# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Brian K Nicholson' _publ_contact_author_email B.NICHOLSON@WAIKATO.AC.NZ _publ_section_title ; Ruthenium and osmium carbonyl clusters incorporating stannylene and stannyl ligands ; loop_ _publ_author_name 'B Nicholson' 'Mohammad R. Hassan' 'Shariff E Kabir' 'Arun K Raha' 'Edward Rosenberg' ; L.Salassa ; 'Ayesha Sharmin' # Attachment 'collected_cifs.cif' data_akr20c _database_code_depnum_ccdc_archive 'CCDC 661316' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C68 H50 O8 Ru3 S2 Sn3' _chemical_formula_sum 'C68 H50 O8 Ru3 S2 Sn3' _chemical_formula_weight 1718.48 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' 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' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.826(1) _cell_length_b 13.944(1) _cell_length_c 17.434(1) _cell_angle_alpha 73.71(1) _cell_angle_beta 79.20(1) _cell_angle_gamma 82.45(1) _cell_volume 3157.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 89(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _exptl_crystal_description block _exptl_crystal_colour dark _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.807 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1672 _exptl_absorpt_coefficient_mu 1.988 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.501 _exptl_absorpt_correction_T_max 0.593 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 89(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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29546 _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_av_sigmaI/netI 0.0441 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 26.44 _reflns_number_total 12812 _reflns_number_gt 10971 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0047P)^2^+21.5020P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12812 _refine_ls_number_parameters 757 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0571 _refine_ls_R_factor_gt 0.0452 _refine_ls_wR_factor_ref 0.0971 _refine_ls_wR_factor_gt 0.0921 _refine_ls_goodness_of_fit_ref 1.155 _refine_ls_restrained_S_all 1.155 _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 Sn1 Sn 0.23157(3) 0.75452(3) 0.29480(2) 0.01918(9) Uani 1 1 d . . . Sn2 Sn 0.80673(3) 0.18388(3) 0.21112(3) 0.02307(10) Uani 1 1 d . . . Sn3 Sn 0.43312(3) 0.36996(3) 0.30174(2) 0.02176(9) Uani 1 1 d . . . Ru1 Ru 0.35160(3) 0.59272(3) 0.27509(3) 0.01757(10) Uani 1 1 d . . . Ru2 Ru 0.55026(3) 0.50563(3) 0.23317(3) 0.01819(10) Uani 1 1 d . . . Ru3 Ru 0.64933(3) 0.30509(3) 0.25044(3) 0.02016(10) Uani 1 1 d . . . S1 S 0.50197(10) 0.67654(10) 0.22016(8) 0.0197(3) Uani 1 1 d . . . S2 S 0.71076(11) 0.46455(11) 0.17254(9) 0.0221(3) Uani 1 1 d . . . O1 O 0.3851(3) 0.5943(4) 0.4445(3) 0.0358(11) Uani 1 1 d . . . O2 O 0.1739(3) 0.4709(3) 0.3429(3) 0.0336(10) Uani 1 1 d . . . O3 O 0.2927(3) 0.6400(3) 0.1056(3) 0.0304(10) Uani 1 1 d . . . O4 O 0.4823(4) 0.5116(4) 0.0740(3) 0.0529(15) Uani 1 1 d . . . O5 O 0.6056(3) 0.5105(3) 0.3944(3) 0.0325(10) Uani 1 1 d . . . O6 O 0.7454(4) 0.3171(3) 0.3934(3) 0.0354(11) Uani 1 1 d . . . O7 O 0.5688(3) 0.1117(3) 0.3607(3) 0.0361(11) Uani 1 1 d . . . O8 O 0.5877(4) 0.2899(4) 0.0932(3) 0.0389(11) Uani 1 1 d . . . C1 C 0.3732(4) 0.5914(4) 0.3818(3) 0.0221(12) Uani 1 1 d . . . C2 C 0.2426(4) 0.5141(5) 0.3190(4) 0.0249(13) Uani 1 1 d . . . C3 C 0.3163(4) 0.6206(4) 0.1676(4) 0.0207(12) Uani 1 1 d . . . C4 C 0.5086(5) 0.5087(5) 0.1328(4) 0.0315(15) Uani 1 1 d . . . C5 C 0.5857(4) 0.5061(4) 0.3349(4) 0.0210(12) Uani 1 1 d . . . C6 C 0.7082(5) 0.3123(4) 0.3416(4) 0.0289(14) Uani 1 1 d . . . C7 C 0.5954(4) 0.1855(5) 0.3169(4) 0.0275(13) Uani 1 1 d . . . C8 C 0.6090(5) 0.2942(5) 0.1520(4) 0.0287(14) Uani 1 1 d . . . C11 C 0.5109(4) 0.7468(4) 0.1160(3) 0.0218(12) Uani 1 1 d . . . C12 C 0.4399(5) 0.8243(4) 0.0913(4) 0.0266(13) Uani 1 1 d . . . H12 H 0.3845 0.8360 0.1280 0.032 Uiso 1 1 calc R . . C13 C 0.4509(5) 0.8837(5) 0.0131(4) 0.0308(14) Uani 1 1 d . . . H13 H 0.4029 0.9353 -0.0025 0.037 Uiso 1 1 calc R . . C14 C 0.5320(5) 0.8675(5) -0.0422(4) 0.0338(15) Uani 1 1 d . . . H14 H 0.5395 0.9078 -0.0951 0.041 Uiso 1 1 calc R . . C15 C 0.6026(6) 0.7896(6) -0.0177(4) 0.0411(17) Uani 1 1 d . . . H15 H 0.6578 0.7780 -0.0547 0.049 Uiso 1 1 calc R . . C16 C 0.5924(5) 0.7293(5) 0.0606(4) 0.0330(15) Uani 1 1 d . . . H16 H 0.6400 0.6772 0.0761 0.040 Uiso 1 1 calc R . . C21 C 0.8044(4) 0.5017(4) 0.2142(4) 0.0241(12) Uani 1 1 d . . . C22 C 0.7868(5) 0.5850(4) 0.2451(4) 0.0282(14) Uani 1 1 d . . . H22 H 0.7252 0.6211 0.2458 0.034 Uiso 1 1 calc R . . C23 C 0.8617(5) 0.6143(5) 0.2751(4) 0.0346(16) Uani 1 1 d . . . H23 H 0.8502 0.6704 0.2954 0.042 Uiso 1 1 calc R . . C24 C 0.9532(5) 0.5599(5) 0.2746(4) 0.0344(15) Uani 1 1 d . . . H24 H 1.0022 0.5774 0.2968 0.041 Uiso 1 1 calc R . . C25 C 0.9706(5) 0.4797(5) 0.2408(4) 0.0353(16) Uani 1 1 d . . . H25 H 1.0328 0.4448 0.2385 0.042 Uiso 1 1 calc R . . C26 C 0.8973(5) 0.4502(5) 0.2103(4) 0.0303(14) Uani 1 1 d . . . H26 H 0.9102 0.3962 0.1874 0.036 Uiso 1 1 calc R . . C31 C 0.0988(4) 0.7137(4) 0.3766(4) 0.0238(12) Uani 1 1 d . . . C32 C 0.0965(5) 0.6459(5) 0.4519(4) 0.0352(15) Uani 1 1 d . . . H32 H 0.1553 0.6126 0.4676 0.042 Uiso 1 1 calc R . . C33 C 0.0086(6) 0.6262(5) 0.5047(5) 0.0443(18) Uani 1 1 d . . . H33 H 0.0091 0.5810 0.5552 0.053 Uiso 1 1 calc R . . C34 C -0.0791(6) 0.6737(6) 0.4821(5) 0.0457(19) Uani 1 1 d . . . H34 H -0.1381 0.6604 0.5174 0.055 Uiso 1 1 calc R . . C35 C -0.0797(5) 0.7411(6) 0.4072(5) 0.0421(18) Uani 1 1 d . . . H35 H -0.1391 0.7735 0.3920 0.050 Uiso 1 1 calc R . . C36 C 0.0081(5) 0.7607(5) 0.3546(4) 0.0345(15) Uani 1 1 d . . . H36 H 0.0069 0.8057 0.3040 0.041 Uiso 1 1 calc R . . C41 C 0.2987(4) 0.8440(4) 0.3498(4) 0.0228(12) Uani 1 1 d . . . C42 C 0.2540(5) 0.8605(5) 0.4230(4) 0.0335(15) Uani 1 1 d . . . H42 H 0.1936 0.8351 0.4472 0.040 Uiso 1 1 calc R . . C43 C 0.2978(6) 0.9146(6) 0.4613(5) 0.0442(18) Uani 1 1 d . . . H43 H 0.2671 0.9240 0.5112 0.053 Uiso 1 1 calc R . . C44 C 0.3860(5) 0.9540(5) 0.4257(4) 0.0358(16) Uani 1 1 d . . . H44 H 0.4149 0.9909 0.4510 0.043 Uiso 1 1 calc R . . C45 C 0.4316(5) 0.9389(5) 0.3525(5) 0.0359(16) Uani 1 1 d . . . H45 H 0.4916 0.9653 0.3282 0.043 Uiso 1 1 calc R . . C46 C 0.3883(5) 0.8844(4) 0.3149(4) 0.0289(14) Uani 1 1 d . . . H46 H 0.4197 0.8747 0.2653 0.035 Uiso 1 1 calc R . . C51 C 0.1835(4) 0.8489(4) 0.1863(4) 0.0239(12) Uani 1 1 d . . . C52 C 0.2133(5) 0.9459(5) 0.1533(4) 0.0283(13) Uani 1 1 d . . . H52 H 0.2519 0.9711 0.1802 0.034 Uiso 1 1 calc R . . C53 C 0.1863(5) 1.0051(5) 0.0809(4) 0.0356(15) Uani 1 1 d . . . H53 H 0.2076 1.0691 0.0594 0.043 Uiso 1 1 calc R . . C54 C 0.1279(5) 0.9693(5) 0.0408(4) 0.0361(16) Uani 1 1 d . . . H54 H 0.1094 1.0095 -0.0074 0.043 Uiso 1 1 calc R . . C55 C 0.0971(5) 0.8743(5) 0.0719(4) 0.0343(15) Uani 1 1 d . . . H55 H 0.0580 0.8502 0.0446 0.041 Uiso 1 1 calc R . . C56 C 0.1246(4) 0.8141(5) 0.1444(4) 0.0259(13) Uani 1 1 d . . . H56 H 0.1034 0.7499 0.1652 0.031 Uiso 1 1 calc R . . C61 C 0.8999(4) 0.2534(4) 0.1010(4) 0.0257(13) Uani 1 1 d . . . C62 C 0.8652(5) 0.3297(5) 0.0392(4) 0.0333(15) Uani 1 1 d . . . H62 H 0.7986 0.3524 0.0447 0.040 Uiso 1 1 calc R . . C63 C 0.9280(5) 0.3725(5) -0.0304(4) 0.0396(17) Uani 1 1 d . . . H63 H 0.9035 0.4240 -0.0706 0.048 Uiso 1 1 calc R . . C64 C 1.0274(5) 0.3387(5) -0.0405(4) 0.0394(16) Uani 1 1 d . . . H64 H 1.0698 0.3677 -0.0871 0.047 Uiso 1 1 calc R . . C65 C 1.0626(5) 0.2619(5) 0.0193(5) 0.0385(16) Uani 1 1 d . . . H65 H 1.1291 0.2389 0.0131 0.046 Uiso 1 1 calc R . . C66 C 0.9990(5) 0.2184(5) 0.0890(4) 0.0330(15) Uani 1 1 d . . . H66 H 1.0233 0.1652 0.1281 0.040 Uiso 1 1 calc R . . C71 C 0.9052(5) 0.1335(5) 0.2984(4) 0.0282(13) Uani 1 1 d . . . C72 C 0.9587(6) 0.1968(6) 0.3174(5) 0.053(2) Uani 1 1 d . . . H72 H 0.9477 0.2651 0.2938 0.063 Uiso 1 1 calc R . . C73 C 1.0282(6) 0.1671(6) 0.3693(5) 0.052(2) Uani 1 1 d . . . H73 H 1.0613 0.2141 0.3806 0.062 Uiso 1 1 calc R . . C74 C 1.0462(9) 0.0696(7) 0.4024(6) 0.081(4) Uani 1 1 d . . . H74 H 1.0945 0.0479 0.4354 0.097 Uiso 1 1 calc R . . C75 C 0.9944(12) 0.0010(7) 0.3883(8) 0.127(7) Uani 1 1 d . . . H75 H 1.0063 -0.0669 0.4127 0.153 Uiso 1 1 calc R . . C76 C 0.9232(9) 0.0334(7) 0.3370(6) 0.073(3) Uani 1 1 d . . . H76 H 0.8873 -0.0136 0.3286 0.088 Uiso 1 1 calc R . . C81 C 0.7686(5) 0.0464(4) 0.1934(4) 0.0262(13) Uani 1 1 d . . . C82 C 0.8439(5) -0.0287(5) 0.1847(4) 0.0311(14) Uani 1 1 d . . . H82 H 0.9081 -0.0198 0.1884 0.037 Uiso 1 1 calc R . . C83 C 0.8237(6) -0.1171(5) 0.1704(4) 0.0395(17) Uani 1 1 d . . . H83 H 0.8746 -0.1666 0.1651 0.047 Uiso 1 1 calc R . . C84 C 0.7297(5) -0.1319(5) 0.1642(4) 0.0342(15) Uani 1 1 d . . . H84 H 0.7169 -0.1915 0.1554 0.041 Uiso 1 1 calc R . . C85 C 0.6548(6) -0.0587(5) 0.1708(4) 0.0358(16) Uani 1 1 d . . . H85 H 0.5912 -0.0678 0.1656 0.043 Uiso 1 1 calc R . . C86 C 0.6744(5) 0.0300(5) 0.1855(4) 0.0343(15) Uani 1 1 d . . . H86 H 0.6230 0.0793 0.1900 0.041 Uiso 1 1 calc R . . C91 C 0.3449(5) 0.3016(5) 0.2456(4) 0.0298(14) Uani 1 1 d . . . C92 C 0.3483(5) 0.1963(5) 0.2662(4) 0.0326(15) Uani 1 1 d . . . H92 H 0.3954 0.1583 0.2966 0.039 Uiso 1 1 calc R . . C93 C 0.2823(5) 0.1487(5) 0.2416(4) 0.0366(16) Uani 1 1 d . . . H93 H 0.2848 0.0790 0.2566 0.044 Uiso 1 1 calc R . . C94 C 0.2136(5) 0.2027(5) 0.1958(4) 0.0369(16) Uani 1 1 d . . . H94 H 0.1689 0.1700 0.1805 0.044 Uiso 1 1 calc R . . C95 C 0.2108(5) 0.3074(5) 0.1719(5) 0.0388(17) Uani 1 1 d . . . H95 H 0.1651 0.3451 0.1400 0.047 Uiso 1 1 calc R . . C96 C 0.2778(5) 0.3540(5) 0.1968(4) 0.0346(15) Uani 1 1 d . . . H96 H 0.2772 0.4235 0.1796 0.042 Uiso 1 1 calc R . . C101 C 0.3961(4) 0.2942(4) 0.4279(4) 0.0249(13) Uani 1 1 d . . . C102 C 0.3327(5) 0.2167(5) 0.4530(4) 0.0358(15) Uani 1 1 d . . . H102 H 0.3033 0.2005 0.4149 0.043 Uiso 1 1 calc R . . C103 C 0.3131(5) 0.1637(5) 0.5340(4) 0.0408(17) Uani 1 1 d . . . H103 H 0.2717 0.1119 0.5496 0.049 Uiso 1 1 calc R . . C104 C 0.3545(5) 0.1877(5) 0.5901(4) 0.0384(16) Uani 1 1 d . . . H104 H 0.3414 0.1520 0.6442 0.046 Uiso 1 1 calc R . . C105 C 0.4152(6) 0.2642(6) 0.5678(5) 0.0473(19) Uani 1 1 d . . . H105 H 0.4417 0.2816 0.6068 0.057 Uiso 1 1 calc R . . C106 C 0.4371(6) 0.3156(5) 0.4868(4) 0.0382(16) Uani 1 1 d . . . H106 H 0.4806 0.3656 0.4720 0.046 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 Sn1 0.01908(19) 0.01746(19) 0.0215(2) -0.00456(15) -0.00507(15) -0.00180(15) Sn2 0.0214(2) 0.0202(2) 0.0297(2) -0.00943(17) -0.00717(17) 0.00172(16) Sn3 0.0206(2) 0.0209(2) 0.0270(2) -0.00876(16) -0.00671(16) -0.00355(15) Ru1 0.0178(2) 0.0170(2) 0.0183(2) -0.00401(17) -0.00552(17) -0.00064(17) Ru2 0.0182(2) 0.0179(2) 0.0201(2) -0.00637(18) -0.00667(18) 0.00053(17) Ru3 0.0185(2) 0.0175(2) 0.0273(2) -0.00901(19) -0.00649(18) -0.00047(17) S1 0.0210(7) 0.0183(7) 0.0199(7) -0.0034(5) -0.0049(5) -0.0027(5) S2 0.0209(7) 0.0210(7) 0.0241(7) -0.0063(6) -0.0034(6) -0.0002(6) O1 0.038(3) 0.044(3) 0.026(2) -0.009(2) -0.011(2) 0.002(2) O2 0.028(2) 0.029(2) 0.042(3) -0.006(2) -0.001(2) -0.009(2) O3 0.036(3) 0.033(2) 0.025(2) -0.0102(19) -0.011(2) 0.002(2) O4 0.061(4) 0.070(4) 0.036(3) -0.029(3) -0.024(3) 0.023(3) O5 0.039(3) 0.035(3) 0.028(2) -0.010(2) -0.018(2) -0.001(2) O6 0.046(3) 0.030(2) 0.034(3) -0.003(2) -0.024(2) -0.003(2) O7 0.035(3) 0.025(2) 0.049(3) -0.007(2) -0.008(2) -0.007(2) O8 0.046(3) 0.038(3) 0.041(3) -0.018(2) -0.019(2) 0.001(2) C1 0.021(3) 0.021(3) 0.022(3) -0.002(2) -0.003(2) -0.002(2) C2 0.023(3) 0.026(3) 0.027(3) -0.010(3) -0.004(2) 0.000(3) C3 0.017(3) 0.016(3) 0.030(3) -0.009(2) -0.003(2) -0.003(2) C4 0.030(3) 0.038(4) 0.029(4) -0.018(3) -0.009(3) 0.013(3) C5 0.022(3) 0.014(3) 0.028(3) -0.005(2) -0.007(2) 0.000(2) C6 0.026(3) 0.019(3) 0.041(4) -0.004(3) -0.009(3) -0.002(2) C7 0.023(3) 0.025(3) 0.037(4) -0.011(3) -0.007(3) 0.001(3) C8 0.029(3) 0.022(3) 0.037(4) -0.011(3) -0.010(3) 0.003(3) C11 0.021(3) 0.019(3) 0.023(3) -0.001(2) -0.001(2) -0.007(2) C12 0.027(3) 0.026(3) 0.025(3) -0.004(3) -0.002(3) -0.004(3) C13 0.033(4) 0.024(3) 0.035(4) -0.003(3) -0.011(3) -0.005(3) C14 0.043(4) 0.033(4) 0.023(3) -0.003(3) -0.003(3) -0.010(3) C15 0.041(4) 0.044(4) 0.030(4) -0.003(3) 0.006(3) -0.006(3) C16 0.026(3) 0.034(4) 0.030(3) 0.002(3) 0.000(3) 0.001(3) C21 0.019(3) 0.019(3) 0.033(3) -0.002(2) -0.004(2) -0.006(2) C22 0.023(3) 0.021(3) 0.040(4) -0.007(3) -0.006(3) -0.003(2) C23 0.042(4) 0.017(3) 0.049(4) -0.010(3) -0.013(3) -0.006(3) C24 0.027(3) 0.027(3) 0.052(4) -0.009(3) -0.012(3) -0.008(3) C25 0.023(3) 0.025(3) 0.057(5) -0.009(3) -0.009(3) 0.001(3) C26 0.024(3) 0.023(3) 0.044(4) -0.007(3) -0.007(3) -0.003(3) C31 0.023(3) 0.018(3) 0.032(3) -0.009(2) -0.004(2) -0.004(2) C32 0.030(4) 0.035(4) 0.033(4) -0.003(3) 0.004(3) -0.001(3) C33 0.044(4) 0.035(4) 0.041(4) 0.001(3) 0.009(3) -0.002(3) C34 0.037(4) 0.049(5) 0.050(5) -0.020(4) 0.016(3) -0.016(4) C35 0.018(3) 0.062(5) 0.046(4) -0.017(4) -0.002(3) 0.001(3) C36 0.030(4) 0.042(4) 0.030(4) -0.008(3) -0.006(3) -0.002(3) C41 0.025(3) 0.014(3) 0.031(3) -0.006(2) -0.011(3) 0.003(2) C42 0.036(4) 0.036(4) 0.032(4) -0.012(3) -0.004(3) -0.011(3) C43 0.063(5) 0.041(4) 0.036(4) -0.016(3) -0.016(4) -0.008(4) C44 0.046(4) 0.025(3) 0.045(4) -0.012(3) -0.025(3) -0.003(3) C45 0.030(4) 0.027(3) 0.056(5) -0.013(3) -0.013(3) -0.006(3) C46 0.026(3) 0.023(3) 0.039(4) -0.011(3) -0.006(3) -0.003(3) C51 0.022(3) 0.022(3) 0.026(3) -0.006(2) -0.006(2) 0.003(2) C52 0.030(3) 0.024(3) 0.031(3) -0.006(3) -0.008(3) 0.000(3) C53 0.038(4) 0.025(3) 0.039(4) -0.003(3) -0.006(3) 0.001(3) C54 0.044(4) 0.029(3) 0.030(4) -0.001(3) -0.012(3) 0.007(3) C55 0.034(4) 0.044(4) 0.028(3) -0.013(3) -0.013(3) 0.002(3) C56 0.022(3) 0.027(3) 0.029(3) -0.007(3) -0.004(3) -0.002(2) C61 0.026(3) 0.022(3) 0.032(3) -0.009(3) -0.012(3) 0.000(2) C62 0.031(4) 0.033(4) 0.036(4) -0.015(3) -0.002(3) 0.004(3) C63 0.045(4) 0.033(4) 0.036(4) -0.003(3) -0.007(3) 0.002(3) C64 0.040(4) 0.041(4) 0.033(4) -0.004(3) 0.002(3) -0.009(3) C65 0.028(4) 0.034(4) 0.052(4) -0.007(3) -0.008(3) -0.004(3) C66 0.031(4) 0.028(3) 0.039(4) -0.002(3) -0.012(3) -0.005(3) C71 0.033(3) 0.026(3) 0.026(3) -0.008(3) -0.010(3) 0.004(3) C72 0.057(5) 0.035(4) 0.071(6) 0.001(4) -0.040(5) -0.012(4) C73 0.054(5) 0.049(5) 0.063(5) -0.014(4) -0.033(4) -0.008(4) C74 0.126(9) 0.049(5) 0.088(7) -0.025(5) -0.084(7) 0.030(6) C75 0.238(17) 0.038(5) 0.147(12) -0.022(7) -0.162(13) 0.023(8) C76 0.124(9) 0.042(5) 0.069(6) -0.008(4) -0.067(6) -0.001(5) C81 0.033(3) 0.019(3) 0.026(3) -0.003(2) -0.006(3) -0.002(2) C82 0.030(3) 0.026(3) 0.036(4) -0.005(3) -0.003(3) -0.003(3) C83 0.048(4) 0.018(3) 0.047(4) -0.008(3) 0.002(3) 0.000(3) C84 0.051(4) 0.019(3) 0.030(3) -0.003(3) 0.000(3) -0.010(3) C85 0.047(4) 0.025(3) 0.039(4) -0.006(3) -0.015(3) -0.011(3) C86 0.035(4) 0.024(3) 0.046(4) -0.008(3) -0.016(3) 0.002(3) C91 0.023(3) 0.035(4) 0.037(4) -0.017(3) -0.004(3) -0.006(3) C92 0.037(4) 0.022(3) 0.042(4) -0.006(3) -0.014(3) -0.005(3) C93 0.041(4) 0.032(4) 0.042(4) -0.012(3) -0.011(3) -0.010(3) C94 0.028(4) 0.040(4) 0.054(4) -0.024(3) -0.014(3) -0.003(3) C95 0.034(4) 0.038(4) 0.054(5) -0.024(4) -0.020(3) 0.006(3) C96 0.037(4) 0.027(3) 0.044(4) -0.013(3) -0.011(3) -0.001(3) C101 0.028(3) 0.019(3) 0.027(3) -0.004(2) -0.009(3) 0.004(2) C102 0.030(4) 0.036(4) 0.043(4) -0.011(3) -0.007(3) -0.009(3) C103 0.038(4) 0.034(4) 0.042(4) -0.002(3) 0.005(3) -0.008(3) C104 0.038(4) 0.033(4) 0.036(4) -0.001(3) -0.001(3) 0.002(3) C105 0.072(6) 0.038(4) 0.038(4) -0.010(3) -0.017(4) -0.012(4) C106 0.054(5) 0.030(4) 0.033(4) -0.004(3) -0.011(3) -0.016(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 Sn1 C31 2.136(6) . ? Sn1 C51 2.143(6) . ? Sn1 C41 2.156(6) . ? Sn1 Ru1 2.6832(6) . ? Sn2 C71 2.142(6) . ? Sn2 C61 2.154(6) . ? Sn2 C81 2.169(6) . ? Sn2 Ru3 2.6808(7) . ? Sn3 C91 2.152(6) . ? Sn3 C101 2.152(6) . ? Sn3 Ru2 2.5380(7) . ? Sn3 Ru3 3.0488(7) . ? Sn3 Ru1 3.0986(7) . ? Ru1 C2 1.895(6) . ? Ru1 C1 1.934(6) . ? Ru1 C3 1.945(6) . ? Ru1 S1 2.4227(15) . ? Ru1 Ru2 2.9020(7) . ? Ru2 C5 1.927(6) . ? Ru2 C4 1.930(6) . ? Ru2 S2 2.3445(15) . ? Ru2 S1 2.3477(14) . ? Ru2 Ru3 2.9090(7) . ? Ru3 C7 1.896(6) . ? Ru3 C6 1.949(7) . ? Ru3 C8 1.950(6) . ? Ru3 S2 2.4248(15) . ? S1 C11 1.795(6) . ? S2 C21 1.792(6) . ? O1 C1 1.147(7) . ? O2 C2 1.140(7) . ? O3 C3 1.138(7) . ? O4 C4 1.139(7) . ? O5 C5 1.142(7) . ? O6 C6 1.141(7) . ? O7 C7 1.154(7) . ? O8 C8 1.138(7) . ? C11 C16 1.382(8) . ? C11 C12 1.392(8) . ? C12 C13 1.374(9) . ? C13 C14 1.375(9) . ? C14 C15 1.390(10) . ? C15 C16 1.381(9) . ? C21 C26 1.386(8) . ? C21 C22 1.388(8) . ? C22 C23 1.395(9) . ? C23 C24 1.387(9) . ? C24 C25 1.379(9) . ? C25 C26 1.384(9) . ? C31 C32 1.384(9) . ? C31 C36 1.404(9) . ? C32 C33 1.387(9) . ? C33 C34 1.372(11) . ? C34 C35 1.380(11) . ? C35 C36 1.385(9) . ? C41 C42 1.376(9) . ? C41 C46 1.390(8) . ? C42 C43 1.391(9) . ? C43 C44 1.370(10) . ? C44 C45 1.373(10) . ? C45 C46 1.381(9) . ? C51 C52 1.397(8) . ? C51 C56 1.399(8) . ? C52 C53 1.387(9) . ? C53 C54 1.380(10) . ? C54 C55 1.374(10) . ? C55 C56 1.396(9) . ? C61 C66 1.391(9) . ? C61 C62 1.393(9) . ? C62 C63 1.384(10) . ? C63 C64 1.388(10) . ? C64 C65 1.378(10) . ? C65 C66 1.393(10) . ? C71 C72 1.365(9) . ? C71 C76 1.382(10) . ? C72 C73 1.387(10) . ? C73 C74 1.329(12) . ? C74 C75 1.366(14) . ? C75 C76 1.399(13) . ? C81 C86 1.390(9) . ? C81 C82 1.395(9) . ? C82 C83 1.396(9) . ? C83 C84 1.370(10) . ? C84 C85 1.367(10) . ? C85 C86 1.400(9) . ? C91 C96 1.373(9) . ? C91 C92 1.407(9) . ? C92 C93 1.386(9) . ? C93 C94 1.367(10) . ? C94 C95 1.399(10) . ? C95 C96 1.391(9) . ? C101 C106 1.379(9) . ? C101 C102 1.402(9) . ? C102 C103 1.392(10) . ? C103 C104 1.357(10) . ? C104 C105 1.368(10) . ? C105 C106 1.388(10) . ? 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 C31 Sn1 C51 105.1(2) . . ? C31 Sn1 C41 104.5(2) . . ? C51 Sn1 C41 108.9(2) . . ? C31 Sn1 Ru1 111.69(15) . . ? C51 Sn1 Ru1 114.80(16) . . ? C41 Sn1 Ru1 111.26(15) . . ? C71 Sn2 C61 104.1(2) . . ? C71 Sn2 C81 104.0(2) . . ? C61 Sn2 C81 105.8(2) . . ? C71 Sn2 Ru3 115.38(16) . . ? C61 Sn2 Ru3 112.89(16) . . ? C81 Sn2 Ru3 113.62(17) . . ? C91 Sn3 C101 102.4(2) . . ? C91 Sn3 Ru2 127.67(18) . . ? C101 Sn3 Ru2 129.93(16) . . ? C91 Sn3 Ru3 107.70(17) . . ? C101 Sn3 Ru3 106.58(16) . . ? Ru2 Sn3 Ru3 61.961(17) . . ? C91 Sn3 Ru1 106.58(18) . . ? C101 Sn3 Ru1 108.76(15) . . ? Ru2 Sn3 Ru1 61.018(17) . . ? Ru3 Sn3 Ru1 122.98(2) . . ? C2 Ru1 C1 91.6(2) . . ? C2 Ru1 C3 90.2(2) . . ? C1 Ru1 C3 168.4(2) . . ? C2 Ru1 S1 173.89(18) . . ? C1 Ru1 S1 88.23(17) . . ? C3 Ru1 S1 91.18(17) . . ? C2 Ru1 Sn1 88.57(18) . . ? C1 Ru1 Sn1 81.02(17) . . ? C3 Ru1 Sn1 87.62(16) . . ? S1 Ru1 Sn1 97.45(4) . . ? C2 Ru1 Ru2 122.55(18) . . ? C1 Ru1 Ru2 92.90(17) . . ? C3 Ru1 Ru2 95.74(16) . . ? S1 Ru1 Ru2 51.36(4) . . ? Sn1 Ru1 Ru2 148.59(2) . . ? C2 Ru1 Sn3 72.81(18) . . ? C1 Ru1 Sn3 90.67(17) . . ? C3 Ru1 Sn3 100.77(16) . . ? S1 Ru1 Sn3 101.07(4) . . ? Sn1 Ru1 Sn3 159.44(2) . . ? Ru2 Ru1 Sn3 49.912(16) . . ? C5 Ru2 C4 177.2(2) . . ? C5 Ru2 S2 96.00(17) . . ? C4 Ru2 S2 86.72(19) . . ? C5 Ru2 S1 85.17(16) . . ? C4 Ru2 S1 92.91(19) . . ? S2 Ru2 S1 116.94(5) . . ? C5 Ru2 Sn3 92.07(17) . . ? C4 Ru2 Sn3 87.2(2) . . ? S2 Ru2 Sn3 120.47(4) . . ? S1 Ru2 Sn3 122.49(4) . . ? C5 Ru2 Ru1 92.11(17) . . ? C4 Ru2 Ru1 85.07(18) . . ? S2 Ru2 Ru1 167.10(4) . . ? S1 Ru2 Ru1 53.71(4) . . ? Sn3 Ru2 Ru1 69.070(18) . . ? C5 Ru2 Ru3 88.98(16) . . ? C4 Ru2 Ru3 93.28(19) . . ? S2 Ru2 Ru3 53.68(4) . . ? S1 Ru2 Ru3 168.37(4) . . ? Sn3 Ru2 Ru3 67.678(18) . . ? Ru1 Ru2 Ru3 136.75(2) . . ? C7 Ru3 C6 88.1(3) . . ? C7 Ru3 C8 94.8(3) . . ? C6 Ru3 C8 172.1(3) . . ? C7 Ru3 S2 175.68(19) . . ? C6 Ru3 S2 89.96(18) . . ? C8 Ru3 S2 87.64(19) . . ? C7 Ru3 Sn2 85.14(18) . . ? C6 Ru3 Sn2 88.57(19) . . ? C8 Ru3 Sn2 84.34(18) . . ? S2 Ru3 Sn2 98.65(4) . . ? C7 Ru3 Ru2 125.07(18) . . ? C6 Ru3 Ru2 92.49(18) . . ? C8 Ru3 Ru2 91.87(18) . . ? S2 Ru3 Ru2 51.17(4) . . ? Sn2 Ru3 Ru2 149.78(2) . . ? C7 Ru3 Sn3 75.75(18) . . ? C6 Ru3 Sn3 101.54(19) . . ? C8 Ru3 Sn3 86.33(19) . . ? S2 Ru3 Sn3 100.90(4) . . ? Sn2 Ru3 Sn3 157.92(2) . . ? Ru2 Ru3 Sn3 50.362(16) . . ? C11 S1 Ru2 111.7(2) . . ? C11 S1 Ru1 115.02(19) . . ? Ru2 S1 Ru1 74.92(4) . . ? C21 S2 Ru2 113.0(2) . . ? C21 S2 Ru3 113.6(2) . . ? Ru2 S2 Ru3 75.15(5) . . ? O1 C1 Ru1 177.5(5) . . ? O2 C2 Ru1 176.3(6) . . ? O3 C3 Ru1 177.1(5) . . ? O4 C4 Ru2 178.6(6) . . ? O5 C5 Ru2 177.2(5) . . ? O6 C6 Ru3 177.8(6) . . ? O7 C7 Ru3 174.6(5) . . ? O8 C8 Ru3 177.8(6) . . ? C16 C11 C12 119.2(5) . . ? C16 C11 S1 120.2(5) . . ? C12 C11 S1 120.4(5) . . ? C13 C12 C11 120.6(6) . . ? C12 C13 C14 120.7(6) . . ? C13 C14 C15 118.7(6) . . ? C16 C15 C14 121.1(7) . . ? C15 C16 C11 119.6(6) . . ? C26 C21 C22 120.0(6) . . ? C26 C21 S2 119.2(5) . . ? C22 C21 S2 120.7(5) . . ? C21 C22 C23 119.8(6) . . ? C24 C23 C22 120.1(6) . . ? C25 C24 C23 119.3(6) . . ? C24 C25 C26 121.1(6) . . ? C25 C26 C21 119.5(6) . . ? C32 C31 C36 117.3(6) . . ? C32 C31 Sn1 124.0(5) . . ? C36 C31 Sn1 118.7(5) . . ? C31 C32 C33 121.7(7) . . ? C34 C33 C32 119.9(7) . . ? C33 C34 C35 120.0(7) . . ? C34 C35 C36 120.1(7) . . ? C35 C36 C31 121.0(6) . . ? C42 C41 C46 117.8(6) . . ? C42 C41 Sn1 120.0(5) . . ? C46 C41 Sn1 122.2(4) . . ? C41 C42 C43 121.2(7) . . ? C44 C43 C42 120.1(7) . . ? C43 C44 C45 119.7(6) . . ? C44 C45 C46 120.0(6) . . ? C45 C46 C41 121.2(6) . . ? C52 C51 C56 117.7(5) . . ? C52 C51 Sn1 121.0(4) . . ? C56 C51 Sn1 121.2(4) . . ? C53 C52 C51 121.0(6) . . ? C54 C53 C52 120.2(6) . . ? C55 C54 C53 120.2(6) . . ? C54 C55 C56 119.9(6) . . ? C55 C56 C51 121.0(6) . . ? C66 C61 C62 117.7(6) . . ? C66 C61 Sn2 118.9(5) . . ? C62 C61 Sn2 123.3(5) . . ? C63 C62 C61 121.3(6) . . ? C62 C63 C64 120.3(7) . . ? C65 C64 C63 119.2(7) . . ? C64 C65 C66 120.4(7) . . ? C61 C66 C65 121.1(6) . . ? C72 C71 C76 114.7(7) . . ? C72 C71 Sn2 122.9(5) . . ? C76 C71 Sn2 122.4(5) . . ? C71 C72 C73 125.0(7) . . ? C74 C73 C72 118.3(8) . . ? C73 C74 C75 120.7(8) . . ? C74 C75 C76 119.7(9) . . ? C71 C76 C75 121.6(9) . . ? C86 C81 C82 117.2(6) . . ? C86 C81 Sn2 124.2(5) . . ? C82 C81 Sn2 118.5(5) . . ? C81 C82 C83 120.7(6) . . ? C84 C83 C82 120.8(6) . . ? C85 C84 C83 119.8(6) . . ? C84 C85 C86 119.7(7) . . ? C81 C86 C85 121.8(6) . . ? C96 C91 C92 117.3(6) . . ? C96 C91 Sn3 124.1(5) . . ? C92 C91 Sn3 118.3(5) . . ? C93 C92 C91 120.6(6) . . ? C94 C93 C92 120.9(6) . . ? C93 C94 C95 119.7(6) . . ? C96 C95 C94 118.7(6) . . ? C91 C96 C95 122.7(6) . . ? C106 C101 C102 117.2(6) . . ? C106 C101 Sn3 121.9(5) . . ? C102 C101 Sn3 120.8(5) . . ? C103 C102 C101 120.9(6) . . ? C104 C103 C102 120.0(7) . . ? C103 C104 C105 120.4(7) . . ? C104 C105 C106 119.9(7) . . ? C101 C106 C105 121.5(6) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 26.44 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 2.460 _refine_diff_density_min -1.282 _refine_diff_density_rms 0.142 #===END data_akr18g _database_code_depnum_ccdc_archive 'CCDC 661317' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H23 N O9 Os3 S Sn' _chemical_formula_sum 'C35 H23 N O9 Os3 S Sn' _chemical_formula_weight 1322.89 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' 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' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.9339(2) _cell_length_b 22.8143(2) _cell_length_c 14.4812(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.212(1) _cell_angle_gamma 90.00 _cell_volume 3597.39(9) _cell_formula_units_Z 4 _cell_measurement_temperature 89(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.443 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2424 _exptl_absorpt_coefficient_mu 11.361 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.1074 _exptl_absorpt_correction_T_max 0.1727 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 89(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 'BRUKER SMART CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21313 _diffrn_reflns_av_R_equivalents 0.0235 _diffrn_reflns_av_sigmaI/netI 0.0254 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 26.33 _reflns_number_total 7303 _reflns_number_gt 6640 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0116P)^2^+10.3200P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7303 _refine_ls_number_parameters 452 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0254 _refine_ls_R_factor_gt 0.0204 _refine_ls_wR_factor_ref 0.0454 _refine_ls_wR_factor_gt 0.0435 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.110 _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 Os1 Os 0.903359(14) 0.211645(7) 0.840393(11) 0.01335(4) Uani 1 1 d . . . Os2 Os 0.948877(14) 0.258587(7) 0.650117(11) 0.01392(4) Uani 1 1 d . . . Os3 Os 0.985150(14) 0.388139(7) 0.630545(11) 0.01543(4) Uani 1 1 d . . . Sn1 Sn 0.91296(2) 0.338923(12) 0.790033(19) 0.01372(6) Uani 1 1 d . . . S1 S 0.92691(9) 0.15952(4) 0.69874(7) 0.01468(19) Uani 1 1 d . . . C1 C 0.8636(4) 0.25328(18) 0.9473(3) 0.0185(9) Uani 1 1 d . . . C2 C 1.0713(4) 0.21283(18) 0.8800(3) 0.0170(8) Uani 1 1 d . . . C3 C 1.1255(4) 0.25416(19) 0.6841(3) 0.0196(9) Uani 1 1 d . . . C4 C 0.7710(4) 0.26166(17) 0.6212(3) 0.0169(8) Uani 1 1 d . . . C5 C 0.9724(4) 0.25784(19) 0.5224(3) 0.0207(9) Uani 1 1 d . . . C6 C 1.1545(4) 0.3826(2) 0.6855(3) 0.0234(10) Uani 1 1 d . . . C7 C 0.8119(4) 0.38696(18) 0.5826(3) 0.0204(9) Uani 1 1 d . . . C8 C 0.9763(4) 0.4656(2) 0.6786(3) 0.0217(9) Uani 1 1 d . . . C9 C 1.0344(4) 0.38996(19) 0.5047(3) 0.0238(10) Uani 1 1 d . . . O1 O 0.8395(3) 0.27567(14) 1.0147(2) 0.0293(8) Uani 1 1 d . . . O2 O 1.1744(3) 0.21100(14) 0.9042(2) 0.0240(7) Uani 1 1 d . . . O3 O 1.2288(3) 0.24918(15) 0.7037(2) 0.0297(8) Uani 1 1 d . . . O4 O 0.6668(3) 0.26138(14) 0.6050(2) 0.0241(7) Uani 1 1 d . . . O5 O 0.9841(3) 0.25873(14) 0.4442(2) 0.0267(7) Uani 1 1 d . . . O6 O 1.2532(3) 0.38046(16) 0.7182(3) 0.0342(8) Uani 1 1 d . . . O7 O 0.7126(3) 0.38668(14) 0.5536(3) 0.0325(8) Uani 1 1 d . . . O8 O 0.9724(3) 0.51191(14) 0.7091(2) 0.0301(8) Uani 1 1 d . . . O9 O 1.0588(3) 0.39367(16) 0.4296(2) 0.0345(8) Uani 1 1 d . . . C11 C 0.8845(4) 0.13250(18) 0.9165(3) 0.0154(8) Uani 1 1 d . . . C12 C 0.8308(4) 0.08242(18) 0.8722(3) 0.0195(9) Uani 1 1 d . . . H12 H 0.8014 0.0845 0.8086 0.023 Uiso 1 1 calc R . . C13 C 0.8202(4) 0.0300(2) 0.9201(3) 0.0243(10) Uani 1 1 d . . . H13 H 0.7850 -0.0033 0.8885 0.029 Uiso 1 1 calc R . . C14 C 0.8606(4) 0.0259(2) 1.0137(3) 0.0236(10) Uani 1 1 d . . . H14 H 0.8529 -0.0098 1.0463 0.028 Uiso 1 1 calc R . . C15 C 0.9125(4) 0.0747(2) 1.0589(3) 0.0232(10) Uani 1 1 d . . . H15 H 0.9403 0.0724 1.1229 0.028 Uiso 1 1 calc R . . C16 C 0.9239(4) 0.12699(19) 1.0108(3) 0.0197(9) Uani 1 1 d . . . H16 H 0.9595 0.1600 1.0430 0.024 Uiso 1 1 calc R . . C21 C 1.0642(4) 0.11774(18) 0.6913(3) 0.0173(9) Uani 1 1 d . . . C22 C 1.1016(4) 0.1079(2) 0.6026(3) 0.0249(10) Uani 1 1 d . . . H22 H 1.0619 0.1276 0.5504 0.030 Uiso 1 1 calc R . . C23 C 1.1972(4) 0.0691(2) 0.5918(4) 0.0326(12) Uani 1 1 d . . . H23 H 1.2214 0.0617 0.5315 0.039 Uiso 1 1 calc R . . C24 C 1.2573(4) 0.0412(2) 0.6671(3) 0.0260(10) Uani 1 1 d . . . H24 H 1.3233 0.0152 0.6588 0.031 Uiso 1 1 calc R . . C25 C 1.2210(4) 0.0514(2) 0.7555(3) 0.0257(10) Uani 1 1 d . . . H25 H 1.2629 0.0325 0.8076 0.031 Uiso 1 1 calc R . . C26 C 1.1237(4) 0.08911(19) 0.7679(3) 0.0202(9) Uani 1 1 d . . . H26 H 1.0980 0.0953 0.8280 0.024 Uiso 1 1 calc R . . C31 C 0.7351(4) 0.37578(18) 0.8137(3) 0.0164(8) Uani 1 1 d . . . C32 C 0.7189(4) 0.43677(18) 0.8068(3) 0.0202(9) Uani 1 1 d . . . H32 H 0.7861 0.4609 0.7941 0.024 Uiso 1 1 calc R . . C33 C 0.6055(4) 0.4623(2) 0.8183(3) 0.0255(10) Uani 1 1 d . . . H33 H 0.5962 0.5036 0.8132 0.031 Uiso 1 1 calc R . . C34 C 0.5065(4) 0.4280(2) 0.8371(3) 0.0235(10) Uani 1 1 d . . . H34 H 0.4294 0.4456 0.8450 0.028 Uiso 1 1 calc R . . C35 C 0.5206(4) 0.3685(2) 0.8440(3) 0.0234(10) Uani 1 1 d . . . H35 H 0.4527 0.3446 0.8566 0.028 Uiso 1 1 calc R . . C36 C 0.6343(4) 0.3425(2) 0.8329(3) 0.0212(9) Uani 1 1 d . . . H36 H 0.6426 0.3011 0.8386 0.025 Uiso 1 1 calc R . . C41 C 1.0352(4) 0.37031(18) 0.9061(3) 0.0176(9) Uani 1 1 d . . . C42 C 0.9893(4) 0.4087(2) 0.9697(4) 0.0324(12) Uani 1 1 d . . . H42 H 0.9049 0.4192 0.9627 0.039 Uiso 1 1 calc R . . C43 C 1.0655(5) 0.4319(2) 1.0433(4) 0.0395(13) Uani 1 1 d . . . H43 H 1.0327 0.4576 1.0864 0.047 Uiso 1 1 calc R . . C44 C 1.1881(4) 0.4174(2) 1.0536(4) 0.0305(11) Uani 1 1 d . . . H44 H 1.2402 0.4334 1.1032 0.037 Uiso 1 1 calc R . . C45 C 1.2354(4) 0.3793(2) 0.9913(3) 0.0260(10) Uani 1 1 d . . . H45 H 1.3199 0.3691 0.9984 0.031 Uiso 1 1 calc R . . C46 C 1.1593(4) 0.35616(19) 0.9188(3) 0.0207(9) Uani 1 1 d . . . H46 H 1.1926 0.3300 0.8767 0.025 Uiso 1 1 calc R . . N1 N 0.7169(3) 0.19859(15) 0.7953(2) 0.0164(7) Uani 1 1 d . . . C51 C 0.6185(4) 0.18570(19) 0.7691(3) 0.0192(9) Uani 1 1 d . . . C52 C 0.4932(4) 0.1702(2) 0.7339(4) 0.0301(11) Uani 1 1 d . . . H52A H 0.4777 0.1834 0.6695 0.045 Uiso 1 1 calc R . . H52B H 0.4350 0.1891 0.7719 0.045 Uiso 1 1 calc R . . H52C H 0.4830 0.1275 0.7366 0.045 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 Os1 0.01349(8) 0.01390(8) 0.01288(8) 0.00053(6) 0.00234(6) 0.00030(6) Os2 0.01446(8) 0.01392(8) 0.01363(8) 0.00087(6) 0.00267(6) 0.00042(6) Os3 0.01451(8) 0.01533(8) 0.01666(9) 0.00147(6) 0.00256(6) -0.00144(6) Sn1 0.01195(13) 0.01475(13) 0.01463(14) -0.00076(10) 0.00212(10) -0.00083(10) S1 0.0153(5) 0.0143(5) 0.0145(5) 0.0002(4) 0.0019(4) 0.0009(4) C1 0.017(2) 0.015(2) 0.023(2) -0.0005(17) 0.0035(18) 0.0015(16) C2 0.020(2) 0.014(2) 0.016(2) -0.0004(16) 0.0016(17) -0.0041(16) C3 0.021(2) 0.021(2) 0.018(2) 0.0009(17) 0.0059(18) 0.0012(17) C4 0.022(2) 0.013(2) 0.015(2) 0.0024(16) 0.0035(17) -0.0005(16) C5 0.020(2) 0.017(2) 0.025(3) -0.0002(18) 0.0046(19) 0.0021(17) C6 0.020(2) 0.025(2) 0.026(2) 0.0028(19) 0.008(2) -0.0057(18) C7 0.022(2) 0.011(2) 0.028(2) -0.0024(17) 0.0006(19) 0.0012(16) C8 0.017(2) 0.023(2) 0.025(2) 0.0022(19) 0.0015(18) -0.0051(17) C9 0.026(2) 0.017(2) 0.029(3) 0.0033(18) 0.007(2) -0.0027(18) O1 0.040(2) 0.0291(18) 0.0197(17) -0.0034(14) 0.0102(15) 0.0053(15) O2 0.0168(16) 0.0299(18) 0.0248(17) 0.0013(14) -0.0008(13) -0.0015(13) O3 0.0195(17) 0.038(2) 0.0322(19) 0.0017(15) 0.0042(15) 0.0033(14) O4 0.0197(16) 0.0274(17) 0.0246(17) 0.0076(13) -0.0014(13) -0.0020(13) O5 0.042(2) 0.0206(17) 0.0185(17) 0.0007(13) 0.0082(15) 0.0026(14) O6 0.0192(17) 0.044(2) 0.039(2) 0.0117(17) -0.0003(15) -0.0074(15) O7 0.0242(18) 0.0185(17) 0.052(2) -0.0050(15) -0.0127(17) 0.0010(13) O8 0.0310(18) 0.0179(17) 0.040(2) -0.0049(15) -0.0013(16) -0.0048(14) O9 0.046(2) 0.036(2) 0.0231(19) 0.0018(15) 0.0130(17) -0.0055(17) C11 0.0152(19) 0.016(2) 0.017(2) 0.0044(16) 0.0073(16) 0.0007(15) C12 0.024(2) 0.018(2) 0.017(2) 0.0021(17) 0.0012(18) -0.0022(17) C13 0.024(2) 0.020(2) 0.029(3) 0.0005(19) 0.001(2) -0.0008(18) C14 0.023(2) 0.020(2) 0.029(3) 0.0112(19) 0.0062(19) 0.0039(18) C15 0.023(2) 0.028(2) 0.020(2) 0.0074(19) 0.0052(18) 0.0057(18) C16 0.018(2) 0.024(2) 0.018(2) -0.0015(17) 0.0033(17) 0.0028(17) C21 0.0128(19) 0.017(2) 0.023(2) -0.0004(17) 0.0031(17) -0.0007(16) C22 0.026(2) 0.034(3) 0.015(2) 0.0033(19) 0.0022(19) 0.002(2) C23 0.028(3) 0.044(3) 0.027(3) 0.001(2) 0.012(2) 0.006(2) C24 0.016(2) 0.028(2) 0.034(3) 0.000(2) 0.006(2) 0.0071(18) C25 0.024(2) 0.026(2) 0.028(3) 0.0030(19) 0.003(2) 0.0060(19) C26 0.022(2) 0.021(2) 0.018(2) 0.0014(17) 0.0037(18) 0.0007(17) C31 0.0138(19) 0.021(2) 0.014(2) 0.0005(16) 0.0013(16) 0.0013(16) C32 0.016(2) 0.017(2) 0.029(2) -0.0013(18) 0.0052(18) -0.0019(16) C33 0.024(2) 0.019(2) 0.033(3) -0.0026(19) 0.003(2) 0.0060(18) C34 0.015(2) 0.027(2) 0.028(2) 0.0000(19) 0.0018(18) 0.0055(17) C35 0.018(2) 0.023(2) 0.031(3) 0.0047(19) 0.0059(19) -0.0001(17) C36 0.019(2) 0.020(2) 0.026(2) 0.0018(18) 0.0029(18) 0.0010(17) C41 0.020(2) 0.016(2) 0.016(2) -0.0013(16) -0.0014(17) -0.0028(16) C42 0.022(2) 0.042(3) 0.032(3) -0.013(2) -0.004(2) 0.009(2) C43 0.045(3) 0.041(3) 0.031(3) -0.022(2) -0.007(2) 0.013(3) C44 0.031(3) 0.022(2) 0.035(3) -0.007(2) -0.016(2) 0.000(2) C45 0.020(2) 0.029(3) 0.029(3) 0.000(2) -0.002(2) 0.0032(18) C46 0.022(2) 0.021(2) 0.019(2) 0.0002(17) 0.0015(18) 0.0040(17) N1 0.0174(18) 0.0148(17) 0.0179(18) 0.0025(14) 0.0060(15) 0.0030(14) C51 0.023(2) 0.017(2) 0.018(2) 0.0008(17) 0.0047(18) 0.0013(17) C52 0.017(2) 0.039(3) 0.033(3) -0.001(2) -0.004(2) -0.001(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 Os1 C2 1.873(4) . ? Os1 C1 1.899(4) . ? Os1 N1 2.105(4) . ? Os1 C11 2.135(4) . ? Os1 S1 2.4050(10) . ? Os1 Sn1 2.9981(3) . ? Os1 Os2 3.0391(2) . ? Os2 C5 1.890(5) . ? Os2 C3 1.952(4) . ? Os2 C4 1.953(4) . ? Os2 S1 2.3860(10) . ? Os2 Sn1 2.7862(3) . ? Os2 Os3 2.9990(2) . ? Os3 C8 1.904(5) . ? Os3 C9 1.947(5) . ? Os3 C6 1.952(5) . ? Os3 C7 1.957(4) . ? Os3 Sn1 2.7476(3) . ? Sn1 C41 2.171(4) . ? Sn1 C31 2.174(4) . ? S1 C21 1.790(4) . ? C1 O1 1.154(5) . ? C2 O2 1.151(5) . ? C3 O3 1.145(5) . ? C4 O4 1.141(5) . ? C5 O5 1.152(5) . ? C6 O6 1.139(5) . ? C7 O7 1.128(5) . ? C8 O8 1.148(5) . ? C9 O9 1.145(6) . ? C11 C16 1.401(6) . ? C11 C12 1.411(6) . ? C12 C13 1.393(6) . ? C13 C14 1.390(7) . ? C14 C15 1.385(7) . ? C15 C16 1.393(6) . ? C21 C26 1.396(6) . ? C21 C22 1.401(6) . ? C22 C23 1.389(7) . ? C23 C24 1.377(7) . ? C24 C25 1.394(7) . ? C25 C26 1.393(6) . ? C31 C36 1.388(6) . ? C31 C32 1.405(6) . ? C32 C33 1.393(6) . ? C33 C34 1.383(6) . ? C34 C35 1.370(6) . ? C35 C36 1.400(6) . ? C41 C46 1.391(6) . ? C41 C42 1.396(6) . ? C42 C43 1.397(7) . ? C43 C44 1.375(7) . ? C44 C45 1.385(7) . ? C45 C46 1.384(6) . ? N1 C51 1.145(5) . ? C51 C52 1.461(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Os1 C1 91.92(18) . . ? C2 Os1 N1 172.67(15) . . ? C1 Os1 N1 92.11(16) . . ? C2 Os1 C11 89.55(17) . . ? C1 Os1 C11 87.86(17) . . ? N1 Os1 C11 84.49(14) . . ? C2 Os1 S1 95.19(13) . . ? C1 Os1 S1 172.88(13) . . ? N1 Os1 S1 80.86(10) . . ? C11 Os1 S1 92.56(11) . . ? C2 Os1 Sn1 90.32(12) . . ? C1 Os1 Sn1 74.30(13) . . ? N1 Os1 Sn1 96.66(9) . . ? C11 Os1 Sn1 162.15(11) . . ? S1 Os1 Sn1 105.23(2) . . ? C2 Os1 Os2 92.06(13) . . ? C1 Os1 Os2 129.11(13) . . ? N1 Os1 Os2 90.14(9) . . ? C11 Os1 Os2 142.88(11) . . ? S1 Os1 Os2 50.35(2) . . ? Sn1 Os1 Os2 54.965(7) . . ? C5 Os2 C3 91.51(18) . . ? C5 Os2 C4 90.69(18) . . ? C3 Os2 C4 177.61(17) . . ? C5 Os2 S1 107.85(13) . . ? C3 Os2 S1 90.03(13) . . ? C4 Os2 S1 88.41(12) . . ? C5 Os2 Sn1 139.30(13) . . ? C3 Os2 Sn1 93.01(13) . . ? C4 Os2 Sn1 85.92(12) . . ? S1 Os2 Sn1 112.57(3) . . ? C5 Os2 Os3 83.42(13) . . ? C3 Os2 Os3 86.47(13) . . ? C4 Os2 Os3 94.71(12) . . ? S1 Os2 Os3 168.30(3) . . ? Sn1 Os2 Os3 56.565(7) . . ? C5 Os2 Os1 158.74(13) . . ? C3 Os2 Os1 89.61(13) . . ? C4 Os2 Os1 88.00(12) . . ? S1 Os2 Os1 50.91(2) . . ? Sn1 Os2 Os1 61.769(7) . . ? Os3 Os2 Os1 117.836(7) . . ? C8 Os3 C9 110.48(19) . . ? C8 Os3 C6 89.38(19) . . ? C9 Os3 C6 92.91(19) . . ? C8 Os3 C7 93.59(18) . . ? C9 Os3 C7 90.52(19) . . ? C6 Os3 C7 174.38(18) . . ? C8 Os3 Sn1 92.51(14) . . ? C9 Os3 Sn1 156.99(13) . . ? C6 Os3 Sn1 87.97(13) . . ? C7 Os3 Sn1 87.14(14) . . ? C8 Os3 Os2 150.24(14) . . ? C9 Os3 Os2 99.19(13) . . ? C6 Os3 Os2 91.48(13) . . ? C7 Os3 Os2 83.57(12) . . ? Sn1 Os3 Os2 57.808(7) . . ? C41 Sn1 C31 104.30(16) . . ? C41 Sn1 Os3 108.19(11) . . ? C31 Sn1 Os3 107.68(11) . . ? C41 Sn1 Os2 131.47(11) . . ? C31 Sn1 Os2 123.79(11) . . ? Os3 Sn1 Os2 65.627(8) . . ? C41 Sn1 Os1 99.43(11) . . ? C31 Sn1 Os1 106.54(11) . . ? Os3 Sn1 Os1 128.270(11) . . ? Os2 Sn1 Os1 63.266(7) . . ? C21 S1 Os2 112.28(14) . . ? C21 S1 Os1 118.03(15) . . ? Os2 S1 Os1 78.74(3) . . ? O1 C1 Os1 176.2(4) . . ? O2 C2 Os1 177.1(4) . . ? O3 C3 Os2 177.3(4) . . ? O4 C4 Os2 177.6(4) . . ? O5 C5 Os2 177.9(4) . . ? O6 C6 Os3 178.6(4) . . ? O7 C7 Os3 178.8(4) . . ? O8 C8 Os3 178.6(4) . . ? O9 C9 Os3 176.1(4) . . ? C16 C11 C12 116.6(4) . . ? C16 C11 Os1 122.9(3) . . ? C12 C11 Os1 120.4(3) . . ? C13 C12 C11 121.3(4) . . ? C14 C13 C12 120.5(4) . . ? C15 C14 C13 119.2(4) . . ? C14 C15 C16 120.2(4) . . ? C15 C16 C11 122.1(4) . . ? C26 C21 C22 120.0(4) . . ? C26 C21 S1 122.3(3) . . ? C22 C21 S1 117.2(3) . . ? C23 C22 C21 119.4(4) . . ? C24 C23 C22 121.0(5) . . ? C23 C24 C25 119.6(4) . . ? C26 C25 C24 120.4(4) . . ? C25 C26 C21 119.6(4) . . ? C36 C31 C32 117.3(4) . . ? C36 C31 Sn1 123.9(3) . . ? C32 C31 Sn1 118.7(3) . . ? C33 C32 C31 120.9(4) . . ? C34 C33 C32 120.5(4) . . ? C35 C34 C33 119.4(4) . . ? C34 C35 C36 120.4(4) . . ? C31 C36 C35 121.4(4) . . ? C46 C41 C42 117.5(4) . . ? C46 C41 Sn1 123.4(3) . . ? C42 C41 Sn1 119.0(3) . . ? C41 C42 C43 121.1(4) . . ? C44 C43 C42 119.9(5) . . ? C43 C44 C45 119.9(4) . . ? C46 C45 C44 119.9(4) . . ? C45 C46 C41 121.6(4) . . ? C51 N1 Os1 173.0(3) . . ? N1 C51 C52 178.7(5) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.33 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.656 _refine_diff_density_min -1.086 _refine_diff_density_rms 0.131 #===END data_akr29b _database_code_depnum_ccdc_archive 'CCDC 661318' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C55 H42 O6 P2 Ru3 S2 Sn, C H2 Cl2' _chemical_formula_sum 'C56 H44 Cl2 O6 P2 Ru3 S2 Sn' _chemical_formula_weight 1431.77 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9706(3) _cell_length_b 12.1970(3) _cell_length_c 19.8844(5) _cell_angle_alpha 101.979(1) _cell_angle_beta 103.852(1) _cell_angle_gamma 92.297(1) _cell_volume 2745.07(12) _cell_formula_units_Z 2 _cell_measurement_temperature 89(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.732 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1412 _exptl_absorpt_coefficient_mu 1.540 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.700 _exptl_absorpt_correction_T_max 0.781 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 89(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 'Bruker SMART CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26441 _diffrn_reflns_av_R_equivalents 0.0200 _diffrn_reflns_av_sigmaI/netI 0.0274 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.08 _diffrn_reflns_theta_max 26.31 _reflns_number_total 11038 _reflns_number_gt 9692 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0180P)^2^+3.8844P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11038 _refine_ls_number_parameters 649 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0299 _refine_ls_R_factor_gt 0.0224 _refine_ls_wR_factor_ref 0.0536 _refine_ls_wR_factor_gt 0.0501 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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 Sn1 Sn 0.173989(14) 0.494549(14) 0.311863(9) 0.01462(4) Uani 1 1 d . . . Ru1 Ru 0.371809(16) 0.585594(16) 0.305915(10) 0.01296(5) Uani 1 1 d . . . Ru2 Ru 0.472589(16) 0.764021(16) 0.256124(10) 0.01182(5) Uani 1 1 d . . . Ru3 Ru 0.255906(16) 0.760605(16) 0.168740(10) 0.01176(5) Uani 1 1 d . . . P1 P 0.48756(5) 0.95875(5) 0.27323(3) 0.01217(12) Uani 1 1 d . . . P2 P 0.23579(5) 0.95223(5) 0.19121(3) 0.01255(12) Uani 1 1 d . . . S2 S 0.29615(5) 0.76711(5) 0.29758(3) 0.01366(12) Uani 1 1 d . . . S1 S 0.34669(5) 0.59924(5) 0.18684(3) 0.01337(12) Uani 1 1 d . . . O1 O 0.45684(18) 0.35361(17) 0.28592(11) 0.0310(5) Uani 1 1 d . . . O2 O 0.43987(18) 0.62317(17) 0.46613(10) 0.0304(5) Uani 1 1 d . . . O3 O 0.64541(17) 0.76847(17) 0.39774(10) 0.0274(4) Uani 1 1 d . . . O4 O 0.66622(16) 0.72756(16) 0.18096(10) 0.0261(4) Uani 1 1 d . . . O5 O 0.33065(16) 0.76567(15) 0.03400(9) 0.0210(4) Uani 1 1 d . . . O6 O -0.00140(17) 0.68314(18) 0.10327(11) 0.0300(5) Uani 1 1 d . . . C1 C 0.4280(2) 0.4432(2) 0.29602(14) 0.0198(5) Uani 1 1 d . . . C2 C 0.4123(2) 0.6098(2) 0.40508(14) 0.0187(5) Uani 1 1 d . . . C3 C 0.5781(2) 0.7597(2) 0.34450(14) 0.0179(5) Uani 1 1 d . . . C4 C 0.5917(2) 0.7430(2) 0.20848(13) 0.0181(5) Uani 1 1 d . . . C5 C 0.2989(2) 0.7654(2) 0.08430(13) 0.0157(5) Uani 1 1 d . . . C6 C 0.0939(2) 0.7125(2) 0.12939(13) 0.0186(5) Uani 1 1 d . . . C7 C 0.3488(2) 1.0219(2) 0.27121(13) 0.0145(5) Uani 1 1 d . . . H7A H 0.3234 1.0150 0.3141 0.017 Uiso 1 1 calc R . . H7B H 0.3602 1.1031 0.2719 0.017 Uiso 1 1 calc R . . C11 C 0.5814(2) 1.0280(2) 0.36012(13) 0.0154(5) Uani 1 1 d . . . C12 C 0.5383(2) 1.0609(2) 0.41999(14) 0.0225(6) Uani 1 1 d . . . H12 H 0.4573 1.0535 0.4152 0.027 Uiso 1 1 calc R . . C13 C 0.6135(3) 1.1045(2) 0.48681(14) 0.0269(6) Uani 1 1 d . . . H13 H 0.5833 1.1265 0.5271 0.032 Uiso 1 1 calc R . . C14 C 0.7320(3) 1.1158(2) 0.49460(15) 0.0268(6) Uani 1 1 d . . . H14 H 0.7828 1.1469 0.5399 0.032 Uiso 1 1 calc R . . C15 C 0.7759(2) 1.0813(2) 0.43581(15) 0.0275(6) Uani 1 1 d . . . H15 H 0.8570 1.0877 0.4411 0.033 Uiso 1 1 calc R . . C16 C 0.7014(2) 1.0375(2) 0.36917(14) 0.0227(6) Uani 1 1 d . . . H16 H 0.7323 1.0137 0.3293 0.027 Uiso 1 1 calc R . . C21 C 0.5458(2) 1.0238(2) 0.21170(13) 0.0139(5) Uani 1 1 d . . . C22 C 0.5443(2) 0.9628(2) 0.14356(13) 0.0164(5) Uani 1 1 d . . . H22 H 0.5173 0.8851 0.1295 0.020 Uiso 1 1 calc R . . C23 C 0.5823(2) 1.0155(2) 0.09634(14) 0.0213(6) Uani 1 1 d . . . H23 H 0.5816 0.9733 0.0503 0.026 Uiso 1 1 calc R . . C24 C 0.6211(2) 1.1287(2) 0.11561(15) 0.0238(6) Uani 1 1 d . . . H24 H 0.6468 1.1641 0.0830 0.029 Uiso 1 1 calc R . . C25 C 0.6223(2) 1.1908(2) 0.18326(15) 0.0219(6) Uani 1 1 d . . . H25 H 0.6485 1.2686 0.1965 0.026 Uiso 1 1 calc R . . C26 C 0.5853(2) 1.1392(2) 0.23131(14) 0.0166(5) Uani 1 1 d . . . H26 H 0.5867 1.1817 0.2774 0.020 Uiso 1 1 calc R . . C31 C 0.2420(2) 1.0237(2) 0.11999(13) 0.0155(5) Uani 1 1 d . . . C32 C 0.3066(2) 1.1265(2) 0.13042(14) 0.0176(5) Uani 1 1 d . . . H32 H 0.3547 1.1605 0.1761 0.021 Uiso 1 1 calc R . . C33 C 0.3009(2) 1.1791(2) 0.07404(15) 0.0219(6) Uani 1 1 d . . . H33 H 0.3456 1.2487 0.0814 0.026 Uiso 1 1 calc R . . C34 C 0.2302(2) 1.1307(2) 0.00710(14) 0.0230(6) Uani 1 1 d . . . H34 H 0.2270 1.1668 -0.0312 0.028 Uiso 1 1 calc R . . C35 C 0.1642(2) 1.0291(2) -0.00372(14) 0.0233(6) Uani 1 1 d . . . H35 H 0.1152 0.9961 -0.0493 0.028 Uiso 1 1 calc R . . C36 C 0.1704(2) 0.9760(2) 0.05238(13) 0.0185(5) Uani 1 1 d . . . H36 H 0.1254 0.9065 0.0448 0.022 Uiso 1 1 calc R . . C41 C 0.0978(2) 0.9939(2) 0.20850(12) 0.0145(5) Uani 1 1 d . . . C42 C 0.0514(2) 1.0902(2) 0.19007(13) 0.0177(5) Uani 1 1 d . . . H42 H 0.0960 1.1404 0.1738 0.021 Uiso 1 1 calc R . . C43 C -0.0596(2) 1.1134(2) 0.19532(14) 0.0213(6) Uani 1 1 d . . . H43 H -0.0902 1.1793 0.1831 0.026 Uiso 1 1 calc R . . C44 C -0.1255(2) 1.0394(2) 0.21860(14) 0.0239(6) Uani 1 1 d . . . H44 H -0.2021 1.0537 0.2209 0.029 Uiso 1 1 calc R . . C45 C -0.0794(2) 0.9449(2) 0.23847(15) 0.0247(6) Uani 1 1 d . . . H45 H -0.1242 0.8952 0.2549 0.030 Uiso 1 1 calc R . . C46 C 0.0322(2) 0.9226(2) 0.23436(14) 0.0196(5) Uani 1 1 d . . . H46 H 0.0640 0.8588 0.2492 0.024 Uiso 1 1 calc R . . C51 C 0.1905(2) 0.3529(2) 0.36272(13) 0.0181(5) Uani 1 1 d . . . C52 C 0.0934(2) 0.2763(2) 0.35029(14) 0.0217(6) Uani 1 1 d . . . H52 H 0.0213 0.2897 0.3222 0.026 Uiso 1 1 calc R . . C53 C 0.1016(3) 0.1803(2) 0.37881(15) 0.0267(6) Uani 1 1 d . . . H53 H 0.0356 0.1280 0.3691 0.032 Uiso 1 1 calc R . . C54 C 0.2058(3) 0.1614(2) 0.42118(15) 0.0259(6) Uani 1 1 d . . . H54 H 0.2113 0.0962 0.4405 0.031 Uiso 1 1 calc R . . C55 C 0.3020(3) 0.2374(2) 0.43531(14) 0.0245(6) Uani 1 1 d . . . H55 H 0.3731 0.2251 0.4650 0.029 Uiso 1 1 calc R . . C56 C 0.2947(2) 0.3323(2) 0.40597(14) 0.0229(6) Uani 1 1 d . . . H56 H 0.3613 0.3836 0.4155 0.028 Uiso 1 1 calc R . . C61 C 0.0749(2) 0.6064(2) 0.36800(13) 0.0186(5) Uani 1 1 d . . . C62 C 0.0211(3) 0.6923(2) 0.33984(15) 0.0266(6) Uani 1 1 d . . . H62 H 0.0278 0.7016 0.2946 0.032 Uiso 1 1 calc R . . C63 C -0.0420(3) 0.7647(3) 0.37676(16) 0.0315(7) Uani 1 1 d . . . H63 H -0.0781 0.8225 0.3566 0.038 Uiso 1 1 calc R . . C64 C -0.0524(3) 0.7526(3) 0.44296(16) 0.0286(6) Uani 1 1 d . . . H64 H -0.0958 0.8016 0.4681 0.034 Uiso 1 1 calc R . . C65 C 0.0009(3) 0.6686(3) 0.47203(15) 0.0289(6) Uani 1 1 d . . . H65 H -0.0053 0.6603 0.5175 0.035 Uiso 1 1 calc R . . C66 C 0.0638(2) 0.5959(2) 0.43476(14) 0.0248(6) Uani 1 1 d . . . H66 H 0.0997 0.5383 0.4552 0.030 Uiso 1 1 calc R . . C71 C 0.0661(2) 0.4338(2) 0.20532(13) 0.0181(5) Uani 1 1 d . . . C72 C 0.1133(2) 0.3790(2) 0.15116(14) 0.0213(6) Uani 1 1 d . . . H72 H 0.1927 0.3661 0.1619 0.026 Uiso 1 1 calc R . . C73 C 0.0459(2) 0.3426(2) 0.08138(15) 0.0270(6) Uani 1 1 d . . . H73 H 0.0791 0.3051 0.0451 0.032 Uiso 1 1 calc R . . C74 C -0.0701(3) 0.3618(3) 0.06546(15) 0.0320(7) Uani 1 1 d . . . H74 H -0.1161 0.3382 0.0180 0.038 Uiso 1 1 calc R . . C75 C -0.1190(2) 0.4150(3) 0.11835(16) 0.0318(7) Uani 1 1 d . . . H75 H -0.1986 0.4273 0.1073 0.038 Uiso 1 1 calc R . . C76 C -0.0511(2) 0.4507(2) 0.18805(15) 0.0250(6) Uani 1 1 d . . . H76 H -0.0852 0.4869 0.2242 0.030 Uiso 1 1 calc R . . C81 C 0.3856(2) 0.5061(2) 0.11578(13) 0.0151(5) Uani 1 1 d . . . C82 C 0.3054(2) 0.4792(2) 0.04944(13) 0.0169(5) Uani 1 1 d . . . H82 H 0.2321 0.5084 0.0433 0.020 Uiso 1 1 calc R . . C83 C 0.3341(2) 0.4090(2) -0.00776(13) 0.0191(5) Uani 1 1 d . . . H83 H 0.2803 0.3902 -0.0530 0.023 Uiso 1 1 calc R . . C84 C 0.4421(2) 0.3664(2) 0.00177(14) 0.0203(5) Uani 1 1 d . . . H84 H 0.4618 0.3189 -0.0371 0.024 Uiso 1 1 calc R . . C85 C 0.5207(2) 0.3935(2) 0.06808(14) 0.0190(5) Uani 1 1 d . . . H85 H 0.5939 0.3642 0.0742 0.023 Uiso 1 1 calc R . . C86 C 0.4929(2) 0.4634(2) 0.12580(14) 0.0175(5) Uani 1 1 d . . . H86 H 0.5465 0.4815 0.1712 0.021 Uiso 1 1 calc R . . C9 C 0.7239(4) 0.5005(3) 0.3871(2) 0.0509(10) Uani 1 1 d . . . H9A H 0.7886 0.5488 0.4230 0.061 Uiso 1 1 calc R . . H9B H 0.6508 0.5275 0.3961 0.061 Uiso 1 1 calc R . . Cl1 Cl 0.73134(8) 0.51370(9) 0.30089(5) 0.0510(2) Uani 1 1 d . . . Cl2 Cl 0.73075(13) 0.36099(10) 0.39696(7) 0.0906(5) 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 Sn1 0.01403(8) 0.01636(9) 0.01330(8) 0.00347(6) 0.00329(6) -0.00018(6) Ru1 0.01335(10) 0.01335(10) 0.01258(9) 0.00330(7) 0.00374(7) 0.00106(7) Ru2 0.01121(9) 0.01239(9) 0.01193(9) 0.00209(7) 0.00361(7) 0.00110(7) Ru3 0.01151(9) 0.01221(9) 0.01124(9) 0.00185(7) 0.00301(7) 0.00060(7) P1 0.0111(3) 0.0131(3) 0.0117(3) 0.0015(2) 0.0031(2) 0.0004(2) P2 0.0112(3) 0.0138(3) 0.0128(3) 0.0025(2) 0.0037(2) 0.0014(2) S2 0.0136(3) 0.0147(3) 0.0132(3) 0.0023(2) 0.0051(2) 0.0013(2) S1 0.0150(3) 0.0125(3) 0.0126(3) 0.0018(2) 0.0043(2) 0.0014(2) O1 0.0371(12) 0.0218(11) 0.0392(12) 0.0087(9) 0.0164(10) 0.0118(9) O2 0.0391(12) 0.0323(11) 0.0162(10) 0.0053(8) 0.0009(9) -0.0002(9) O3 0.0257(11) 0.0318(11) 0.0216(10) 0.0098(9) -0.0024(8) -0.0032(9) O4 0.0231(10) 0.0292(11) 0.0295(11) 0.0041(9) 0.0149(9) 0.0050(8) O5 0.0242(10) 0.0234(10) 0.0164(9) 0.0035(8) 0.0081(8) 0.0017(8) O6 0.0183(10) 0.0367(12) 0.0302(11) 0.0035(9) 0.0015(8) -0.0059(9) C1 0.0203(13) 0.0219(14) 0.0180(13) 0.0054(11) 0.0054(10) 0.0022(11) C2 0.0174(13) 0.0167(13) 0.0219(14) 0.0058(10) 0.0039(10) -0.0008(10) C3 0.0172(13) 0.0165(13) 0.0215(13) 0.0048(10) 0.0077(11) 0.0016(10) C4 0.0210(13) 0.0141(12) 0.0178(13) 0.0028(10) 0.0034(11) 0.0011(10) C5 0.0138(12) 0.0129(12) 0.0179(13) 0.0005(10) 0.0016(10) 0.0019(9) C6 0.0215(14) 0.0192(13) 0.0164(12) 0.0048(10) 0.0064(11) 0.0015(11) C7 0.0137(12) 0.0153(12) 0.0138(12) -0.0002(9) 0.0051(9) 0.0014(9) C11 0.0176(12) 0.0119(11) 0.0151(12) 0.0022(9) 0.0024(10) -0.0008(9) C12 0.0222(14) 0.0256(14) 0.0175(13) 0.0006(11) 0.0047(11) 0.0023(11) C13 0.0345(16) 0.0266(15) 0.0157(13) -0.0022(11) 0.0047(12) 0.0039(12) C14 0.0324(16) 0.0216(14) 0.0183(13) 0.0009(11) -0.0050(12) -0.0025(12) C15 0.0194(14) 0.0327(16) 0.0263(15) 0.0073(12) -0.0010(11) -0.0069(12) C16 0.0175(13) 0.0288(15) 0.0208(13) 0.0051(11) 0.0037(11) -0.0013(11) C21 0.0100(11) 0.0167(12) 0.0157(12) 0.0054(10) 0.0030(9) 0.0016(9) C22 0.0131(12) 0.0188(12) 0.0180(12) 0.0052(10) 0.0042(10) 0.0028(10) C23 0.0199(13) 0.0300(15) 0.0163(13) 0.0081(11) 0.0058(10) 0.0076(11) C24 0.0204(13) 0.0322(15) 0.0276(15) 0.0182(12) 0.0118(11) 0.0084(12) C25 0.0193(13) 0.0185(13) 0.0318(15) 0.0117(11) 0.0082(11) 0.0036(10) C26 0.0135(12) 0.0171(12) 0.0192(12) 0.0038(10) 0.0040(10) 0.0032(10) C31 0.0152(12) 0.0181(12) 0.0151(12) 0.0044(10) 0.0065(10) 0.0044(10) C32 0.0143(12) 0.0182(13) 0.0211(13) 0.0046(10) 0.0058(10) 0.0026(10) C33 0.0194(13) 0.0207(13) 0.0297(15) 0.0105(11) 0.0098(11) 0.0037(11) C34 0.0267(14) 0.0268(14) 0.0220(14) 0.0133(12) 0.0108(11) 0.0077(11) C35 0.0267(15) 0.0252(14) 0.0163(13) 0.0040(11) 0.0026(11) 0.0051(11) C36 0.0201(13) 0.0174(12) 0.0188(13) 0.0044(10) 0.0059(10) 0.0025(10) C41 0.0125(11) 0.0172(12) 0.0127(11) 0.0012(10) 0.0029(9) 0.0015(9) C42 0.0188(13) 0.0183(13) 0.0162(12) 0.0037(10) 0.0051(10) 0.0020(10) C43 0.0210(13) 0.0233(14) 0.0191(13) 0.0028(11) 0.0048(10) 0.0089(11) C44 0.0142(13) 0.0343(16) 0.0236(14) 0.0056(12) 0.0056(11) 0.0067(11) C45 0.0186(14) 0.0312(15) 0.0289(15) 0.0115(12) 0.0109(11) 0.0014(11) C46 0.0195(13) 0.0193(13) 0.0222(13) 0.0057(11) 0.0082(11) 0.0029(10) C51 0.0227(13) 0.0187(13) 0.0151(12) 0.0050(10) 0.0078(10) 0.0023(10) C52 0.0243(14) 0.0230(14) 0.0167(13) 0.0027(11) 0.0050(11) -0.0019(11) C53 0.0371(17) 0.0198(14) 0.0235(14) 0.0004(11) 0.0135(12) -0.0050(12) C54 0.0427(17) 0.0182(13) 0.0216(14) 0.0057(11) 0.0155(13) 0.0066(12) C55 0.0317(15) 0.0249(15) 0.0189(13) 0.0063(11) 0.0079(12) 0.0081(12) C56 0.0247(14) 0.0241(14) 0.0198(13) 0.0044(11) 0.0062(11) -0.0005(11) C61 0.0167(13) 0.0192(13) 0.0188(13) 0.0021(10) 0.0050(10) -0.0015(10) C62 0.0324(16) 0.0301(16) 0.0222(14) 0.0092(12) 0.0127(12) 0.0067(12) C63 0.0347(17) 0.0320(17) 0.0312(16) 0.0099(13) 0.0107(13) 0.0144(13) C64 0.0253(15) 0.0300(16) 0.0287(15) -0.0030(13) 0.0120(12) 0.0008(12) C65 0.0354(17) 0.0338(16) 0.0198(14) 0.0042(12) 0.0137(12) -0.0003(13) C66 0.0288(15) 0.0257(15) 0.0213(14) 0.0066(12) 0.0074(12) 0.0037(12) C71 0.0183(13) 0.0164(12) 0.0186(13) 0.0051(10) 0.0028(10) -0.0026(10) C72 0.0177(13) 0.0212(14) 0.0222(13) 0.0015(11) 0.0029(11) -0.0002(10) C73 0.0264(15) 0.0295(15) 0.0198(14) -0.0034(12) 0.0041(11) -0.0018(12) C74 0.0282(16) 0.0392(18) 0.0193(14) 0.0008(13) -0.0055(12) -0.0039(13) C75 0.0158(14) 0.0433(18) 0.0313(16) 0.0063(14) -0.0017(12) 0.0008(13) C76 0.0202(14) 0.0297(15) 0.0246(14) 0.0034(12) 0.0070(11) 0.0014(11) C81 0.0209(13) 0.0115(11) 0.0150(12) 0.0039(9) 0.0077(10) -0.0002(10) C82 0.0202(13) 0.0139(12) 0.0180(12) 0.0055(10) 0.0063(10) 0.0013(10) C83 0.0270(14) 0.0161(12) 0.0143(12) 0.0044(10) 0.0048(10) 0.0009(10) C84 0.0287(14) 0.0137(12) 0.0211(13) 0.0015(10) 0.0134(11) 0.0004(10) C85 0.0205(13) 0.0141(12) 0.0263(14) 0.0068(11) 0.0115(11) 0.0028(10) C86 0.0200(13) 0.0146(12) 0.0181(12) 0.0034(10) 0.0054(10) 0.0031(10) C9 0.054(2) 0.041(2) 0.045(2) 0.0021(17) -0.0037(18) -0.0033(17) Cl1 0.0374(5) 0.0639(6) 0.0498(5) 0.0044(5) 0.0157(4) -0.0026(4) Cl2 0.1091(10) 0.0480(6) 0.0779(8) 0.0209(6) -0.0491(8) -0.0122(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 C61 2.155(3) . ? Sn1 C71 2.160(3) . ? Sn1 C51 2.169(3) . ? Sn1 Ru1 2.6139(3) . ? Ru1 C2 1.871(3) . ? Ru1 C1 1.878(3) . ? Ru1 S1 2.3562(6) . ? Ru1 S2 2.4476(6) . ? Ru1 Ru2 2.9030(3) . ? Ru2 C4 1.890(3) . ? Ru2 C3 1.915(3) . ? Ru2 P1 2.3217(6) . ? Ru2 S1 2.4130(6) . ? Ru2 S2 2.4432(6) . ? Ru2 Ru3 2.7481(3) . ? Ru3 C5 1.882(3) . ? Ru3 C6 1.925(3) . ? Ru3 P2 2.3202(6) . ? Ru3 S1 2.3371(6) . ? Ru3 S2 2.4746(6) . ? P1 C11 1.830(2) . ? P1 C21 1.839(2) . ? P1 C7 1.854(2) . ? P2 C31 1.825(3) . ? P2 C41 1.836(2) . ? P2 C7 1.844(2) . ? S1 C81 1.787(2) . ? O1 C1 1.151(3) . ? O2 C2 1.154(3) . ? O3 C3 1.149(3) . ? O4 C4 1.155(3) . ? O5 C5 1.152(3) . ? O6 C6 1.143(3) . ? C11 C12 1.399(4) . ? C11 C16 1.401(4) . ? C12 C13 1.398(4) . ? C13 C14 1.387(4) . ? C14 C15 1.388(4) . ? C15 C16 1.392(4) . ? C21 C22 1.400(3) . ? C21 C26 1.409(3) . ? C22 C23 1.390(4) . ? C23 C24 1.383(4) . ? C24 C25 1.396(4) . ? C25 C26 1.391(4) . ? C31 C32 1.396(4) . ? C31 C36 1.402(3) . ? C32 C33 1.393(4) . ? C33 C34 1.389(4) . ? C34 C35 1.391(4) . ? C35 C36 1.390(4) . ? C41 C42 1.400(3) . ? C41 C46 1.401(4) . ? C42 C43 1.393(4) . ? C43 C44 1.394(4) . ? C44 C45 1.387(4) . ? C45 C46 1.392(4) . ? C51 C56 1.400(4) . ? C51 C52 1.401(4) . ? C52 C53 1.401(4) . ? C53 C54 1.386(4) . ? C54 C55 1.385(4) . ? C55 C56 1.397(4) . ? C61 C66 1.396(4) . ? C61 C62 1.397(4) . ? C62 C63 1.393(4) . ? C63 C64 1.388(4) . ? C64 C65 1.383(4) . ? C65 C66 1.396(4) . ? C71 C72 1.396(4) . ? C71 C76 1.397(4) . ? C72 C73 1.397(4) . ? C73 C74 1.389(4) . ? C74 C75 1.383(4) . ? C75 C76 1.397(4) . ? C81 C86 1.391(3) . ? C81 C82 1.399(3) . ? C82 C83 1.397(3) . ? C83 C84 1.398(4) . ? C84 C85 1.391(4) . ? C85 C86 1.398(3) . ? C9 Cl2 1.756(4) . ? C9 Cl1 1.778(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C61 Sn1 C71 106.13(10) . . ? C61 Sn1 C51 104.97(10) . . ? C71 Sn1 C51 107.29(10) . . ? C61 Sn1 Ru1 115.13(7) . . ? C71 Sn1 Ru1 109.31(7) . . ? C51 Sn1 Ru1 113.49(7) . . ? C2 Ru1 C1 91.96(11) . . ? C2 Ru1 S1 165.74(8) . . ? C1 Ru1 S1 96.89(8) . . ? C2 Ru1 S2 97.45(8) . . ? C1 Ru1 S2 170.43(8) . . ? S1 Ru1 S2 73.54(2) . . ? C2 Ru1 Sn1 85.78(8) . . ? C1 Ru1 Sn1 89.48(8) . . ? S1 Ru1 Sn1 105.386(17) . . ? S2 Ru1 Sn1 92.908(16) . . ? C2 Ru1 Ru2 112.38(8) . . ? C1 Ru1 Ru2 120.92(8) . . ? S1 Ru1 Ru2 53.398(15) . . ? S2 Ru1 Ru2 53.518(15) . . ? Sn1 Ru1 Ru2 142.342(9) . . ? C4 Ru2 C3 91.03(11) . . ? C4 Ru2 P1 95.22(8) . . ? C3 Ru2 P1 95.97(8) . . ? C4 Ru2 S1 97.17(8) . . ? C3 Ru2 S1 120.58(8) . . ? P1 Ru2 S1 140.96(2) . . ? C4 Ru2 S2 169.19(8) . . ? C3 Ru2 S2 97.27(8) . . ? P1 Ru2 S2 90.81(2) . . ? S1 Ru2 S2 72.64(2) . . ? C4 Ru2 Ru3 114.59(8) . . ? C3 Ru2 Ru3 153.69(8) . . ? P1 Ru2 Ru3 87.865(16) . . ? S1 Ru2 Ru3 53.372(15) . . ? S2 Ru2 Ru3 56.572(15) . . ? C4 Ru2 Ru1 122.85(8) . . ? C3 Ru2 Ru1 74.86(8) . . ? P1 Ru2 Ru1 140.443(17) . . ? S1 Ru2 Ru1 51.619(15) . . ? S2 Ru2 Ru1 53.659(15) . . ? Ru3 Ru2 Ru1 85.630(8) . . ? C5 Ru3 C6 99.22(10) . . ? C5 Ru3 P2 91.67(7) . . ? C6 Ru3 P2 96.18(8) . . ? C5 Ru3 S1 95.47(7) . . ? C6 Ru3 S1 106.36(8) . . ? P2 Ru3 S1 154.87(2) . . ? C5 Ru3 S2 153.79(7) . . ? C6 Ru3 S2 106.63(8) . . ? P2 Ru3 S2 89.84(2) . . ? S1 Ru3 S2 73.36(2) . . ? C5 Ru3 Ru2 98.50(7) . . ? C6 Ru3 Ru2 156.12(8) . . ? P2 Ru3 Ru2 99.184(17) . . ? S1 Ru3 Ru2 55.953(16) . . ? S2 Ru3 Ru2 55.484(14) . . ? C11 P1 C21 102.85(11) . . ? C11 P1 C7 104.23(11) . . ? C21 P1 C7 102.59(11) . . ? C11 P1 Ru2 112.21(8) . . ? C21 P1 Ru2 118.93(8) . . ? C7 P1 Ru2 114.34(8) . . ? C31 P2 C41 100.14(11) . . ? C31 P2 C7 108.51(12) . . ? C41 P2 C7 106.07(11) . . ? C31 P2 Ru3 116.75(8) . . ? C41 P2 Ru3 116.21(8) . . ? C7 P2 Ru3 108.40(8) . . ? Ru2 S2 Ru1 72.823(17) . . ? Ru2 S2 Ru3 67.944(16) . . ? Ru1 S2 Ru3 102.63(2) . . ? C81 S1 Ru3 121.04(8) . . ? C81 S1 Ru1 129.05(8) . . ? Ru3 S1 Ru1 109.91(2) . . ? C81 S1 Ru2 121.07(8) . . ? Ru3 S1 Ru2 70.675(17) . . ? Ru1 S1 Ru2 74.983(18) . . ? O1 C1 Ru1 175.5(2) . . ? O2 C2 Ru1 178.1(2) . . ? O3 C3 Ru2 172.8(2) . . ? O4 C4 Ru2 177.5(2) . . ? O5 C5 Ru3 176.3(2) . . ? O6 C6 Ru3 177.2(2) . . ? P2 C7 P1 111.31(12) . . ? C12 C11 C16 118.4(2) . . ? C12 C11 P1 122.0(2) . . ? C16 C11 P1 119.24(19) . . ? C13 C12 C11 120.5(3) . . ? C14 C13 C12 120.4(3) . . ? C13 C14 C15 119.6(3) . . ? C14 C15 C16 120.2(3) . . ? C15 C16 C11 120.8(3) . . ? C22 C21 C26 119.1(2) . . ? C22 C21 P1 121.15(19) . . ? C26 C21 P1 119.65(18) . . ? C23 C22 C21 120.2(2) . . ? C24 C23 C22 120.7(2) . . ? C23 C24 C25 119.6(2) . . ? C26 C25 C24 120.4(2) . . ? C25 C26 C21 120.0(2) . . ? C32 C31 C36 118.8(2) . . ? C32 C31 P2 123.76(19) . . ? C36 C31 P2 117.22(19) . . ? C33 C32 C31 120.2(2) . . ? C34 C33 C32 120.5(3) . . ? C33 C34 C35 119.9(2) . . ? C36 C35 C34 119.7(2) . . ? C35 C36 C31 120.9(2) . . ? C42 C41 C46 118.9(2) . . ? C42 C41 P2 121.29(19) . . ? C46 C41 P2 119.53(19) . . ? C43 C42 C41 120.7(2) . . ? C42 C43 C44 119.7(2) . . ? C45 C44 C43 120.1(2) . . ? C44 C45 C46 120.3(3) . . ? C45 C46 C41 120.3(2) . . ? C56 C51 C52 118.2(2) . . ? C56 C51 Sn1 123.02(19) . . ? C52 C51 Sn1 118.77(19) . . ? C53 C52 C51 120.7(3) . . ? C54 C53 C52 120.1(3) . . ? C55 C54 C53 120.0(3) . . ? C54 C55 C56 120.1(3) . . ? C55 C56 C51 120.9(3) . . ? C66 C61 C62 117.7(2) . . ? C66 C61 Sn1 120.61(19) . . ? C62 C61 Sn1 121.70(19) . . ? C63 C62 C61 121.3(3) . . ? C64 C63 C62 120.1(3) . . ? C65 C64 C63 119.5(3) . . ? C64 C65 C66 120.2(3) . . ? C65 C66 C61 121.2(3) . . ? C72 C71 C76 118.1(2) . . ? C72 C71 Sn1 120.35(19) . . ? C76 C71 Sn1 121.48(19) . . ? C71 C72 C73 121.2(2) . . ? C74 C73 C72 119.5(3) . . ? C75 C74 C73 120.3(3) . . ? C74 C75 C76 119.8(3) . . ? C71 C76 C75 121.0(3) . . ? C86 C81 C82 121.1(2) . . ? C86 C81 S1 121.06(19) . . ? C82 C81 S1 117.82(19) . . ? C83 C82 C81 119.3(2) . . ? C82 C83 C84 119.9(2) . . ? C85 C84 C83 120.1(2) . . ? C84 C85 C86 120.5(2) . . ? C81 C86 C85 119.0(2) . . ? Cl2 C9 Cl1 112.2(2) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.31 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.678 _refine_diff_density_min -1.063 _refine_diff_density_rms 0.080