# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_amm020_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H47 P Ru S3' _chemical_formula_weight 623.89 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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.4357(4) _cell_length_b 10.0451(4) _cell_length_c 17.6088(7) _cell_angle_alpha 88.602(2) _cell_angle_beta 80.783(2) _cell_angle_gamma 86.310(2) _cell_volume 1469.66(11) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.410 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 656 _exptl_absorpt_coefficient_mu 0.818 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8267 _exptl_absorpt_correction_T_max 0.8451 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 42079 _diffrn_reflns_av_R_equivalents 0.0290 _diffrn_reflns_av_sigmaI/netI 0.0262 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 33.24 _reflns_number_total 11193 _reflns_number_gt 10137 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0217P)^2^+0.4355P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11193 _refine_ls_number_parameters 311 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0258 _refine_ls_R_factor_gt 0.0216 _refine_ls_wR_factor_ref 0.0538 _refine_ls_wR_factor_gt 0.0521 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 0.737209(9) 0.658729(7) 0.697430(4) 0.01381(2) Uani 1 1 d . . . S1 S 0.86502(4) 0.56779(3) 0.793661(17) 0.02828(7) Uani 1 1 d . . . S2 S 0.94422(3) 0.54615(3) 0.611024(16) 0.02113(5) Uani 1 1 d . . . S3 S 0.76448(4) 0.83415(3) 0.611038(16) 0.02339(6) Uani 1 1 d . . . P1 P 0.54172(3) 0.78239(2) 0.784362(14) 0.01341(5) Uani 1 1 d . . . C1 C 0.62184(12) 0.88485(10) 0.85484(5) 0.01634(17) Uani 1 1 d . . . H1A H 0.5283 0.9410 0.8817 0.020 Uiso 1 1 calc R . . C2 C 0.69850(14) 0.80945(11) 0.91790(6) 0.0227(2) Uani 1 1 d . . . H2A H 0.6205 0.7495 0.9466 0.027 Uiso 1 1 calc R . . H2B H 0.7939 0.7539 0.8941 0.027 Uiso 1 1 calc R . . C3 C 0.74900(14) 0.90742(12) 0.97358(6) 0.0259(2) Uani 1 1 d . . . H3A H 0.6522 0.9573 1.0007 0.031 Uiso 1 1 calc R . . H3B H 0.8021 0.8571 1.0126 0.031 Uiso 1 1 calc R . . C4 C 0.86401(15) 1.00569(14) 0.93126(7) 0.0300(3) Uani 1 1 d . . . H4A H 0.8893 1.0708 0.9682 0.036 Uiso 1 1 calc R . . H4B H 0.9658 0.9569 0.9088 0.036 Uiso 1 1 calc R . . C5 C 0.79067(17) 1.07945(13) 0.86767(7) 0.0309(3) Uani 1 1 d . . . H5A H 0.8701 1.1383 0.8391 0.037 Uiso 1 1 calc R . . H5B H 0.6956 1.1362 0.8907 0.037 Uiso 1 1 calc R . . C6 C 0.73997(15) 0.98179(12) 0.81190(6) 0.0257(2) Uani 1 1 d . . . H6A H 0.8364 0.9306 0.7854 0.031 Uiso 1 1 calc R . . H6B H 0.6884 1.0322 0.7724 0.031 Uiso 1 1 calc R . . C7 C 0.38757(12) 0.67912(10) 0.84216(6) 0.01783(18) Uani 1 1 d . . . H7 H 0.3133 0.6557 0.8063 0.021 Uiso 1 1 calc R . . C8 C 0.46177(14) 0.54556(11) 0.86928(7) 0.0228(2) Uani 1 1 d . . . H8A H 0.5215 0.4973 0.8241 0.027 Uiso 1 1 calc R . . H8B H 0.5394 0.5635 0.9039 0.027 Uiso 1 1 calc R . . C9 C 0.33395(16) 0.45762(12) 0.91165(7) 0.0287(2) Uani 1 1 d . . . H9A H 0.2652 0.4294 0.8751 0.034 Uiso 1 1 calc R . . H9B H 0.3873 0.3764 0.9315 0.034 Uiso 1 1 calc R . . C10 C 0.22904(15) 0.53007(13) 0.97828(7) 0.0305(3) Uani 1 1 d . . . H10A H 0.2953 0.5500 1.0177 0.037 Uiso 1 1 calc R . . H10B H 0.1437 0.4722 1.0023 0.037 Uiso 1 1 calc R . . C11 C 0.15259(14) 0.65953(13) 0.94982(8) 0.0285(2) Uani 1 1 d . . . H11A H 0.0872 0.7069 0.9939 0.034 Uiso 1 1 calc R . . H11B H 0.0802 0.6389 0.9132 0.034 Uiso 1 1 calc R . . C12 C 0.28144(14) 0.74990(11) 0.91004(7) 0.0256(2) Uani 1 1 d . . . H12A H 0.3494 0.7754 0.9476 0.031 Uiso 1 1 calc R . . H12B H 0.2288 0.8325 0.8913 0.031 Uiso 1 1 calc R . . C13 C 0.42676(12) 0.91594(9) 0.73547(5) 0.01546(17) Uani 1 1 d . . . H13 H 0.5105 0.9598 0.6982 0.019 Uiso 1 1 calc R . . C14 C 0.31425(14) 0.86003(10) 0.68523(7) 0.0224(2) Uani 1 1 d . . . H14A H 0.2232 0.8200 0.7185 0.027 Uiso 1 1 calc R . . H14B H 0.3736 0.7891 0.6520 0.027 Uiso 1 1 calc R . . C15 C 0.24953(15) 0.97124(11) 0.63480(7) 0.0255(2) Uani 1 1 d . . . H15A H 0.3401 1.0053 0.5982 0.031 Uiso 1 1 calc R . . H15B H 0.1739 0.9340 0.6045 0.031 Uiso 1 1 calc R . . C16 C 0.16322(14) 1.08649(12) 0.68313(7) 0.0268(2) Uani 1 1 d . . . H16A H 0.1290 1.1585 0.6488 0.032 Uiso 1 1 calc R . . H16B H 0.0658 1.0550 0.7158 0.032 Uiso 1 1 calc R . . C17 C 0.27369(15) 1.14094(11) 0.73382(7) 0.0257(2) Uani 1 1 d . . . H17A H 0.2138 1.2119 0.7668 0.031 Uiso 1 1 calc R . . H17B H 0.3653 1.1810 0.7009 0.031 Uiso 1 1 calc R . . C18 C 0.33758(16) 1.03066(12) 0.78463(6) 0.0276(2) Uani 1 1 d . . . H18A H 0.2467 0.9957 0.8206 0.033 Uiso 1 1 calc R . . H18B H 0.4118 1.0682 0.8155 0.033 Uiso 1 1 calc R . . C19 C 1.02415(15) 0.45136(13) 0.74749(8) 0.0311(3) Uani 1 1 d . . . H19A H 1.1078 0.4372 0.7809 0.037 Uiso 1 1 calc R . . H19B H 0.9787 0.3643 0.7419 0.037 Uiso 1 1 calc R . . C20 C 1.10034(15) 0.50016(13) 0.66981(8) 0.0327(3) Uani 1 1 d . . . H20A H 1.1754 0.4292 0.6441 0.039 Uiso 1 1 calc R . . H20B H 1.1624 0.5786 0.6757 0.039 Uiso 1 1 calc R . . C21 C 1.03852(15) 0.68027(12) 0.55237(7) 0.0265(2) Uani 1 1 d . . . H21A H 1.1033 0.7308 0.5826 0.032 Uiso 1 1 calc R . . H21B H 1.1103 0.6433 0.5068 0.032 Uiso 1 1 calc R . . C22 C 0.90535(16) 0.77051(12) 0.52768(7) 0.0287(2) Uani 1 1 d . . . H22A H 0.8464 0.7205 0.4945 0.034 Uiso 1 1 calc R . . H22B H 0.9525 0.8464 0.4971 0.034 Uiso 1 1 calc R . . C23 C 0.57873(12) 0.54953(10) 0.67738(6) 0.01744(18) Uani 1 1 d . . . C24 C 0.59742(12) 0.42026(9) 0.63799(6) 0.01614(17) Uani 1 1 d . . . C25 C 0.50919(13) 0.39883(11) 0.57888(6) 0.01936(18) Uani 1 1 d . . . H25 H 0.4368 0.4680 0.5648 0.023 Uiso 1 1 calc R . . C26 C 0.52579(14) 0.27787(12) 0.54049(6) 0.0238(2) Uani 1 1 d . . . H26 H 0.4672 0.2658 0.4996 0.029 Uiso 1 1 calc R . . C27 C 0.62836(15) 0.17480(11) 0.56212(7) 0.0245(2) Uani 1 1 d . . . H27 H 0.6399 0.0921 0.5361 0.029 Uiso 1 1 calc R . . C28 C 0.71353(14) 0.19315(10) 0.62171(7) 0.0228(2) Uani 1 1 d . . . H28 H 0.7824 0.1224 0.6370 0.027 Uiso 1 1 calc R . . C29 C 0.69879(13) 0.31462(10) 0.65926(6) 0.02004(19) Uani 1 1 d . . . H29 H 0.7582 0.3261 0.6999 0.024 Uiso 1 1 calc R . . H1 H 0.4671(17) 0.5812(14) 0.6908(8) 0.023(3) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01363(4) 0.01182(4) 0.01567(4) -0.00259(2) -0.00158(3) 0.00051(2) S1 0.02815(14) 0.03244(15) 0.02449(13) -0.00665(11) -0.01046(11) 0.01459(12) S2 0.01781(11) 0.01723(11) 0.02651(13) -0.00796(9) 0.00393(10) -0.00280(9) S3 0.03040(14) 0.01498(11) 0.02197(12) 0.00011(9) 0.00416(10) -0.00093(10) P1 0.01377(11) 0.01276(10) 0.01342(10) -0.00057(8) -0.00191(8) 0.00068(8) C1 0.0169(4) 0.0175(4) 0.0147(4) -0.0023(3) -0.0026(3) -0.0001(3) C2 0.0252(5) 0.0241(5) 0.0201(5) -0.0019(4) -0.0088(4) 0.0020(4) C3 0.0242(5) 0.0345(6) 0.0204(5) -0.0068(4) -0.0088(4) 0.0022(4) C4 0.0231(6) 0.0392(7) 0.0299(6) -0.0124(5) -0.0084(5) -0.0044(5) C5 0.0362(7) 0.0299(6) 0.0292(6) -0.0046(5) -0.0084(5) -0.0130(5) C6 0.0298(6) 0.0292(6) 0.0196(5) -0.0015(4) -0.0037(4) -0.0129(5) C7 0.0176(4) 0.0171(4) 0.0186(4) 0.0025(3) -0.0024(3) -0.0016(3) C8 0.0240(5) 0.0192(5) 0.0239(5) 0.0055(4) -0.0019(4) 0.0006(4) C9 0.0309(6) 0.0240(5) 0.0315(6) 0.0117(4) -0.0062(5) -0.0058(4) C10 0.0241(6) 0.0367(6) 0.0296(6) 0.0148(5) -0.0011(5) -0.0059(5) C11 0.0191(5) 0.0315(6) 0.0323(6) 0.0072(5) 0.0037(4) -0.0032(4) C12 0.0217(5) 0.0227(5) 0.0288(5) 0.0008(4) 0.0071(4) -0.0023(4) C13 0.0166(4) 0.0137(4) 0.0159(4) -0.0010(3) -0.0030(3) 0.0019(3) C14 0.0251(5) 0.0159(4) 0.0290(5) 0.0015(4) -0.0131(4) -0.0020(4) C15 0.0326(6) 0.0193(5) 0.0285(5) 0.0016(4) -0.0172(5) -0.0018(4) C16 0.0228(5) 0.0241(5) 0.0338(6) 0.0060(4) -0.0082(5) 0.0044(4) C17 0.0322(6) 0.0192(5) 0.0250(5) -0.0026(4) -0.0068(4) 0.0102(4) C18 0.0368(6) 0.0250(5) 0.0194(5) -0.0040(4) -0.0061(4) 0.0161(5) C19 0.0256(6) 0.0291(6) 0.0398(7) -0.0093(5) -0.0130(5) 0.0120(5) C20 0.0176(5) 0.0306(6) 0.0490(8) -0.0082(5) -0.0045(5) 0.0057(4) C21 0.0246(5) 0.0242(5) 0.0282(5) -0.0076(4) 0.0076(4) -0.0097(4) C22 0.0342(6) 0.0262(5) 0.0226(5) -0.0019(4) 0.0068(5) -0.0057(5) C23 0.0174(4) 0.0145(4) 0.0201(4) -0.0014(3) -0.0020(3) -0.0005(3) C24 0.0168(4) 0.0136(4) 0.0175(4) -0.0001(3) 0.0000(3) -0.0032(3) C25 0.0187(5) 0.0205(5) 0.0187(4) -0.0004(3) -0.0020(4) -0.0025(4) C26 0.0257(5) 0.0268(5) 0.0196(5) -0.0049(4) -0.0018(4) -0.0083(4) C27 0.0294(6) 0.0174(5) 0.0247(5) -0.0055(4) 0.0049(4) -0.0065(4) C28 0.0244(5) 0.0137(4) 0.0286(5) 0.0009(4) 0.0011(4) -0.0011(4) C29 0.0209(5) 0.0158(4) 0.0238(5) 0.0003(4) -0.0046(4) -0.0022(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 C23 1.8639(11) . ? Ru1 S1 2.2916(3) . ? Ru1 S3 2.2981(3) . ? Ru1 S2 2.3711(3) . ? Ru1 P1 2.3720(3) . ? S1 C19 1.8236(12) . ? S2 C21 1.8225(12) . ? S2 C20 1.8316(13) . ? S3 C22 1.8343(12) . ? P1 C1 1.8646(10) . ? P1 C7 1.8710(11) . ? P1 C13 1.8774(9) . ? C1 C2 1.5332(14) . ? C1 C6 1.5363(15) . ? C1 H1A 1.0000 . ? C2 C3 1.5317(16) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.5254(19) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.5191(18) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.5315(17) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C12 1.5338(15) . ? C7 C8 1.5416(14) . ? C7 H7 1.0000 . ? C8 C9 1.5271(16) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.5218(19) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.5238(17) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.5324(16) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.5365(15) . ? C13 C18 1.5401(14) . ? C13 H13 1.0000 . ? C14 C15 1.5372(14) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.5282(17) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.5233(17) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.5322(15) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.500(2) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.5097(18) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.4746(14) . ? C23 H1 0.968(14) . ? C24 C25 1.4011(14) . ? C24 C29 1.4015(14) . ? C25 C26 1.3932(15) . ? C25 H25 0.9500 . ? C26 C27 1.3917(17) . ? C26 H26 0.9500 . ? C27 C28 1.3852(17) . ? C27 H27 0.9500 . ? C28 C29 1.3910(15) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? 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 C23 Ru1 S1 110.51(3) . . ? C23 Ru1 S3 110.97(3) . . ? S1 Ru1 S3 138.172(13) . . ? C23 Ru1 S2 93.96(3) . . ? S1 Ru1 S2 86.255(11) . . ? S3 Ru1 S2 85.792(10) . . ? C23 Ru1 P1 89.68(3) . . ? S1 Ru1 P1 93.182(10) . . ? S3 Ru1 P1 92.207(10) . . ? S2 Ru1 P1 176.285(10) . . ? C19 S1 Ru1 106.28(4) . . ? C21 S2 C20 100.24(6) . . ? C21 S2 Ru1 103.74(4) . . ? C20 S2 Ru1 104.08(4) . . ? C22 S3 Ru1 105.44(4) . . ? C1 P1 C7 106.13(5) . . ? C1 P1 C13 100.13(4) . . ? C7 P1 C13 106.17(5) . . ? C1 P1 Ru1 115.76(3) . . ? C7 P1 Ru1 114.27(3) . . ? C13 P1 Ru1 113.02(3) . . ? C2 C1 C6 109.89(9) . . ? C2 C1 P1 117.03(7) . . ? C6 C1 P1 109.85(7) . . ? C2 C1 H1A 106.5 . . ? C6 C1 H1A 106.5 . . ? P1 C1 H1A 106.5 . . ? C3 C2 C1 110.57(9) . . ? C3 C2 H2A 109.5 . . ? C1 C2 H2A 109.5 . . ? C3 C2 H2B 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? C4 C3 C2 111.33(10) . . ? C4 C3 H3A 109.4 . . ? C2 C3 H3A 109.4 . . ? C4 C3 H3B 109.4 . . ? C2 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? C5 C4 C3 111.04(10) . . ? C5 C4 H4A 109.4 . . ? C3 C4 H4A 109.4 . . ? C5 C4 H4B 109.4 . . ? C3 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? C4 C5 C6 111.14(10) . . ? C4 C5 H5A 109.4 . . ? C6 C5 H5A 109.4 . . ? C4 C5 H5B 109.4 . . ? C6 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? C5 C6 C1 110.89(9) . . ? C5 C6 H6A 109.5 . . ? C1 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? C12 C7 C8 110.21(9) . . ? C12 C7 P1 115.51(7) . . ? C8 C7 P1 112.24(7) . . ? C12 C7 H7 106.1 . . ? C8 C7 H7 106.1 . . ? P1 C7 H7 106.1 . . ? C9 C8 C7 111.99(9) . . ? C9 C8 H8A 109.2 . . ? C7 C8 H8A 109.2 . . ? C9 C8 H8B 109.2 . . ? C7 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? C10 C9 C8 111.89(10) . . ? C10 C9 H9A 109.2 . . ? C8 C9 H9A 109.2 . . ? C10 C9 H9B 109.2 . . ? C8 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? C9 C10 C11 110.26(10) . . ? C9 C10 H10A 109.6 . . ? C11 C10 H10A 109.6 . . ? C9 C10 H10B 109.6 . . ? C11 C10 H10B 109.6 . . ? H10A C10 H10B 108.1 . . ? C10 C11 C12 110.97(10) . . ? C10 C11 H11A 109.4 . . ? C12 C11 H11A 109.4 . . ? C10 C11 H11B 109.4 . . ? C12 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? C11 C12 C7 111.06(10) . . ? C11 C12 H12A 109.4 . . ? C7 C12 H12A 109.4 . . ? C11 C12 H12B 109.4 . . ? C7 C12 H12B 109.4 . . ? H12A C12 H12B 108.0 . . ? C14 C13 C18 109.86(9) . . ? C14 C13 P1 113.12(7) . . ? C18 C13 P1 118.21(7) . . ? C14 C13 H13 104.7 . . ? C18 C13 H13 104.7 . . ? P1 C13 H13 104.7 . . ? C13 C14 C15 110.53(9) . . ? C13 C14 H14A 109.5 . . ? C15 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? C15 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? C16 C15 C14 111.72(10) . . ? C16 C15 H15A 109.3 . . ? C14 C15 H15A 109.3 . . ? C16 C15 H15B 109.3 . . ? C14 C15 H15B 109.3 . . ? H15A C15 H15B 107.9 . . ? C17 C16 C15 110.56(9) . . ? C17 C16 H16A 109.5 . . ? C15 C16 H16A 109.5 . . ? C17 C16 H16B 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 108.1 . . ? C16 C17 C18 111.25(10) . . ? C16 C17 H17A 109.4 . . ? C18 C17 H17A 109.4 . . ? C16 C17 H17B 109.4 . . ? C18 C17 H17B 109.4 . . ? H17A C17 H17B 108.0 . . ? C17 C18 C13 110.99(9) . . ? C17 C18 H18A 109.4 . . ? C13 C18 H18A 109.4 . . ? C17 C18 H18B 109.4 . . ? C13 C18 H18B 109.4 . . ? H18A C18 H18B 108.0 . . ? C20 C19 S1 112.51(8) . . ? C20 C19 H19A 109.1 . . ? S1 C19 H19A 109.1 . . ? C20 C19 H19B 109.1 . . ? S1 C19 H19B 109.1 . . ? H19A C19 H19B 107.8 . . ? C19 C20 S2 109.73(9) . . ? C19 C20 H20A 109.7 . . ? S2 C20 H20A 109.7 . . ? C19 C20 H20B 109.7 . . ? S2 C20 H20B 109.7 . . ? H20A C20 H20B 108.2 . . ? C22 C21 S2 107.32(8) . . ? C22 C21 H21A 110.3 . . ? S2 C21 H21A 110.3 . . ? C22 C21 H21B 110.3 . . ? S2 C21 H21B 110.3 . . ? H21A C21 H21B 108.5 . . ? C21 C22 S3 111.28(8) . . ? C21 C22 H22A 109.4 . . ? S3 C22 H22A 109.4 . . ? C21 C22 H22B 109.4 . . ? S3 C22 H22B 109.4 . . ? H22A C22 H22B 108.0 . . ? C24 C23 Ru1 128.96(8) . . ? C24 C23 H1 112.5(8) . . ? Ru1 C23 H1 118.4(8) . . ? C25 C24 C29 117.97(9) . . ? C25 C24 C23 120.13(9) . . ? C29 C24 C23 121.87(9) . . ? C26 C25 C24 121.13(10) . . ? C26 C25 H25 119.4 . . ? C24 C25 H25 119.4 . . ? C27 C26 C25 119.85(10) . . ? C27 C26 H26 120.1 . . ? C25 C26 H26 120.1 . . ? C28 C27 C26 119.78(10) . . ? C28 C27 H27 120.1 . . ? C26 C27 H27 120.1 . . ? C27 C28 C29 120.36(10) . . ? C27 C28 H28 119.8 . . ? C29 C28 H28 119.8 . . ? C28 C29 C24 120.88(10) . . ? C28 C29 H29 119.6 . . ? C24 C29 H29 119.6 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 33.24 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.552 _refine_diff_density_min -0.730 _refine_diff_density_rms 0.060 _database_code_depnum_ccdc_archive 'CCDC 971468' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_amm027_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H47 O P Ru S2' _chemical_formula_weight 703.91 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' 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' _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 10.4646(7) _cell_length_b 18.4403(12) _cell_length_c 17.6740(11) _cell_angle_alpha 90.00 _cell_angle_beta 94.848(2) _cell_angle_gamma 90.00 _cell_volume 3398.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.376 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 0.659 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8822 _exptl_absorpt_correction_T_max 0.8934 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 30892 _diffrn_reflns_av_R_equivalents 0.0480 _diffrn_reflns_av_sigmaI/netI 0.0499 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 27.84 _reflns_number_total 8032 _reflns_number_gt 6258 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0349P)^2^+5.9134P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8032 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0596 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.0958 _refine_ls_wR_factor_gt 0.0873 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.983 _refine_ls_shift/su_max 0.002 _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 0.24231(2) 0.119130(12) 0.762867(13) 0.01801(7) Uani 1 1 d . . . S1 S 0.08005(7) 0.19667(4) 0.71808(5) 0.02738(17) Uani 1 1 d . . . S2 S 0.40773(7) 0.05567(4) 0.71788(4) 0.02483(17) Uani 1 1 d . . . P1 P 0.36915(7) 0.20024(4) 0.83097(4) 0.01743(15) Uani 1 1 d . . . O1 O 0.12767(18) 0.04377(11) 0.68901(12) 0.0229(4) Uani 1 1 d . . . C32 C 0.2985(3) 0.24282(15) 0.91404(17) 0.0232(6) Uani 1 1 d . . . H32A H 0.3116 0.2069 0.9564 0.028 Uiso 1 1 calc R . . C33 C 0.1532(3) 0.25575(18) 0.9029(2) 0.0307(7) Uani 1 1 d . . . H33A H 0.1345 0.2929 0.8631 0.037 Uiso 1 1 calc R . . H33B H 0.1096 0.2103 0.8856 0.037 Uiso 1 1 calc R . . C34 C 0.1010(4) 0.2810(2) 0.9769(2) 0.0436(9) Uani 1 1 d . . . H34A H 0.0081 0.2910 0.9675 0.052 Uiso 1 1 calc R . . H34B H 0.1120 0.2417 1.0150 0.052 Uiso 1 1 calc R . . C35 C 0.1686(4) 0.3487(2) 1.0084(2) 0.0424(9) Uani 1 1 d . . . H35A H 0.1482 0.3899 0.9735 0.051 Uiso 1 1 calc R . . H35B H 0.1373 0.3609 1.0582 0.051 Uiso 1 1 calc R . . C36 C 0.3125(4) 0.3377(2) 1.0180(2) 0.0459(10) Uani 1 1 d . . . H36A H 0.3335 0.3008 1.0578 0.055 Uiso 1 1 calc R . . H36B H 0.3546 0.3837 1.0347 0.055 Uiso 1 1 calc R . . C37 C 0.3641(3) 0.31303(19) 0.9439(2) 0.0356(8) Uani 1 1 d . . . H37A H 0.4577 0.3048 0.9525 0.043 Uiso 1 1 calc R . . H37B H 0.3496 0.3517 0.9053 0.043 Uiso 1 1 calc R . . C20 C 0.4268(3) 0.27688(15) 0.77519(17) 0.0214(6) Uani 1 1 d . . . H20A H 0.4822 0.3075 0.8113 0.026 Uiso 1 1 calc R . . C21 C 0.5116(3) 0.25106(18) 0.7139(2) 0.0338(8) Uani 1 1 d . . . H21A H 0.4601 0.2210 0.6762 0.041 Uiso 1 1 calc R . . H21B H 0.5822 0.2207 0.7374 0.041 Uiso 1 1 calc R . . C22 C 0.5677(4) 0.3161(2) 0.6738(2) 0.0448(10) Uani 1 1 d . . . H22A H 0.6273 0.3427 0.7105 0.054 Uiso 1 1 calc R . . H22B H 0.6175 0.2984 0.6323 0.054 Uiso 1 1 calc R . . C23 C 0.4638(4) 0.36760(19) 0.6412(2) 0.0412(9) Uani 1 1 d . . . H23A H 0.5042 0.4108 0.6199 0.049 Uiso 1 1 calc R . . H23B H 0.4115 0.3432 0.5994 0.049 Uiso 1 1 calc R . . C24 C 0.3781(3) 0.39135(17) 0.7012(2) 0.0335(8) Uani 1 1 d . . . H24A H 0.3078 0.4218 0.6774 0.040 Uiso 1 1 calc R . . H24B H 0.4283 0.4212 0.7397 0.040 Uiso 1 1 calc R . . C25 C 0.3208(3) 0.32582(17) 0.74032(19) 0.0293(7) Uani 1 1 d . . . H25A H 0.2677 0.3430 0.7805 0.035 Uiso 1 1 calc R . . H25B H 0.2650 0.2981 0.7027 0.035 Uiso 1 1 calc R . . C26 C 0.5229(3) 0.15770(15) 0.87019(17) 0.0212(6) Uani 1 1 d . . . H26A H 0.5614 0.1362 0.8254 0.025 Uiso 1 1 calc R . . C27 C 0.5028(3) 0.09386(18) 0.92326(19) 0.0309(7) Uani 1 1 d . . . H27A H 0.4404 0.0595 0.8979 0.037 Uiso 1 1 calc R . . H27B H 0.4671 0.1118 0.9699 0.037 Uiso 1 1 calc R . . C28 C 0.6302(3) 0.05457(19) 0.9445(2) 0.0356(8) Uani 1 1 d . . . H28A H 0.6157 0.0151 0.9808 0.043 Uiso 1 1 calc R . . H28B H 0.6608 0.0324 0.8984 0.043 Uiso 1 1 calc R . . C29 C 0.7318(3) 0.1046(2) 0.9796(2) 0.0364(8) Uani 1 1 d . . . H29A H 0.8130 0.0776 0.9903 0.044 Uiso 1 1 calc R . . H29B H 0.7053 0.1237 1.0283 0.044 Uiso 1 1 calc R . . C30 C 0.7527(3) 0.1673(2) 0.9262(3) 0.0473(10) Uani 1 1 d . . . H30A H 0.7846 0.1484 0.8788 0.057 Uiso 1 1 calc R . . H30B H 0.8181 0.2007 0.9503 0.057 Uiso 1 1 calc R . . C31 C 0.6262(3) 0.20863(19) 0.9073(2) 0.0424(9) Uani 1 1 d . . . H31A H 0.5964 0.2294 0.9544 0.051 Uiso 1 1 calc R . . H31B H 0.6407 0.2491 0.8722 0.051 Uiso 1 1 calc R . . C1 C 0.1945(3) 0.07735(16) 0.85120(18) 0.0242(6) Uani 1 1 d . . . H1A H 0.2181 0.1018 0.8976 0.029 Uiso 1 1 calc R . . C2 C 0.1224(3) 0.00894(16) 0.85528(16) 0.0223(6) Uani 1 1 d . . . C3 C 0.1567(3) -0.05421(16) 0.81873(18) 0.0267(7) Uani 1 1 d . . . H3A H 0.2290 -0.0540 0.7897 0.032 Uiso 1 1 calc R . . C4 C 0.0860(3) -0.11731(17) 0.82442(19) 0.0323(7) Uani 1 1 d . . . H4A H 0.1101 -0.1600 0.7992 0.039 Uiso 1 1 calc R . . C5 C -0.0195(3) -0.11834(18) 0.8666(2) 0.0360(8) Uani 1 1 d . . . H5A H -0.0677 -0.1616 0.8706 0.043 Uiso 1 1 calc R . . C6 C -0.0540(3) -0.0558(2) 0.9028(2) 0.0348(8) Uani 1 1 d . . . H6A H -0.1269 -0.0560 0.9315 0.042 Uiso 1 1 calc R . . C7 C 0.0166(3) 0.00705(17) 0.89765(18) 0.0275(7) Uani 1 1 d . . . H7A H -0.0076 0.0495 0.9234 0.033 Uiso 1 1 calc R . . C14 C -0.0379(3) 0.13067(16) 0.69164(17) 0.0245(6) Uani 1 1 d . . . C19 C -0.0049(3) 0.05849(16) 0.68160(17) 0.0233(6) Uani 1 1 d . . . C18 C -0.0955(3) 0.00340(18) 0.67336(19) 0.0302(7) Uani 1 1 d . . . H18A H -0.0699 -0.0459 0.6709 0.036 Uiso 1 1 calc R . . C17 C -0.2242(3) 0.02209(19) 0.6689(2) 0.0351(8) Uani 1 1 d . . . H17A H -0.2880 -0.0146 0.6629 0.042 Uiso 1 1 calc R . . C16 C -0.2601(3) 0.0942(2) 0.6731(2) 0.0362(8) Uani 1 1 d . . . H16A H -0.3484 0.1069 0.6676 0.043 Uiso 1 1 calc R . . C15 C -0.1681(3) 0.14796(19) 0.6851(2) 0.0320(7) Uani 1 1 d . . . H15A H -0.1939 0.1971 0.6890 0.038 Uiso 1 1 calc R . . C13 C 0.1895(3) 0.00091(15) 0.63731(17) 0.0228(6) Uani 1 1 d . . . C12 C 0.1254(3) -0.03573(17) 0.57623(19) 0.0302(7) Uani 1 1 d . . . H12A H 0.0346 -0.0335 0.5684 0.036 Uiso 1 1 calc R . . C11 C 0.1948(4) -0.0753(2) 0.5271(2) 0.0388(8) Uani 1 1 d . . . H11A H 0.1517 -0.1002 0.4854 0.047 Uiso 1 1 calc R . . C10 C 0.3265(3) -0.0784(2) 0.5391(2) 0.0386(8) Uani 1 1 d . . . H10A H 0.3741 -0.1064 0.5062 0.046 Uiso 1 1 calc R . . C9 C 0.3897(3) -0.04067(18) 0.59892(19) 0.0312(7) Uani 1 1 d . . . H9A H 0.4806 -0.0429 0.6061 0.037 Uiso 1 1 calc R . . C8 C 0.3226(3) 0.00052(16) 0.64892(17) 0.0229(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01601(11) 0.01533(11) 0.02231(12) -0.00002(9) -0.00059(8) -0.00048(9) S1 0.0218(3) 0.0185(4) 0.0406(5) 0.0011(3) -0.0047(3) -0.0003(3) S2 0.0175(3) 0.0282(4) 0.0283(4) -0.0061(3) -0.0005(3) 0.0003(3) P1 0.0176(3) 0.0140(3) 0.0204(4) 0.0009(3) -0.0005(3) -0.0011(3) O1 0.0170(9) 0.0222(11) 0.0288(11) -0.0035(9) -0.0018(9) -0.0003(8) C32 0.0284(15) 0.0180(14) 0.0231(15) -0.0020(11) 0.0008(13) -0.0002(12) C33 0.0281(16) 0.0256(16) 0.0398(19) -0.0091(14) 0.0106(15) -0.0020(13) C34 0.045(2) 0.037(2) 0.053(2) -0.0132(17) 0.0232(19) -0.0071(17) C35 0.053(2) 0.0342(19) 0.042(2) -0.0133(16) 0.0161(18) -0.0001(17) C36 0.061(3) 0.041(2) 0.035(2) -0.0191(17) -0.0033(19) 0.0013(19) C37 0.0322(17) 0.0342(19) 0.040(2) -0.0153(15) 0.0015(15) -0.0047(15) C20 0.0215(14) 0.0189(14) 0.0237(15) 0.0019(11) 0.0013(12) -0.0040(11) C21 0.0422(19) 0.0260(17) 0.0352(19) 0.0077(14) 0.0142(16) 0.0035(15) C22 0.051(2) 0.037(2) 0.051(2) 0.0135(17) 0.0280(19) 0.0000(17) C23 0.059(2) 0.0286(19) 0.037(2) 0.0133(15) 0.0109(18) -0.0066(17) C24 0.0340(17) 0.0252(17) 0.0410(19) 0.0111(14) 0.0008(15) 0.0004(14) C25 0.0266(15) 0.0256(16) 0.0351(18) 0.0111(13) -0.0008(14) -0.0010(13) C26 0.0213(14) 0.0195(14) 0.0219(15) 0.0019(11) -0.0028(12) -0.0004(11) C27 0.0280(16) 0.0317(17) 0.0324(18) 0.0111(14) -0.0017(14) 0.0031(14) C28 0.0341(18) 0.0322(18) 0.039(2) 0.0113(15) -0.0033(16) 0.0064(15) C29 0.0301(17) 0.046(2) 0.0316(18) -0.0017(15) -0.0061(15) 0.0136(15) C30 0.0245(17) 0.040(2) 0.073(3) 0.0089(19) -0.0176(19) -0.0034(16) C31 0.0302(17) 0.0254(17) 0.067(3) 0.0011(17) -0.0215(18) -0.0028(14) C1 0.0239(14) 0.0216(15) 0.0269(16) -0.0021(12) 0.0011(13) 0.0002(12) C2 0.0244(14) 0.0217(14) 0.0198(15) 0.0018(11) -0.0033(12) -0.0019(12) C3 0.0287(16) 0.0243(16) 0.0268(16) 0.0015(12) 0.0009(13) -0.0018(13) C4 0.0398(18) 0.0192(15) 0.0370(18) -0.0017(14) -0.0024(15) 0.0021(14) C5 0.0367(18) 0.0278(17) 0.042(2) 0.0057(15) -0.0084(16) -0.0159(15) C6 0.0248(16) 0.043(2) 0.0363(19) 0.0035(16) 0.0030(15) -0.0074(15) C7 0.0237(15) 0.0283(16) 0.0303(17) -0.0005(13) 0.0019(13) -0.0004(13) C14 0.0213(14) 0.0275(16) 0.0244(15) -0.0021(12) 0.0006(12) -0.0012(12) C19 0.0188(13) 0.0275(16) 0.0234(15) -0.0010(12) 0.0013(12) -0.0028(12) C18 0.0273(16) 0.0294(17) 0.0338(18) -0.0028(14) 0.0021(14) -0.0034(13) C17 0.0267(16) 0.0373(19) 0.042(2) -0.0054(15) 0.0047(15) -0.0098(14) C16 0.0143(14) 0.048(2) 0.047(2) -0.0088(17) 0.0037(14) 0.0001(14) C15 0.0269(16) 0.0292(17) 0.0399(19) -0.0039(14) 0.0025(15) 0.0045(14) C13 0.0240(14) 0.0165(14) 0.0276(16) 0.0002(11) 0.0002(13) 0.0024(12) C12 0.0260(15) 0.0286(17) 0.0346(18) -0.0064(14) -0.0048(14) 0.0012(13) C11 0.0414(19) 0.037(2) 0.037(2) -0.0127(15) -0.0050(17) 0.0022(16) C10 0.0388(19) 0.040(2) 0.037(2) -0.0133(16) -0.0013(16) 0.0122(16) C9 0.0265(16) 0.0350(18) 0.0318(18) -0.0063(14) 0.0000(14) 0.0068(14) C8 0.0238(14) 0.0204(14) 0.0238(15) 0.0004(12) -0.0019(12) 0.0023(12) _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 C1 1.848(3) . ? Ru1 O1 2.1931(19) . ? Ru1 P1 2.2754(7) . ? Ru1 S2 2.2870(8) . ? Ru1 S1 2.3080(8) . ? S1 C14 1.768(3) . ? S2 C8 1.769(3) . ? P1 C20 1.853(3) . ? P1 C32 1.872(3) . ? P1 C26 1.870(3) . ? O1 C13 1.406(3) . ? O1 C19 1.409(3) . ? C32 C33 1.535(4) . ? C32 C37 1.538(4) . ? C32 H32A 1.0000 . ? C33 C34 1.532(5) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.518(5) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.514(5) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.526(5) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C20 C25 1.519(4) . ? C20 C21 1.534(4) . ? C20 H20A 1.0000 . ? C21 C22 1.535(4) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.520(5) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.510(5) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.539(4) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.531(4) . ? C26 C31 1.536(4) . ? C26 H26A 1.0000 . ? C27 C28 1.536(4) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.502(5) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.519(5) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.540(5) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C1 C2 1.475(4) . ? C1 H1A 0.9500 . ? C2 C7 1.389(4) . ? C2 C3 1.393(4) . ? C3 C4 1.387(4) . ? C3 H3A 0.9500 . ? C4 C5 1.383(5) . ? C4 H4A 0.9500 . ? C5 C6 1.383(5) . ? C5 H5A 0.9500 . ? C6 C7 1.382(4) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C14 C19 1.390(4) . ? C14 C15 1.395(4) . ? C19 C18 1.389(4) . ? C18 C17 1.386(4) . ? C18 H18A 0.9500 . ? C17 C16 1.386(5) . ? C17 H17A 0.9500 . ? C16 C15 1.386(5) . ? C16 H16A 0.9500 . ? C15 H15A 0.9500 . ? C13 C8 1.391(4) . ? C13 C12 1.396(4) . ? C12 C11 1.385(5) . ? C12 H12A 0.9500 . ? C11 C10 1.378(5) . ? C11 H11A 0.9500 . ? C10 C9 1.386(5) . ? C10 H10A 0.9500 . ? C9 C8 1.398(4) . ? C9 H9A 0.9500 . ? 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 C1 Ru1 O1 93.73(11) . . ? C1 Ru1 P1 90.84(10) . . ? O1 Ru1 P1 175.32(6) . . ? C1 Ru1 S2 110.34(9) . . ? O1 Ru1 S2 82.00(5) . . ? P1 Ru1 S2 95.48(3) . . ? C1 Ru1 S1 107.70(9) . . ? O1 Ru1 S1 80.73(6) . . ? P1 Ru1 S1 98.83(3) . . ? S2 Ru1 S1 138.96(3) . . ? C14 S1 Ru1 98.11(10) . . ? C8 S2 Ru1 100.48(10) . . ? C20 P1 C32 105.39(13) . . ? C20 P1 C26 102.05(13) . . ? C32 P1 C26 105.66(14) . . ? C20 P1 Ru1 114.93(10) . . ? C32 P1 Ru1 116.05(10) . . ? C26 P1 Ru1 111.44(9) . . ? C13 O1 C19 123.5(2) . . ? C13 O1 Ru1 118.96(16) . . ? C19 O1 Ru1 114.72(17) . . ? C33 C32 C37 108.8(2) . . ? C33 C32 P1 114.7(2) . . ? C37 C32 P1 115.3(2) . . ? C33 C32 H32A 105.7 . . ? C37 C32 H32A 105.7 . . ? P1 C32 H32A 105.7 . . ? C34 C33 C32 111.0(3) . . ? C34 C33 H33A 109.4 . . ? C32 C33 H33A 109.4 . . ? C34 C33 H33B 109.4 . . ? C32 C33 H33B 109.4 . . ? H33A C33 H33B 108.0 . . ? C35 C34 C33 112.0(3) . . ? C35 C34 H34A 109.2 . . ? C33 C34 H34A 109.2 . . ? C35 C34 H34B 109.2 . . ? C33 C34 H34B 109.2 . . ? H34A C34 H34B 107.9 . . ? C36 C35 C34 111.0(3) . . ? C36 C35 H35A 109.4 . . ? C34 C35 H35A 109.4 . . ? C36 C35 H35B 109.4 . . ? C34 C35 H35B 109.4 . . ? H35A C35 H35B 108.0 . . ? C35 C36 C37 111.4(3) . . ? C35 C36 H36A 109.3 . . ? C37 C36 H36A 109.3 . . ? C35 C36 H36B 109.3 . . ? C37 C36 H36B 109.3 . . ? H36A C36 H36B 108.0 . . ? C36 C37 C32 111.4(3) . . ? C36 C37 H37A 109.3 . . ? C32 C37 H37A 109.3 . . ? C36 C37 H37B 109.3 . . ? C32 C37 H37B 109.3 . . ? H37A C37 H37B 108.0 . . ? C25 C20 C21 110.1(3) . . ? C25 C20 P1 114.2(2) . . ? C21 C20 P1 111.9(2) . . ? C25 C20 H20A 106.7 . . ? C21 C20 H20A 106.7 . . ? P1 C20 H20A 106.7 . . ? C20 C21 C22 110.5(3) . . ? C20 C21 H21A 109.6 . . ? C22 C21 H21A 109.6 . . ? C20 C21 H21B 109.6 . . ? C22 C21 H21B 109.6 . . ? H21A C21 H21B 108.1 . . ? C23 C22 C21 111.9(3) . . ? C23 C22 H22A 109.2 . . ? C21 C22 H22A 109.2 . . ? C23 C22 H22B 109.2 . . ? C21 C22 H22B 109.2 . . ? H22A C22 H22B 107.9 . . ? C24 C23 C22 111.3(3) . . ? C24 C23 H23A 109.4 . . ? C22 C23 H23A 109.4 . . ? C24 C23 H23B 109.4 . . ? C22 C23 H23B 109.4 . . ? H23A C23 H23B 108.0 . . ? C23 C24 C25 111.4(3) . . ? C23 C24 H24A 109.3 . . ? C25 C24 H24A 109.3 . . ? C23 C24 H24B 109.3 . . ? C25 C24 H24B 109.3 . . ? H24A C24 H24B 108.0 . . ? C20 C25 C24 110.5(3) . . ? C20 C25 H25A 109.5 . . ? C24 C25 H25A 109.5 . . ? C20 C25 H25B 109.5 . . ? C24 C25 H25B 109.6 . . ? H25A C25 H25B 108.1 . . ? C27 C26 C31 109.7(3) . . ? C27 C26 P1 113.1(2) . . ? C31 C26 P1 117.0(2) . . ? C27 C26 H26A 105.3 . . ? C31 C26 H26A 105.3 . . ? P1 C26 H26A 105.3 . . ? C26 C27 C28 110.6(3) . . ? C26 C27 H27A 109.5 . . ? C28 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? C28 C27 H27B 109.5 . . ? H27A C27 H27B 108.1 . . ? C29 C28 C27 112.4(3) . . ? C29 C28 H28A 109.1 . . ? C27 C28 H28A 109.1 . . ? C29 C28 H28B 109.1 . . ? C27 C28 H28B 109.1 . . ? H28A C28 H28B 107.9 . . ? C28 C29 C30 110.2(3) . . ? C28 C29 H29A 109.6 . . ? C30 C29 H29A 109.6 . . ? C28 C29 H29B 109.6 . . ? C30 C29 H29B 109.6 . . ? H29A C29 H29B 108.1 . . ? C29 C30 C31 110.2(3) . . ? C29 C30 H30A 109.6 . . ? C31 C30 H30A 109.6 . . ? C29 C30 H30B 109.6 . . ? C31 C30 H30B 109.6 . . ? H30A C30 H30B 108.1 . . ? C26 C31 C30 110.5(3) . . ? C26 C31 H31A 109.5 . . ? C30 C31 H31A 109.5 . . ? C26 C31 H31B 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 108.1 . . ? C2 C1 Ru1 125.0(2) . . ? C2 C1 H1A 117.5 . . ? Ru1 C1 H1A 117.5 . . ? C7 C2 C3 118.5(3) . . ? C7 C2 C1 118.8(3) . . ? C3 C2 C1 122.6(3) . . ? C4 C3 C2 120.5(3) . . ? C4 C3 H3A 119.7 . . ? C2 C3 H3A 119.7 . . ? C5 C4 C3 120.4(3) . . ? C5 C4 H4A 119.8 . . ? C3 C4 H4A 119.8 . . ? C6 C5 C4 119.4(3) . . ? C6 C5 H5A 120.3 . . ? C4 C5 H5A 120.3 . . ? C5 C6 C7 120.4(3) . . ? C5 C6 H6A 119.8 . . ? C7 C6 H6A 119.8 . . ? C6 C7 C2 120.8(3) . . ? C6 C7 H7A 119.6 . . ? C2 C7 H7A 119.6 . . ? C19 C14 C15 117.4(3) . . ? C19 C14 S1 121.2(2) . . ? C15 C14 S1 121.3(2) . . ? C14 C19 C18 122.6(3) . . ? C14 C19 O1 115.2(2) . . ? C18 C19 O1 121.8(3) . . ? C17 C18 C19 118.4(3) . . ? C17 C18 H18A 120.8 . . ? C19 C18 H18A 120.8 . . ? C16 C17 C18 120.1(3) . . ? C16 C17 H17A 119.9 . . ? C18 C17 H17A 119.9 . . ? C15 C16 C17 120.4(3) . . ? C15 C16 H16A 119.8 . . ? C17 C16 H16A 119.8 . . ? C16 C15 C14 120.7(3) . . ? C16 C15 H15A 119.6 . . ? C14 C15 H15A 119.6 . . ? C8 C13 C12 121.4(3) . . ? C8 C13 O1 114.6(2) . . ? C12 C13 O1 123.8(3) . . ? C11 C12 C13 119.7(3) . . ? C11 C12 H12A 120.1 . . ? C13 C12 H12A 120.1 . . ? C10 C11 C12 119.8(3) . . ? C10 C11 H11A 120.1 . . ? C12 C11 H11A 120.1 . . ? C11 C10 C9 120.2(3) . . ? C11 C10 H10A 119.9 . . ? C9 C10 H10A 119.9 . . ? C10 C9 C8 121.5(3) . . ? C10 C9 H9A 119.3 . . ? C8 C9 H9A 119.3 . . ? C9 C8 C13 117.4(3) . . ? C9 C8 S2 119.8(2) . . ? C13 C8 S2 122.6(2) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.84 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.293 _refine_diff_density_min -0.507 _refine_diff_density_rms 0.087 _database_code_depnum_ccdc_archive 'CCDC 971469' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_cll032_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H42 Cl2 N2 Ru S3' _chemical_formula_weight 734.84 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' 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 11.0572(10) _cell_length_b 26.702(2) _cell_length_c 12.1075(11) _cell_angle_alpha 90.00 _cell_angle_beta 114.176(3) _cell_angle_gamma 90.00 _cell_volume 3261.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 0.863 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6502 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 28644 _diffrn_reflns_av_R_equivalents 0.0458 _diffrn_reflns_av_sigmaI/netI 0.0431 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 27.54 _reflns_number_total 7483 _reflns_number_gt 6329 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0471P)^2^+21.7724P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7483 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0748 _refine_ls_R_factor_gt 0.0616 _refine_ls_wR_factor_ref 0.1571 _refine_ls_wR_factor_gt 0.1498 _refine_ls_goodness_of_fit_ref 1.123 _refine_ls_restrained_S_all 1.123 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 2.80713(4) 0.163416(13) 1.96838(3) 0.01648(11) Uani 1 1 d . . . S2 S 2.62183(12) 0.20629(5) 1.95998(11) 0.0228(3) Uani 1 1 d . . . S3 S 2.83543(12) 0.23041(5) 1.85144(11) 0.0229(3) Uani 1 1 d . . . S1 S 2.86892(14) 0.11174(5) 1.84461(12) 0.0261(3) Uani 1 1 d . . . N1 N 2.6781(4) 0.06947(15) 2.0179(4) 0.0220(9) Uani 1 1 d . . . C21 C 3.0135(5) 0.09027(18) 2.2287(4) 0.0234(10) Uani 1 1 d . . . C15 C 2.5440(5) 0.08237(17) 1.9391(4) 0.0196(9) Uani 1 1 d . . . C22 C 3.0285(5) 0.11457(19) 2.3357(5) 0.0242(10) Uani 1 1 d . . . C2 C 3.0758(5) 0.21162(17) 2.1176(4) 0.0201(9) Uani 1 1 d . . . C1 C 2.9541(5) 0.18543(18) 2.1023(4) 0.0206(9) Uani 1 1 d . . . H1A H 2.9489 0.1780 2.1770 0.025 Uiso 1 1 calc R . . C12 C 2.7868(5) 0.09935(17) 2.0576(4) 0.0176(9) Uani 1 1 d . . . N2 N 2.8838(4) 0.07360(15) 2.1475(4) 0.0229(9) Uani 1 1 d . . . C7 C 3.1461(5) 0.23822(18) 2.2257(4) 0.0231(10) Uani 1 1 d . . . H7A H 3.1139 0.2384 2.2873 0.028 Uiso 1 1 calc R . . C19 C 2.3305(5) 0.11362(18) 1.9151(5) 0.0246(10) Uani 1 1 d . . . H19A H 2.2758 0.1294 1.9481 0.029 Uiso 1 1 calc R . . C16 C 2.4905(5) 0.06653(18) 1.8184(5) 0.0215(10) Uani 1 1 d . . . C17 C 2.3573(5) 0.07617(18) 1.7469(4) 0.0223(10) Uani 1 1 d . . . H17A H 2.3210 0.0665 1.6641 0.027 Uiso 1 1 calc R . . C11 C 2.6234(5) 0.26494(19) 1.8812(5) 0.0271(11) Uani 1 1 d . . . H11A H 2.5332 0.2795 1.8465 0.033 Uiso 1 1 calc R . . H11B H 2.6833 0.2893 1.9399 0.033 Uiso 1 1 calc R . . C10 C 2.6691(5) 0.2562(2) 1.7815(5) 0.0283(11) Uani 1 1 d . . . H10A H 2.6697 0.2881 1.7401 0.034 Uiso 1 1 calc R . . H10B H 2.6089 0.2325 1.7211 0.034 Uiso 1 1 calc R . . C5 C 3.3112(5) 0.2628(2) 2.1571(5) 0.0324(12) Uani 1 1 d . . . H5A H 3.3889 0.2813 2.1689 0.039 Uiso 1 1 calc R . . C18 C 2.2761(5) 0.09963(18) 1.7939(5) 0.0233(10) Uani 1 1 d . . . C9 C 2.8536(6) 0.2011(2) 1.7233(5) 0.0321(12) Uani 1 1 d . . . H9A H 2.8051 0.2210 1.6493 0.039 Uiso 1 1 calc R . . H9B H 2.9485 0.2007 1.7379 0.039 Uiso 1 1 calc R . . C25 C 3.2479(5) 0.0960(2) 2.2852(5) 0.0307(12) Uani 1 1 d . . . H25A H 3.3233 0.0894 2.2687 0.037 Uiso 1 1 calc R . . C26 C 3.1235(5) 0.07905(19) 2.2030(5) 0.0257(11) Uani 1 1 d . . . C20 C 2.4634(5) 0.10511(18) 1.9890(5) 0.0229(10) Uani 1 1 d . . . C24 C 3.2650(6) 0.1221(2) 2.3895(5) 0.0308(12) Uani 1 1 d . . . C27 C 2.5713(5) 0.0370(2) 1.7657(5) 0.0325(12) Uani 1 1 d . . . H27A H 2.5165 0.0295 1.6805 0.049 Uiso 1 1 calc R . . H27B H 2.6012 0.0056 1.8107 0.049 Uiso 1 1 calc R . . H27C H 2.6485 0.0568 1.7718 0.049 Uiso 1 1 calc R . . C29 C 2.5170(6) 0.1198(2) 2.1211(5) 0.0327(12) Uani 1 1 d . . . H29A H 2.4459 0.1349 2.1385 0.049 Uiso 1 1 calc R . . H29B H 2.5890 0.1440 2.1387 0.049 Uiso 1 1 calc R . . H29C H 2.5507 0.0900 2.1716 0.049 Uiso 1 1 calc R . . C23 C 3.1543(5) 0.1306(2) 2.4136(5) 0.0289(11) Uani 1 1 d . . . H23A H 3.1648 0.1480 2.4854 0.035 Uiso 1 1 calc R . . C8 C 2.8011(6) 0.1482(2) 1.7042(5) 0.0304(12) Uani 1 1 d . . . H8A H 2.8244 0.1317 1.6423 0.036 Uiso 1 1 calc R . . H8B H 2.7032 0.1490 1.6734 0.036 Uiso 1 1 calc R . . C6 C 3.2602(5) 0.2639(2) 2.2437(5) 0.0292(12) Uani 1 1 d . . . H6A H 3.3042 0.2824 2.3162 0.035 Uiso 1 1 calc R . . C4 C 3.2484(6) 0.2346(2) 2.0525(5) 0.0327(12) Uani 1 1 d . . . H4A H 3.2856 0.2326 1.9945 0.039 Uiso 1 1 calc R . . C3 C 3.1313(5) 0.2092(2) 2.0323(5) 0.0271(11) Uani 1 1 d . . . H3A H 3.0887 0.1902 1.9603 0.033 Uiso 1 1 calc R . . C32 C 3.1112(6) 0.0498(2) 2.0925(5) 0.0359(13) Uani 1 1 d . . . H32A H 3.0181 0.0410 2.0453 0.054 Uiso 1 1 calc R . . H32B H 3.1643 0.0192 2.1175 0.054 Uiso 1 1 calc R . . H32C H 3.1432 0.0703 2.0428 0.054 Uiso 1 1 calc R . . C14 C 2.8427(5) 0.02311(19) 2.1683(5) 0.0309(12) Uani 1 1 d . . . H14A H 2.8541 0.0190 2.2532 0.037 Uiso 1 1 calc R . . H14B H 2.8938 -0.0032 2.1486 0.037 Uiso 1 1 calc R . . C30 C 2.9109(6) 0.1265(2) 2.3634(5) 0.0322(12) Uani 1 1 d . . . H30A H 2.8306 0.1125 2.2999 0.048 Uiso 1 1 calc R . . H30B H 2.9017 0.1629 2.3667 0.048 Uiso 1 1 calc R . . H30C H 2.9240 0.1118 2.4417 0.048 Uiso 1 1 calc R . . C13 C 2.6979(6) 0.0215(2) 2.0821(6) 0.0349(13) Uani 1 1 d . . . H13A H 2.6793 -0.0070 2.0254 0.042 Uiso 1 1 calc R . . H13B H 2.6405 0.0189 2.1267 0.042 Uiso 1 1 calc R . . C28 C 2.1305(5) 0.1094(2) 1.7147(5) 0.0310(12) Uani 1 1 d . . . H28A H 2.1093 0.0971 1.6326 0.046 Uiso 1 1 calc R . . H28B H 2.1131 0.1455 1.7120 0.046 Uiso 1 1 calc R . . H28C H 2.0755 0.0920 1.7486 0.046 Uiso 1 1 calc R . . C31 C 3.3994(6) 0.1415(3) 2.4725(6) 0.0470(17) Uani 1 1 d . . . H31A H 3.3927 0.1589 2.5412 0.071 Uiso 1 1 calc R . . H31B H 3.4314 0.1649 2.4281 0.071 Uiso 1 1 calc R . . H31C H 3.4614 0.1135 2.5023 0.071 Uiso 1 1 calc R . . Cl2 Cl 3.8933(6) 0.00620(13) 2.5267(4) 0.186(3) Uani 1 1 d . . . Cl1 Cl 3.6433(6) 0.05203(17) 2.4644(4) 0.1560(19) Uani 1 1 d . . . C101 C 3.752(3) 0.0188(8) 2.5748(17) 0.273(18) Uani 1 1 d . . . H10C H 3.7122 -0.0130 2.5855 0.327 Uiso 1 1 calc R . . H10D H 3.7844 0.0377 2.6519 0.327 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 0.01501(18) 0.01625(18) 0.01668(18) 0.00125(14) 0.00495(13) -0.00154(14) S2 0.0202(6) 0.0227(6) 0.0262(6) 0.0026(5) 0.0103(5) 0.0022(5) S3 0.0212(6) 0.0230(6) 0.0220(6) 0.0051(5) 0.0063(5) -0.0028(5) S1 0.0290(7) 0.0247(6) 0.0283(6) -0.0020(5) 0.0156(5) -0.0015(5) N1 0.017(2) 0.0205(19) 0.024(2) 0.0040(16) 0.0027(16) -0.0044(16) C21 0.020(2) 0.019(2) 0.023(2) 0.0064(19) 0.0007(19) 0.0013(19) C15 0.012(2) 0.018(2) 0.025(2) 0.0037(18) 0.0049(18) -0.0040(17) C22 0.022(2) 0.026(2) 0.022(2) 0.0064(19) 0.006(2) 0.000(2) C2 0.019(2) 0.018(2) 0.018(2) 0.0033(17) 0.0025(18) 0.0019(18) C1 0.022(2) 0.019(2) 0.019(2) 0.0031(18) 0.0070(19) -0.0018(18) C12 0.015(2) 0.018(2) 0.019(2) -0.0018(17) 0.0063(18) -0.0001(17) N2 0.016(2) 0.020(2) 0.027(2) 0.0067(16) 0.0039(17) -0.0026(16) C7 0.024(3) 0.022(2) 0.023(2) 0.0003(19) 0.009(2) -0.0006(19) C19 0.023(3) 0.022(2) 0.030(3) -0.001(2) 0.011(2) 0.0000(19) C16 0.018(2) 0.021(2) 0.027(2) 0.0001(19) 0.011(2) -0.0021(18) C17 0.022(2) 0.024(2) 0.021(2) -0.0016(19) 0.0085(19) -0.0031(19) C11 0.026(3) 0.023(2) 0.030(3) 0.003(2) 0.008(2) 0.003(2) C10 0.023(3) 0.030(3) 0.028(3) 0.012(2) 0.006(2) 0.005(2) C5 0.020(3) 0.042(3) 0.031(3) 0.009(2) 0.006(2) -0.004(2) C18 0.017(2) 0.022(2) 0.030(3) 0.004(2) 0.008(2) -0.0020(19) C9 0.028(3) 0.043(3) 0.025(3) 0.007(2) 0.010(2) -0.002(2) C25 0.021(3) 0.035(3) 0.033(3) 0.002(2) 0.008(2) -0.001(2) C26 0.024(3) 0.022(2) 0.026(2) 0.003(2) 0.004(2) 0.001(2) C20 0.026(3) 0.018(2) 0.026(2) -0.0009(18) 0.011(2) -0.0031(19) C24 0.024(3) 0.034(3) 0.027(3) 0.001(2) 0.003(2) -0.008(2) C27 0.021(3) 0.040(3) 0.035(3) -0.010(2) 0.010(2) -0.002(2) C29 0.034(3) 0.034(3) 0.029(3) -0.004(2) 0.012(2) -0.007(2) C23 0.027(3) 0.033(3) 0.023(2) 0.003(2) 0.007(2) -0.004(2) C8 0.026(3) 0.041(3) 0.022(2) -0.004(2) 0.008(2) -0.002(2) C6 0.026(3) 0.028(3) 0.026(3) -0.002(2) 0.003(2) -0.006(2) C4 0.025(3) 0.046(3) 0.029(3) 0.005(2) 0.013(2) 0.003(2) C3 0.025(3) 0.032(3) 0.022(2) 0.001(2) 0.007(2) 0.001(2) C32 0.032(3) 0.035(3) 0.035(3) -0.005(2) 0.008(2) 0.005(2) C14 0.027(3) 0.020(2) 0.040(3) 0.012(2) 0.007(2) -0.005(2) C30 0.026(3) 0.042(3) 0.028(3) 0.004(2) 0.011(2) 0.002(2) C13 0.025(3) 0.023(3) 0.047(3) 0.014(2) 0.006(2) -0.005(2) C28 0.022(3) 0.034(3) 0.032(3) 0.007(2) 0.006(2) 0.005(2) C31 0.026(3) 0.069(5) 0.037(3) -0.007(3) 0.004(3) -0.019(3) Cl2 0.246(5) 0.0715(19) 0.108(3) 0.0116(19) -0.061(3) 0.009(3) Cl1 0.213(5) 0.128(3) 0.105(3) -0.037(2) 0.044(3) -0.056(3) C101 0.52(5) 0.20(2) 0.144(16) 0.085(15) 0.18(2) 0.25(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C1 1.860(5) . ? Ru1 C12 2.084(5) . ? Ru1 S2 2.3126(13) . ? Ru1 S1 2.3356(13) . ? Ru1 S3 2.3803(12) . ? S2 C11 1.838(5) . ? S3 C10 1.816(5) . ? S3 C9 1.821(6) . ? S1 C8 1.833(6) . ? N1 C12 1.357(6) . ? N1 C15 1.438(6) . ? N1 C13 1.467(6) . ? C21 C22 1.397(7) . ? C21 C26 1.406(8) . ? C21 N2 1.437(6) . ? C15 C16 1.398(7) . ? C15 C20 1.403(7) . ? C22 C23 1.391(7) . ? C22 C30 1.503(8) . ? C2 C3 1.402(7) . ? C2 C7 1.410(7) . ? C2 C1 1.459(7) . ? C12 N2 1.360(6) . ? N2 C14 1.477(6) . ? C7 C6 1.372(7) . ? C19 C18 1.390(7) . ? C19 C20 1.391(7) . ? C16 C17 1.393(7) . ? C16 C27 1.515(7) . ? C17 C18 1.393(7) . ? C11 C10 1.505(8) . ? C5 C6 1.379(8) . ? C5 C4 1.391(8) . ? C18 C28 1.521(7) . ? C9 C8 1.507(8) . ? C25 C24 1.386(8) . ? C25 C26 1.402(7) . ? C26 C32 1.506(8) . ? C20 C29 1.512(7) . ? C24 C23 1.388(8) . ? C24 C31 1.504(8) . ? C4 C3 1.391(8) . ? C14 C13 1.511(8) . ? Cl2 C101 1.91(2) . ? Cl1 C101 1.644(18) . ? 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 C1 Ru1 C12 92.78(19) . . ? C1 Ru1 S2 108.91(16) . . ? C12 Ru1 S2 98.48(13) . . ? C1 Ru1 S1 111.43(16) . . ? C12 Ru1 S1 88.26(13) . . ? S2 Ru1 S1 138.67(5) . . ? C1 Ru1 S3 90.02(15) . . ? C12 Ru1 S3 173.54(13) . . ? S2 Ru1 S3 86.09(5) . . ? S1 Ru1 S3 85.30(5) . . ? C11 S2 Ru1 104.36(18) . . ? C10 S3 C9 102.1(3) . . ? C10 S3 Ru1 101.98(18) . . ? C9 S3 Ru1 105.69(19) . . ? C8 S1 Ru1 99.50(19) . . ? C12 N1 C15 128.2(4) . . ? C12 N1 C13 114.0(4) . . ? C15 N1 C13 116.8(4) . . ? C22 C21 C26 121.3(5) . . ? C22 C21 N2 119.0(5) . . ? C26 C21 N2 119.6(5) . . ? C16 C15 C20 120.7(4) . . ? C16 C15 N1 120.0(4) . . ? C20 C15 N1 118.8(4) . . ? C23 C22 C21 118.5(5) . . ? C23 C22 C30 120.0(5) . . ? C21 C22 C30 121.3(5) . . ? C3 C2 C7 117.7(5) . . ? C3 C2 C1 123.0(5) . . ? C7 C2 C1 119.2(5) . . ? C2 C1 Ru1 133.9(4) . . ? N1 C12 N2 106.3(4) . . ? N1 C12 Ru1 124.5(3) . . ? N2 C12 Ru1 127.8(3) . . ? C12 N2 C21 129.0(4) . . ? C12 N2 C14 113.7(4) . . ? C21 N2 C14 117.2(4) . . ? C6 C7 C2 121.4(5) . . ? C18 C19 C20 121.5(5) . . ? C17 C16 C15 118.7(5) . . ? C17 C16 C27 119.4(5) . . ? C15 C16 C27 121.9(5) . . ? C18 C17 C16 121.6(5) . . ? C10 C11 S2 111.2(4) . . ? C11 C10 S3 107.1(4) . . ? C6 C5 C4 119.8(5) . . ? C19 C18 C17 118.6(5) . . ? C19 C18 C28 120.5(5) . . ? C17 C18 C28 120.8(5) . . ? C8 C9 S3 111.3(4) . . ? C24 C25 C26 122.5(5) . . ? C25 C26 C21 117.4(5) . . ? C25 C26 C32 120.2(5) . . ? C21 C26 C32 122.3(5) . . ? C19 C20 C15 118.9(5) . . ? C19 C20 C29 119.4(5) . . ? C15 C20 C29 121.7(5) . . ? C25 C24 C23 118.0(5) . . ? C25 C24 C31 120.7(6) . . ? C23 C24 C31 121.2(6) . . ? C24 C23 C22 122.1(5) . . ? C9 C8 S1 111.7(4) . . ? C7 C6 C5 120.3(5) . . ? C5 C4 C3 120.3(5) . . ? C4 C3 C2 120.3(5) . . ? N2 C14 C13 102.7(4) . . ? N1 C13 C14 103.2(4) . . ? Cl1 C101 Cl2 105.4(10) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.963 _refine_diff_density_min -2.142 _refine_diff_density_rms 0.138 #===end _database_code_depnum_ccdc_archive 'CCDC 971470'