? C23A N9 C21A 108.3(15) . . ? C27 N9 C25 106.9(9) . . ? C21 N9 C25 111.1(8) . . ? C27 N9 C23 110.7(8) . . ? C21 N9 C23 107.6(8) . . ? C25 N9 C23 108.0(8) . . ? N9 C21 C22 114.0(12) . . ? C24 C23 N9 114.8(11) . . ? C26 C25 N9 115.6(14) . . ? N9 C27 C28 116.4(12) . . ? C22A C21A N9 113.0(34) . . ? C24A C23A N9 121.3(33) . . ? N9 C25A C26A 116.9(35) . . ? C28A C27A N9 111.9(44) . . ? C37 N10 C33 111.5(18) . . ? C37 N10 C31 110.8(13) . . ? C33 N10 C31 105.3(13) . . ? C31A N10 C37A 99.3(31) . . ? C31A N10 C35A 112.3(25) . . ? C37A N10 C35A 103.5(30) . . ? C31A N10 C33A 107.7(28) . . ? C37A N10 C33A 101.8(26) . . ? C35A N10 C33A 127.6(31) . . ? C37 N10 C35 104.6(16) . . ? C33 N10 C35 117.0(19) . . ? C31 N10 C35 107.6(16) . . ? N10 C31 C32 113.3(16) . . ? N10 C33 C34 106.0(19) . . ? C36 C35 N10 111.4(19) . . ? N10 C37 C38 104.7(17) . . ? N10 C31A C32A 114.1(27) . . ? C34A C33A N10 106.5(36) . . ? N10 C35A C36A 97.7(21) . . ? C38A C37A N10 112.3(27) . . ? _refine_diff_density_max 0.854 _refine_diff_density_min -0.679 _refine_diff_density_rms 0.101 data_la9801 _audit_creation_method SHELXL _chemical_name_systematic ; (Et4N)3[Ru(dithiolate)3].2CH3CN ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C40 H66 N11 Ru S6' _chemical_formula_weight 994.47 _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' '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' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'P-62c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x, y, -z+1/2' '-y, x-y, -z+1/2' '-x+y, -x, -z+1/2' 'y, x, -z' 'x-y, -y, -z' '-x, -x+y, -z' 'y, x, z+1/2' 'x-y, -y, z+1/2' '-x, -x+y, z+1/2' _cell_length_a 13.494(2) _cell_length_b 13.494(2) _cell_length_c 16.834(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2654.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15 _cell_measurement_theta_max 16 _exptl_crystal_description block-shaped _exptl_crystal_colour black _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.244 _exptl_crystal_density_method ? _exptl_crystal_F_000 1046 _exptl_absorpt_coefficient_mu 0.569 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8174 _exptl_absorpt_correction_T_max 1.0000 _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 'Enraf-Nonius CAD4' _diffrn_measurement_method '\w/2q' _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 1797 _diffrn_reflns_av_R_equivalents 0.0157 _diffrn_reflns_av_sigmaI/netI 0.0203 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -4 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 24.97 _reflns_number_total 916 _reflns_number_observed 830 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4 (Enraf-Nonius, 1977)' _computing_cell_refinement 'CAD4 (Enraf-Nonius, 1977)' _computing_data_reduction ; XCAD4 (Harms, 1996) SHELXTL-V5 (Siemens, 1994) ; _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP-III (Burnett & Johnson, 1996)' _computing_publication_material 'SHELXTL-V5 (Siemens, 1994)' _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^)+(0.0354P)^2^+0.4181P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment ; Ammonium hydrogen atoms were refined with idealized riding models, those of acetonitrile refined isotropically without a restraint. ; _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(7) _refine_ls_number_reflns 916 _refine_ls_number_parameters 100 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0252 _refine_ls_R_factor_obs 0.0219 _refine_ls_wR_factor_all 0.0589 _refine_ls_wR_factor_obs 0.0568 _refine_ls_goodness_of_fit_all 0.976 _refine_ls_goodness_of_fit_obs 0.995 _refine_ls_restrained_S_all 0.976 _refine_ls_restrained_S_obs 0.995 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ru Ru 0.0000 1.0000 0.5000 0.03777(15) Uani 1 d S . S S -0.06823(9) 0.83981(7) 0.58354(5) 0.0655(3) Uani 1 d . . C1 C -0.0291(3) 0.7527(3) 0.5360(2) 0.0576(8) Uani 1 d . . C2 C -0.0591(4) 0.6460(4) 0.5727(3) 0.0877(14) Uani 1 d . . N1 N -0.0836(5) 0.5624(4) 0.6036(3) 0.141(2) Uani 1 d . . N2 N 0.3182(3) 0.9517(3) 0.7500 0.0497(9) Uani 1 d S . C3 C 0.3532(5) 1.0771(5) 0.7500 0.0608(12) Uani 1 d S . H3A H 0.3204(5) 1.0924(5) 0.7965 0.073 Uiso 0.50 calc PR . H3B H 0.3204(5) 1.0924(5) 0.7035 0.073 Uiso 0.50 calc PR . C4 C 0.4809(6) 1.1593(6) 0.7500 0.096(2) Uani 1 d S . H4A H 0.4953(6) 1.2366(6) 0.7500 0.145 Uiso 1 calc SR . H4B H 0.5143(6) 1.1468(6) 0.7034 0.145 Uiso 0.50 calc PR . H4C H 0.5143(6) 1.1468(6) 0.7966 0.145 Uiso 0.50 calc PR . C5 C 0.3665(3) 0.9218(3) 0.6785(2) 0.0646(9) Uani 1 d . . H5A H 0.3452(3) 0.8418(3) 0.6824(2) 0.078 Uiso 1 calc R . H5B H 0.4494(3) 0.9667(3) 0.6809(2) 0.078 Uiso 1 calc R . C6 C 0.3279(6) 0.9413(5) 0.5982(2) 0.111(2) Uani 1 d . . H6A H 0.3605(6) 0.9175(5) 0.5568(2) 0.166 Uiso 1 calc R . H6B H 0.3529(6) 1.0211(5) 0.5919(2) 0.166 Uiso 1 calc R . H6C H 0.2459(6) 0.8975(5) 0.5950(2) 0.166 Uiso 1 calc R . C7 C 0.1898(4) 0.8857(5) 0.7500 0.072(2) Uani 1 d S . H7A H 0.1628(4) 0.9076(5) 0.7035 0.086 Uiso 0.50 calc PR . H7B H 0.1628(4) 0.9076(5) 0.7965 0.086 Uiso 0.50 calc PR . C8 C 0.1367(7) 0.7566(6) 0.7500 0.119(3) Uani 1 d S . H8A H 0.0548(7) 0.7215(6) 0.7500 0.178 Uiso 1 calc SR . H8B H 0.1608(7) 0.7333(6) 0.7966 0.178 Uiso 0.50 calc PR . H8C H 0.1608(7) 0.7333(6) 0.7034 0.178 Uiso 0.50 calc PR . C9 C 0.3333 0.6667 0.4560(6) 0.125(3) Uani 1 d S . H9 H 0.4029(54) 0.7345(54) 0.4431(30) 0.177(30) Uiso 1 d . . C10 C 0.3333 0.6667 0.5426(4) 0.081(2) Uani 1 d S . N3 N 0.3333 0.6667 0.6091(4) 0.110(2) Uani 1 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 Ru 0.0331(2) 0.0331(2) 0.0471(2) 0.000 0.000 0.01656(9) S 0.0650(6) 0.0517(4) 0.0761(5) 0.0211(4) 0.0278(5) 0.0264(5) C1 0.050(2) 0.035(2) 0.084(2) 0.004(2) -0.012(2) 0.0179(13) C2 0.093(3) 0.050(2) 0.112(3) 0.007(2) -0.025(3) 0.029(2) N1 0.155(5) 0.058(2) 0.190(5) 0.030(3) -0.049(4) 0.038(3) N2 0.053(2) 0.061(2) 0.045(2) 0.000 0.000 0.036(2) C3 0.068(3) 0.065(3) 0.063(3) 0.000 0.000 0.044(3) C4 0.080(4) 0.069(4) 0.128(5) 0.000 0.000 0.028(4) C5 0.084(3) 0.084(3) 0.052(2) 0.003(2) 0.012(2) 0.061(2) C6 0.181(6) 0.162(5) 0.050(2) 0.004(3) 0.011(3) 0.131(5) C7 0.053(3) 0.082(4) 0.076(3) 0.000 0.000 0.031(3) C8 0.096(6) 0.076(5) 0.144(7) 0.000 0.000 0.013(5) C9 0.141(6) 0.141(6) 0.093(7) 0.000 0.000 0.070(3) C10 0.076(3) 0.076(3) 0.090(5) 0.000 0.000 0.0380(13) N3 0.113(3) 0.113(3) 0.105(4) 0.000 0.000 0.056(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru S 2.3468(8) 2_675 ? Ru S 2.3468(8) 9_556 ? Ru S 2.3468(8) 7_466 ? Ru S 2.3468(8) 8_676 ? Ru S 2.3468(8) . ? Ru S 2.3468(8) 3_465 ? S C1 1.709(4) . ? C1 C1 1.389(7) 9_556 ? C1 C2 1.427(5) . ? C2 N1 1.132(6) . ? N2 C7 1.500(6) . ? N2 C3 1.513(7) . ? N2 C5 1.516(4) 4_556 ? N2 C5 1.516(4) . ? C3 C4 1.513(8) . ? C3 H3A 0.97 . ? C3 H3B 0.97 . ? C4 H4A 0.96 . ? C4 H4B 0.96 . ? C4 H4C 0.96 . ? C5 C6 1.519(5) . ? C5 H5A 0.97 . ? C5 H5B 0.97 . ? C6 H6A 0.96 . ? C6 H6B 0.96 . ? C6 H6C 0.96 . ? C7 C8 1.516(9) . ? C7 H7A 0.97 . ? C7 H7B 0.97 . ? C8 H8A 0.96 . ? C8 H8B 0.96 . ? C8 H8C 0.96 . ? C9 C10 1.458(12) . ? C9 H9 0.95(6) . ? C10 N3 1.119(8) . ? 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 S Ru S 97.90(5) 2_675 9_556 ? S Ru S 172.18(5) 2_675 7_466 ? S Ru S 87.79(3) 9_556 7_466 ? S Ru S 87.08(5) 2_675 8_676 ? S Ru S 87.79(3) 9_556 8_676 ? S Ru S 87.79(3) 7_466 8_676 ? S Ru S 87.79(3) 2_675 . ? S Ru S 87.08(5) 9_556 . ? S Ru S 97.90(5) 7_466 . ? S Ru S 172.18(6) 8_676 . ? S Ru S 87.79(3) 2_675 3_465 ? S Ru S 172.18(6) 9_556 3_465 ? S Ru S 87.08(5) 7_466 3_465 ? S Ru S 97.90(5) 8_676 3_465 ? S Ru S 87.79(3) . 3_465 ? C1 S Ru 103.81(12) . . ? C1 C1 C2 119.9(3) 9_556 . ? C1 C1 S 122.65(12) 9_556 . ? C2 C1 S 117.5(3) . . ? N1 C2 C1 178.2(6) . . ? C7 N2 C3 106.6(4) . . ? C7 N2 C5 111.4(3) . 4_556 ? C3 N2 C5 111.3(3) . 4_556 ? C7 N2 C5 111.4(3) . . ? C3 N2 C5 111.3(3) . . ? C5 N2 C5 105.0(3) 4_556 . ? N2 C3 C4 115.1(4) . . ? N2 C3 H3A 108.50(13) . . ? C4 C3 H3A 108.5(2) . . ? N2 C3 H3B 108.50(13) . . ? C4 C3 H3B 108.5(2) . . ? H3A C3 H3B 107.5 . . ? C3 C4 H4A 109.5(3) . . ? C3 C4 H4B 109.5(2) . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5(2) . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N2 C5 C6 115.5(3) . . ? N2 C5 H5A 108.4(2) . . ? C6 C5 H5A 108.4(3) . . ? N2 C5 H5B 108.4(2) . . ? C6 C5 H5B 108.4(3) . . ? H5A C5 H5B 107.5 . . ? C5 C6 H6A 109.5(2) . . ? C5 C6 H6B 109.5(3) . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5(3) . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C7 C8 115.1(6) . . ? N2 C7 H7A 108.49(15) . . ? C8 C7 H7A 108.5(2) . . ? N2 C7 H7B 108.49(15) . . ? C8 C7 H7B 108.5(2) . . ? H7A C7 H7B 107.5 . . ? C7 C8 H8A 109.5(4) . . ? C7 C8 H8B 109.5(2) . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5(2) . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 H9 103.1(35) . . ? N3 C10 C9 180.000(6) . . ? 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 S Ru S C1 -97.94(13) 2_675 . . . ? S Ru S C1 0.09(12) 9_556 . . . ? S Ru S C1 87.45(13) 7_466 . . . ? S Ru S C1 -48.94(12) 8_676 . . . ? S Ru S C1 174.19(13) 3_465 . . . ? Ru S C1 C1 -0.3(4) . . . 9_556 ? Ru S C1 C2 -180.0(3) . . . . ? C1 C1 C2 N1 167.7(181) 9_556 . . . ? S C1 C2 N1 -12.7(184) . . . . ? C7 N2 C3 C4 180.0 . . . . ? C5 N2 C3 C4 58.4(2) 4_556 . . . ? C5 N2 C3 C4 -58.4(2) . . . . ? C7 N2 C5 C6 57.8(5) . . . . ? C3 N2 C5 C6 -61.0(5) . . . . ? C5 N2 C5 C6 178.5(3) 4_556 . . . ? C3 N2 C7 C8 180.0 . . . . ? C5 N2 C7 C8 -58.4(2) 4_556 . . . ? C5 N2 C7 C8 58.4(2) . . . . ? _refine_diff_density_max 0.168 _refine_diff_density_min -0.235 _refine_diff_density_rms 0.033