# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 _publ_contact_author_name 'Professor E. Canadell' _publ_contact_author_address ; Institut de Ciencia de Materials de Barcelona (CSIC), Campus de la U.A.B., E-08193, Bellaterra, Spain ; _publ_contact_author_email canadell@icmab.es loop_ _publ_author_name _publ_author_address S.V.Simonov ; a - Institute of Solid State Physics, RAS, Chernogolovka, 142432, Russia e-mail: simonovsv@rambler.ru ; I.Yu.Shevyakova ; b - Institute of Problems of Chemical Physics, RAS, Chernogolovka, 142432, Russia ; L.V.Zorina ; a - Institute of Solid State Physics, RAS, Chernogolovka, 142432, Russia e-mail: zorina@issp.ac.ru ; S.S.Khasanov ; a - Institute of Solid State Physics, RAS, Chernogolovka, 142432, Russia e-mail: khasanov@issp.ac.ru ; ; L.I.Buravov ; ; Institute of Problems of Chemical Physics, RAS, Chernogolovka, 142432, Russia ; V.A.Emel'yanov ; a - Institute of Inorganic Chemistry, RAS, Prosp. Akad. Lavrent'eva, 3, Novosibirsk-90, Russia ; E.Canadell ; Institut de Ciencia de Materials de Barcelona (CSIC), Campus de la U.A.B., E-08193, Bellaterra, Spain e-mail: canadell@icmab.es ; R.P.Shibaeva ; a - Institute of Solid State Physics, RAS, Chernogolovka, 142432, Russia e-mail: shibaeva@issp.ac.ru ; E.B.Yagubskii ; Institute of Problems of Chemical Physics, RAS, Chernogolovka, 142432, Russia e-mail: yagubski@icp.ac.ru ; _publ_section_title ; Variety of molecular conducting layers in the family of radical cation salts based on BEDT-TTF with the metal mononitrosyl complex anion [OsNOCl5](2-). ; data_kappa-(BEDT-TTF)4[OsNOCl5]C7H5N _database_code_depnum_ccdc_archive 'CCDC 258887' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C10 H8 S8)4, (Os NO Cl5), (C7 H5 N)' _chemical_formula_sum 'C47 H37 Cl5 N2 O1 Os1 S32' _chemical_formula_weight 2039.16 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' Cl Cl 0.1484 0.1585 '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' Os Os -1.2165 7.6030 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7410(4) _cell_length_b 11.9042(6) _cell_length_c 17.1842(6) _cell_angle_alpha 95.305(4) _cell_angle_beta 92.646(3) _cell_angle_gamma 95.136(4) _cell_volume 1770.61(14) _cell_formula_units_Z 1 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 18 _cell_measurement_theta_max 20 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.912 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1014 _exptl_absorpt_coefficient_mu 2.974 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.5607 _exptl_absorpt_correction_T_max 0.8903 _exptl_absorpt_process_details ; aplication of absorption correction procedure based on crystal sample shape using WinGX facilities ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type Mok\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'Enraf Nonius FR590' _diffrn_radiation_monochromator graphite _diffrn_detector 'scintillation LiI' _diffrn_detector_dtime 1.195 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Enraf Nonius CAD4' _diffrn_measurement_method 'non-profiled omega scans' _diffrn_standards_number 3 _diffrn_standards_interval_time 9000 _diffrn_standards_decay_% 0 _diffrn_reflns_number 8607 _diffrn_reflns_av_R_equivalents 0.0177 _diffrn_reflns_av_sigmaI/netI 0.0435 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 27.46 _reflns_number_total 8066 _reflns_number_gt 6914 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0295P)^2^+1.7311P] 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 8066 _refine_ls_number_parameters 434 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0474 _refine_ls_R_factor_gt 0.0363 _refine_ls_wR_factor_ref 0.0843 _refine_ls_wR_factor_gt 0.0793 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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 S1 S -0.17971(13) 0.24860(9) 0.33744(6) 0.0500(3) Uani 1 1 d . . . S2 S -0.41707(13) 0.06195(9) 0.34876(6) 0.0472(2) Uani 1 1 d . . . S3 S -0.03060(13) 0.20514(9) 0.50775(6) 0.0453(2) Uani 1 1 d . . . S4 S -0.27221(12) 0.01990(9) 0.51743(6) 0.0446(2) Uani 1 1 d . . . S5 S -0.29834(18) 0.30726(11) 0.18501(8) 0.0682(4) Uani 1 1 d . . . S6 S -0.57734(14) 0.08487(10) 0.19628(6) 0.0534(3) Uani 1 1 d . . . S7 S 0.13051(14) 0.17011(10) 0.65840(7) 0.0552(3) Uani 1 1 d . . . S8 S -0.14901(13) -0.05230(9) 0.66419(6) 0.0482(2) Uani 1 1 d . . . C1 C -0.2557(4) 0.1438(3) 0.3925(2) 0.0381(8) Uani 1 1 d . . . C2 C -0.1924(4) 0.1246(3) 0.4634(2) 0.0365(8) Uani 1 1 d . . . C3 C -0.3196(5) 0.2207(3) 0.2604(2) 0.0434(9) Uani 1 1 d . A . C4 C -0.4282(5) 0.1349(3) 0.2653(2) 0.0389(8) Uani 1 1 d . A . C5 C -0.0193(5) 0.1282(3) 0.5887(2) 0.0392(8) Uani 1 1 d . . . C6 C -0.1286(4) 0.0415(3) 0.5929(2) 0.0363(8) Uani 1 1 d . . . C7 C -0.4463(14) 0.2489(8) 0.1117(5) 0.064(3) Uani 0.657(18) 1 d PD A 1 H7A H -0.5381 0.2871 0.1209 0.077 Uiso 0.657(18) 1 calc PR A 1 H7B H -0.4123 0.2661 0.0608 0.077 Uiso 0.657(18) 1 calc PR A 1 C8 C -0.4893(16) 0.1218(7) 0.1086(6) 0.056(3) Uani 0.657(18) 1 d PD A 1 H8A H -0.3976 0.0823 0.1021 0.067 Uiso 0.657(18) 1 calc PR A 1 H8B H -0.5600 0.0977 0.0638 0.067 Uiso 0.657(18) 1 calc PR A 1 C7A C -0.3704(18) 0.2046(18) 0.1082(8) 0.056(5) Uani 0.343(18) 1 d PD A 2 H7A1 H -0.3599 0.2371 0.0588 0.067 Uiso 0.343(18) 1 calc PR A 2 H7A2 H -0.3086 0.1409 0.1077 0.067 Uiso 0.343(18) 1 calc PR A 2 C8A C -0.5364(18) 0.162(2) 0.1150(12) 0.056(5) Uani 0.343(18) 1 d PD A 2 H8A1 H -0.5709 0.1145 0.0675 0.068 Uiso 0.343(18) 1 calc PR A 2 H8A2 H -0.5967 0.2270 0.1176 0.068 Uiso 0.343(18) 1 calc PR A 2 C9 C 0.0302(6) 0.1359(4) 0.7435(3) 0.0603(12) Uani 1 1 d . . . H9A H 0.0965 0.1607 0.7899 0.072 Uiso 1 1 calc R . . H9B H -0.0602 0.1776 0.7465 0.072 Uiso 1 1 calc R . . C10 C -0.0186(6) 0.0125(4) 0.7436(2) 0.0594(12) Uani 1 1 d . . . H10A H -0.0667 0.0012 0.7923 0.071 Uiso 1 1 calc R . . H10B H 0.0731 -0.0277 0.7433 0.071 Uiso 1 1 calc R . . S11 S 0.22108(13) 0.51749(10) 0.49013(6) 0.0477(2) Uani 1 1 d . . . S12 S 0.37606(15) 0.32939(10) 0.41690(7) 0.0521(3) Uani 1 1 d . . . S13 S 0.35310(13) 0.46453(9) 0.65993(6) 0.0451(2) Uani 1 1 d . . . S14 S 0.50785(13) 0.27635(9) 0.58665(7) 0.0489(2) Uani 1 1 d . . . S15 S 0.07257(17) 0.57632(15) 0.34526(8) 0.0725(4) Uani 1 1 d . . . S16 S 0.2457(2) 0.34456(15) 0.25868(8) 0.0867(5) Uani 1 1 d . . . S17 S 0.4223(2) 0.41657(12) 0.82113(7) 0.0783(5) Uani 1 1 d . . . S18 S 0.61349(15) 0.19757(11) 0.73656(8) 0.0613(3) Uani 1 1 d . . . C11 C 0.3385(5) 0.4091(3) 0.5020(2) 0.0405(8) Uani 1 1 d . . . C12 C 0.3928(4) 0.3865(3) 0.5739(2) 0.0394(8) Uani 1 1 d . . . C13 C 0.1884(5) 0.4851(4) 0.3893(2) 0.0454(9) Uani 1 1 d . B . C14 C 0.2575(5) 0.3979(4) 0.3562(2) 0.0497(10) Uani 1 1 d . B . C15 C 0.4436(5) 0.3804(3) 0.7221(2) 0.0431(9) Uani 1 1 d . C . C16 C 0.5164(5) 0.2957(3) 0.6884(2) 0.0438(9) Uani 1 1 d . C . C17 C 0.033(2) 0.5122(13) 0.2511(7) 0.068(4) Uani 0.59(3) 1 d P B 1 H17A H -0.0492 0.4524 0.2519 0.081 Uiso 0.59(3) 1 calc PR B 1 H17B H -0.0027 0.5677 0.2185 0.081 Uiso 0.59(3) 1 calc PR B 1 C18 C 0.170(2) 0.4620(15) 0.2139(6) 0.068(4) Uani 0.59(3) 1 d P B 1 H18A H 0.2523 0.5221 0.2141 0.081 Uiso 0.59(3) 1 calc PR B 1 H18B H 0.1396 0.4366 0.1596 0.081 Uiso 0.59(3) 1 calc PR B 1 C17A C 0.114(3) 0.5354(17) 0.2422(9) 0.060(5) Uani 0.41(3) 1 d P B 2 H17C H 0.0386 0.5666 0.2089 0.073 Uiso 0.41(3) 1 calc PR B 2 H17D H 0.2138 0.5720 0.2328 0.073 Uiso 0.41(3) 1 calc PR B 2 C18A C 0.113(3) 0.413(2) 0.2159(10) 0.067(5) Uani 0.41(3) 1 d P B 2 H18C H 0.1251 0.4048 0.1600 0.081 Uiso 0.41(3) 1 calc PR B 2 H18D H 0.0125 0.3756 0.2248 0.081 Uiso 0.41(3) 1 calc PR B 2 C19 C 0.4972(13) 0.2997(7) 0.8681(5) 0.060(2) Uiso 0.650(15) 1 d PD C 1 H19A H 0.6028 0.3230 0.8864 0.072 Uiso 0.650(15) 1 calc PR C 1 H19B H 0.4390 0.2879 0.9138 0.072 Uiso 0.650(15) 1 calc PR C 1 C20 C 0.4942(9) 0.1886(6) 0.8198(4) 0.049(2) Uiso 0.650(15) 1 d PD C 1 H20A H 0.3891 0.1634 0.8013 0.059 Uiso 0.650(15) 1 calc PR C 1 H20B H 0.5302 0.1327 0.8522 0.059 Uiso 0.650(15) 1 calc PR C 1 C19A C 0.434(2) 0.2853(14) 0.8593(10) 0.064(5) Uiso 0.350(15) 1 d PD C 2 H19C H 0.4344 0.2948 0.9160 0.077 Uiso 0.350(15) 1 calc PR C 2 H19D H 0.3467 0.2327 0.8397 0.077 Uiso 0.350(15) 1 calc PR C 2 C20A C 0.582(2) 0.241(2) 0.8335(13) 0.103(8) Uiso 0.350(15) 1 d PD C 2 H20C H 0.5977 0.1766 0.8630 0.123 Uiso 0.350(15) 1 calc PR C 2 H20D H 0.6642 0.2990 0.8512 0.123 Uiso 0.350(15) 1 calc PR C 2 Os1 Os 0.0000 0.0000 0.0000 0.03691(7) Uani 1 2 d S . . Cl1 Cl 0.18291(14) -0.09947(10) 0.06595(7) 0.0564(3) Uani 1 1 d . D . Cl2 Cl -0.20152(14) -0.08693(12) 0.06905(7) 0.0607(3) Uani 1 1 d . D . Cl3 Cl 0.0414(5) 0.1506(3) 0.0948(2) 0.0533(9) Uani 0.50 1 d P D 1 N1 N 0.0314(19) 0.1118(11) 0.0738(8) 0.051(3) Uani 0.50 1 d P D 2 O1 O 0.0565(17) 0.1884(10) 0.1196(7) 0.079(3) Uani 0.50 1 d P D 2 C7S C 0.2863(16) 0.4963(11) 0.0003(8) 0.077(3) Uiso 0.50 1 d P . . N1S N 0.4144(16) 0.4958(12) 0.0000(9) 0.115(4) Uiso 0.50 1 d P . . C1S C 0.0280(8) 0.4026(5) -0.0135(4) 0.057(2) Uiso 0.50 1 d PG . . H1S H 0.0693 0.3337 -0.0236 0.085 Uiso 0.50 1 calc PR . . C2S C 0.1246(5) 0.5026(6) -0.0008(4) 0.054(2) Uiso 0.50 1 d PG . . C3S C 0.0629(7) 0.6055(5) 0.0143(4) 0.055(2) Uiso 0.50 1 d PG . . H3S H 0.1275 0.6724 0.0228 0.082 Uiso 0.50 1 calc PR . . C4S C -0.0954(8) 0.6085(6) 0.0166(5) 0.071(3) Uiso 0.50 1 d PG . . H4S H -0.1367 0.6773 0.0267 0.107 Uiso 0.50 1 calc PR . . C5S C -0.1921(5) 0.5085(8) 0.0039(5) 0.078(3) Uiso 0.50 1 d PG . . H5S H -0.2980 0.5105 0.0055 0.117 Uiso 0.50 1 calc PR . . C6S C -0.1303(7) 0.4056(6) -0.0111(5) 0.071(3) Uiso 0.50 1 d PG . . H6S H -0.1950 0.3387 -0.0196 0.106 Uiso 0.50 1 calc PR . . 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 S1 0.0509(6) 0.0506(6) 0.0465(5) 0.0172(5) -0.0125(5) -0.0119(5) S2 0.0475(6) 0.0555(6) 0.0366(5) 0.0160(4) -0.0103(4) -0.0120(5) S3 0.0498(6) 0.0466(5) 0.0367(5) 0.0087(4) -0.0094(4) -0.0094(4) S4 0.0396(5) 0.0588(6) 0.0336(5) 0.0128(4) -0.0061(4) -0.0107(4) S5 0.0841(9) 0.0615(7) 0.0569(7) 0.0320(6) -0.0207(6) -0.0195(7) S6 0.0510(6) 0.0661(7) 0.0407(5) 0.0165(5) -0.0143(5) -0.0115(5) S7 0.0476(6) 0.0631(7) 0.0515(6) 0.0156(5) -0.0203(5) -0.0125(5) S8 0.0557(6) 0.0522(6) 0.0366(5) 0.0142(4) -0.0051(4) -0.0027(5) C1 0.039(2) 0.0389(19) 0.0353(18) 0.0050(15) -0.0048(15) -0.0007(15) C2 0.0362(19) 0.0409(19) 0.0317(17) 0.0055(14) -0.0008(14) -0.0013(15) C3 0.049(2) 0.043(2) 0.0383(19) 0.0101(16) -0.0097(17) 0.0016(17) C4 0.042(2) 0.0412(19) 0.0328(17) 0.0078(15) -0.0056(15) 0.0005(16) C5 0.043(2) 0.0403(19) 0.0328(18) 0.0035(15) -0.0090(15) 0.0012(16) C6 0.0366(19) 0.0416(19) 0.0301(16) 0.0039(14) -0.0048(14) 0.0042(15) C7 0.062(6) 0.082(6) 0.049(4) 0.031(4) -0.014(4) -0.010(5) C8 0.066(7) 0.061(6) 0.040(4) 0.003(4) 0.005(4) 0.006(4) C7A 0.052(9) 0.086(12) 0.031(6) 0.006(6) 0.006(6) 0.013(8) C8A 0.061(12) 0.064(13) 0.040(9) 0.008(9) -0.024(8) -0.002(8) C9 0.059(3) 0.076(3) 0.043(2) -0.004(2) -0.010(2) 0.006(2) C10 0.065(3) 0.078(3) 0.034(2) 0.016(2) -0.009(2) -0.004(2) S11 0.0496(6) 0.0596(6) 0.0350(5) 0.0003(4) 0.0004(4) 0.0168(5) S12 0.0624(7) 0.0466(6) 0.0462(6) -0.0055(4) 0.0016(5) 0.0102(5) S13 0.0474(6) 0.0502(6) 0.0399(5) 0.0059(4) 0.0009(4) 0.0156(4) S14 0.0515(6) 0.0451(5) 0.0510(6) 0.0015(4) 0.0022(5) 0.0126(5) S15 0.0642(8) 0.1114(12) 0.0466(6) 0.0097(7) -0.0061(6) 0.0367(8) S16 0.1221(14) 0.0956(11) 0.0403(6) -0.0182(7) -0.0049(8) 0.0294(10) S17 0.1329(14) 0.0681(8) 0.0426(6) 0.0136(6) 0.0097(7) 0.0464(9) S18 0.0569(7) 0.0565(7) 0.0751(8) 0.0181(6) -0.0016(6) 0.0211(6) C11 0.037(2) 0.043(2) 0.040(2) 0.0016(16) 0.0022(16) 0.0028(16) C12 0.037(2) 0.0403(19) 0.0403(19) 0.0021(15) 0.0017(16) 0.0050(15) C13 0.044(2) 0.060(2) 0.0314(18) 0.0016(17) -0.0006(16) 0.0030(19) C14 0.053(3) 0.058(3) 0.035(2) -0.0058(18) -0.0017(18) 0.003(2) C15 0.044(2) 0.045(2) 0.042(2) 0.0093(17) 0.0007(17) 0.0085(17) C16 0.042(2) 0.041(2) 0.048(2) 0.0060(17) -0.0035(17) 0.0039(16) C17 0.066(9) 0.088(8) 0.043(5) -0.001(5) -0.022(6) -0.004(6) C18 0.084(9) 0.082(9) 0.033(4) 0.013(5) 0.008(5) -0.017(7) C17A 0.063(12) 0.070(10) 0.045(7) 0.001(6) -0.008(8) -0.001(9) C18A 0.070(11) 0.077(13) 0.048(7) 0.003(7) -0.016(7) -0.021(9) Os1 0.03800(12) 0.03861(11) 0.03208(11) 0.00000(8) -0.00418(8) -0.00095(8) Cl1 0.0581(7) 0.0575(6) 0.0522(6) 0.0023(5) -0.0168(5) 0.0109(5) Cl2 0.0504(6) 0.0819(8) 0.0486(6) 0.0144(6) 0.0042(5) -0.0090(6) Cl3 0.080(2) 0.041(3) 0.035(3) -0.0078(16) -0.011(2) 0.003(2) N1 0.061(6) 0.047(8) 0.039(7) -0.010(5) -0.009(5) 0.004(6) O1 0.109(8) 0.062(7) 0.060(8) -0.018(5) -0.020(6) 0.013(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 S1 C1 1.738(4) . ? S1 C3 1.748(4) . ? S2 C1 1.739(4) . ? S2 C4 1.748(4) . ? S3 C2 1.738(4) . ? S3 C5 1.739(4) . ? S4 C2 1.738(4) . ? S4 C6 1.747(4) . ? S5 C3 1.734(4) . ? S5 C7A 1.766(15) . ? S5 C7 1.808(8) . ? S6 C4 1.746(4) . ? S6 C8A 1.78(2) . ? S6 C8 1.795(11) . ? S7 C5 1.740(4) . ? S7 C9 1.800(5) . ? S8 C6 1.737(4) . ? S8 C10 1.805(5) . ? C1 C2 1.362(5) . ? C3 C4 1.342(5) . ? C5 C6 1.352(5) . ? C7 C8 1.521(11) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C7A C8A 1.506(15) . ? C7A H7A1 0.9700 . ? C7A H7A2 0.9700 . ? C8A H8A1 0.9700 . ? C8A H8A2 0.9700 . ? C9 C10 1.492(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? S11 C11 1.740(4) . ? S11 C13 1.745(4) . ? S12 C11 1.728(4) . ? S12 C14 1.742(5) . ? S13 C12 1.738(4) . ? S13 C15 1.741(4) . ? S14 C16 1.740(4) . ? S14 C12 1.746(4) . ? S15 C17 1.730(10) . ? S15 C13 1.748(4) . ? S15 C17A 1.853(17) . ? S16 C18A 1.658(17) . ? S16 C14 1.732(4) . ? S16 C18 1.818(13) . ? S17 C15 1.739(4) . ? S17 C19A 1.760(16) . ? S17 C19 1.827(9) . ? S18 C20A 1.74(2) . ? S18 C16 1.749(4) . ? S18 C20 1.814(7) . ? C11 C12 1.362(5) . ? C13 C14 1.341(6) . ? C15 C16 1.341(6) . ? C17 C18 1.52(3) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C17A C18A 1.49(3) . ? C17A H17C 0.9700 . ? C17A H17D 0.9700 . ? C18A H18C 0.9700 . ? C18A H18D 0.9700 . ? C19 C20 1.492(9) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C19A C20A 1.513(17) . ? C19A H19C 0.9700 . ? C19A H19D 0.9700 . ? C20A H20C 0.9700 . ? C20A H20D 0.9700 . ? Os1 N1 1.745(10) . ? Os1 N1 1.745(10) 2 ? Os1 Cl3 2.299(3) . ? Os1 Cl3 2.299(3) 2 ? Os1 Cl1 2.3796(11) . ? Os1 Cl1 2.3796(11) 2 ? Os1 Cl2 2.3823(11) . ? Os1 Cl2 2.3823(11) 2 ? N1 O1 1.147(11) . ? C7S N1S 1.120(16) . ? C7S C2S 1.422(15) . ? C1S C2S 1.3900 . ? C1S C6S 1.3900 . ? C1S H1S 0.9300 . ? C2S C3S 1.3900 . ? C3S C4S 1.3900 . ? C3S H3S 0.9300 . ? C4S C5S 1.3900 . ? C4S H4S 0.9300 . ? C5S C6S 1.3900 . ? C5S H5S 0.9300 . ? C6S H6S 0.9300 . ? 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 S1 C3 95.54(19) . . ? C1 S2 C4 95.73(18) . . ? C2 S3 C5 95.24(18) . . ? C2 S4 C6 95.26(18) . . ? C3 S5 C7A 96.8(6) . . ? C3 S5 C7 104.3(3) . . ? C7A S5 C7 28.6(5) . . ? C4 S6 C8A 103.6(6) . . ? C4 S6 C8 99.7(4) . . ? C8A S6 C8 21.5(6) . . ? C5 S7 C9 97.8(2) . . ? C6 S8 C10 103.5(2) . . ? C2 C1 S1 123.1(3) . . ? C2 C1 S2 122.2(3) . . ? S1 C1 S2 114.7(2) . . ? C1 C2 S4 121.9(3) . . ? C1 C2 S3 122.8(3) . . ? S4 C2 S3 115.2(2) . . ? C4 C3 S5 127.7(3) . . ? C4 C3 S1 117.2(3) . . ? S5 C3 S1 115.2(2) . . ? C3 C4 S6 127.3(3) . . ? C3 C4 S2 116.8(3) . . ? S6 C4 S2 115.8(2) . . ? C6 C5 S3 117.4(3) . . ? C6 C5 S7 125.2(3) . . ? S3 C5 S7 117.3(2) . . ? C5 C6 S8 129.0(3) . . ? C5 C6 S4 116.6(3) . . ? S8 C6 S4 114.4(2) . . ? C8 C7 S5 115.9(8) . . ? C8 C7 H7A 108.3 . . ? S5 C7 H7A 108.3 . . ? C8 C7 H7B 108.3 . . ? S5 C7 H7B 108.3 . . ? H7A C7 H7B 107.4 . . ? C7 C8 S6 111.2(8) . . ? C7 C8 H8A 109.4 . . ? S6 C8 H8A 109.4 . . ? C7 C8 H8B 109.4 . . ? S6 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? C8A C7A S5 113.4(14) . . ? C8A C7A H7A1 108.9 . . ? S5 C7A H7A1 108.9 . . ? C8A C7A H7A2 108.9 . . ? S5 C7A H7A2 108.9 . . ? H7A1 C7A H7A2 107.7 . . ? C7A C8A S6 116.2(13) . . ? C7A C8A H8A1 108.2 . . ? S6 C8A H8A1 108.2 . . ? C7A C8A H8A2 108.2 . . ? S6 C8A H8A2 108.2 . . ? H8A1 C8A H8A2 107.4 . . ? C10 C9 S7 113.4(3) . . ? C10 C9 H9A 108.9 . . ? S7 C9 H9A 108.9 . . ? C10 C9 H9B 108.9 . . ? S7 C9 H9B 108.9 . . ? H9A C9 H9B 107.7 . . ? C9 C10 S8 117.1(3) . . ? C9 C10 H10A 108.0 . . ? S8 C10 H10A 108.0 . . ? C9 C10 H10B 108.0 . . ? S8 C10 H10B 108.0 . . ? H10A C10 H10B 107.3 . . ? C11 S11 C13 94.9(2) . . ? C11 S12 C14 95.0(2) . . ? C12 S13 C15 95.43(19) . . ? C16 S14 C12 95.13(19) . . ? C17 S15 C13 103.9(5) . . ? C17 S15 C17A 24.1(5) . . ? C13 S15 C17A 97.9(6) . . ? C18A S16 C14 105.5(6) . . ? C18A S16 C18 24.0(6) . . ? C14 S16 C18 100.3(4) . . ? C15 S17 C19A 101.6(6) . . ? C15 S17 C19 103.6(3) . . ? C19A S17 C19 18.2(6) . . ? C20A S18 C16 100.7(7) . . ? C20A S18 C20 30.9(8) . . ? C16 S18 C20 98.5(3) . . ? C12 C11 S12 122.4(3) . . ? C12 C11 S11 121.9(3) . . ? S12 C11 S11 115.6(2) . . ? C11 C12 S13 122.9(3) . . ? C11 C12 S14 122.4(3) . . ? S13 C12 S14 114.8(2) . . ? C14 C13 S11 116.9(3) . . ? C14 C13 S15 129.2(3) . . ? S11 C13 S15 113.8(2) . . ? C13 C14 S16 127.8(4) . . ? C13 C14 S12 117.4(3) . . ? S16 C14 S12 114.8(3) . . ? C16 C15 S17 128.5(3) . . ? C16 C15 S13 117.0(3) . . ? S17 C15 S13 114.5(2) . . ? C15 C16 S14 117.5(3) . . ? C15 C16 S18 126.5(3) . . ? S14 C16 S18 116.0(2) . . ? C18 C17 S15 114.5(14) . . ? C18 C17 H17A 108.6 . . ? S15 C17 H17A 108.6 . . ? C18 C17 H17B 108.6 . . ? S15 C17 H17B 108.6 . . ? H17A C17 H17B 107.6 . . ? C17 C18 S16 117.1(11) . . ? C17 C18 H18A 108.0 . . ? S16 C18 H18A 108.0 . . ? C17 C18 H18B 108.0 . . ? S16 C18 H18B 108.0 . . ? H18A C18 H18B 107.3 . . ? C18A C17A S15 118.1(18) . . ? C18A C17A H17C 107.8 . . ? S15 C17A H17C 107.8 . . ? C18A C17A H17D 107.8 . . ? S15 C17A H17D 107.8 . . ? H17C C17A H17D 107.1 . . ? C17A C18A S16 116.1(16) . . ? C17A C18A H18C 108.3 . . ? S16 C18A H18C 108.3 . . ? C17A C18A H18D 108.3 . . ? S16 C18A H18D 108.3 . . ? H18C C18A H18D 107.4 . . ? C20 C19 S17 117.2(6) . . ? C20 C19 H19A 108.0 . . ? S17 C19 H19A 108.0 . . ? C20 C19 H19B 108.0 . . ? S17 C19 H19B 108.0 . . ? H19A C19 H19B 107.2 . . ? C19 C20 S18 112.0(6) . . ? C19 C20 H20A 109.2 . . ? S18 C20 H20A 109.2 . . ? C19 C20 H20B 109.2 . . ? S18 C20 H20B 109.2 . . ? H20A C20 H20B 107.9 . . ? C20A C19A S17 107.3(14) . . ? C20A C19A H19C 110.3 . . ? S17 C19A H19C 110.3 . . ? C20A C19A H19D 110.3 . . ? S17 C19A H19D 110.3 . . ? H19C C19A H19D 108.5 . . ? C19A C20A S18 123.2(17) . . ? C19A C20A H20C 106.5 . . ? S18 C20A H20C 106.5 . . ? C19A C20A H20D 106.5 . . ? S18 C20A H20D 106.5 . . ? H20C C20A H20D 106.5 . . ? N1 Os1 N1 180.0(13) . 2 ? N1 Os1 Cl3 1.5(6) . . ? N1 Os1 Cl3 178.5(6) 2 . ? N1 Os1 Cl3 178.5(6) . 2 ? N1 Os1 Cl3 1.5(6) 2 2 ? Cl3 Os1 Cl3 180.0(3) . 2 ? N1 Os1 Cl1 89.6(5) . . ? N1 Os1 Cl1 90.4(5) 2 . ? Cl3 Os1 Cl1 90.69(10) . . ? Cl3 Os1 Cl1 89.31(10) 2 . ? N1 Os1 Cl1 90.4(5) . 2 ? N1 Os1 Cl1 89.6(5) 2 2 ? Cl3 Os1 Cl1 89.31(10) . 2 ? Cl3 Os1 Cl1 90.69(10) 2 2 ? Cl1 Os1 Cl1 180.00(7) . 2 ? N1 Os1 Cl2 90.8(5) . . ? N1 Os1 Cl2 89.2(5) 2 . ? Cl3 Os1 Cl2 91.80(10) . . ? Cl3 Os1 Cl2 88.20(10) 2 . ? Cl1 Os1 Cl2 90.42(4) . . ? Cl1 Os1 Cl2 89.58(4) 2 . ? N1 Os1 Cl2 89.2(5) . 2 ? N1 Os1 Cl2 90.8(5) 2 2 ? Cl3 Os1 Cl2 88.20(10) . 2 ? Cl3 Os1 Cl2 91.80(10) 2 2 ? Cl1 Os1 Cl2 89.58(4) . 2 ? Cl1 Os1 Cl2 90.42(4) 2 2 ? Cl2 Os1 Cl2 180.00(8) . 2 ? O1 N1 Os1 176.4(19) . . ? N1S C7S C2S 177.0(15) . . ? C2S C1S C6S 120.0 . . ? C2S C1S H1S 120.0 . . ? C6S C1S H1S 120.0 . . ? C3S C2S C1S 120.0 . . ? C3S C2S C7S 121.3(7) . . ? C1S C2S C7S 118.7(7) . . ? C2S C3S C4S 120.0 . . ? C2S C3S H3S 120.0 . . ? C4S C3S H3S 120.0 . . ? C5S C4S C3S 120.0 . . ? C5S C4S H4S 120.0 . . ? C3S C4S H4S 120.0 . . ? C4S C5S C6S 120.0 . . ? C4S C5S H5S 120.0 . . ? C6S C5S H5S 120.0 . . ? C5S C6S C1S 120.0 . . ? C5S C6S H6S 120.0 . . ? C1S C6S H6S 120.0 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C9 H9B S18 0.97 2.88 3.778(5) 154.0 1_455 C17 H17A S5 0.97 2.79 3.684(19) 153.8 . C17A H17D S18 0.97 3.00 3.78(3) 138.2 2_666 C18 H18A S17 0.97 2.98 3.823(19) 146.4 2_666 C18A H18D S5 0.97 2.80 3.70(2) 153.9 . C20 H20B S6 0.97 2.72 3.388(7) 126.5 2_556 C7A H7A1 Cl1 0.97 3.13 3.652(15) 115.5 2 C7A H7A2 Cl2 0.97 2.97 3.91(2) 161.3 . C8 H8A Cl2 0.97 2.80 3.732(12) 162.3 . C8 H8B Cl2 0.97 3.01 3.950(13) 164.9 2_455 C8A H8A1 Cl2 0.97 2.98 3.807(17) 143.8 2_455 C8A H8A2 O1 0.97 3.03 3.60(2) 119.3 1_455 C9 H9A Cl2 0.97 2.80 3.607(5) 141.6 2_556 C10 H10A Cl1 0.97 2.87 3.731(5) 148.2 2_556 C10 H10A Cl3 0.97 2.79 3.537(6) 134.8 2_556 C10 H10A O1 0.97 2.84 3.512(15) 127.4 2_556 C18A H18C O1 0.97 2.61 3.00(2) 103.8 . C19A H19D Cl2 0.97 2.71 3.337(18) 122.4 2_556 C20 H20B Cl1 0.97 2.89 3.654(7) 135.9 2_656 C20 H20A Cl2 0.97 2.99 3.461(7) 111.4 2_556 C20A H20C Cl1 0.97 2.51 3.29(2) 137.5 2_656 C19 H19A N1S 0.97 2.79 3.185(17) 105.1 2_666 C19 H19A C7S 0.97 2.84 3.517(16) 128.0 2_666 C19 H19B N1S 0.97 2.79 3.254(17) 109.8 1_556 C19A H19C N1S 0.97 2.93 3.51(2) 119.0 2_666 C19A H19C N1S 0.97 2.70 3.34(2) 123.7 1_556 C19A H19C C7S 0.97 3.10 3.69(2) 120.3 1_556 C3S H3S Cl1 0.93 2.74 3.592(6) 152.3 1_565 C4S H4S Cl2 0.93 2.94 3.859(6) 168.1 1_565 C6S H6S Cl1 0.93 2.90 3.661(7) 140.2 2 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.889 _refine_diff_density_min -0.801 _refine_diff_density_rms 0.084 data_beta-(BEDT-TTF)2[OsNOCl5] _database_code_depnum_ccdc_archive 'CCDC 258888' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C10 H8 S8)2, OsNOCl5' _chemical_formula_sum 'C20 H16 Cl5 N1 O1 Os1 S8' _chemical_formula_weight 1166.74 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' Cl Cl 0.1484 0.1585 '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' Os Os -1.2165 7.6030 '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' _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 8.7249(3) _cell_length_b 10.3380(5) _cell_length_c 11.0927(6) _cell_angle_alpha 110.410(4) _cell_angle_beta 98.410(4) _cell_angle_gamma 103.834(4) _cell_volume 881.06(7) _cell_formula_units_Z 1 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 18 _cell_measurement_theta_max 20 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.199 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 568 _exptl_absorpt_coefficient_mu 4.971 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.3696 _exptl_absorpt_correction_T_max 0.6919 _exptl_absorpt_process_details ; aplication absorption correction procedure based on psi-scans data using WinGX facilities ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type Mok\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'Enraf Nonius FR590' _diffrn_radiation_monochromator graphite _diffrn_detector 'scintillation LiI' _diffrn_detector_dtime 1.195 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Enraf Nonius CAD4' _diffrn_measurement_method 'non-profiled omega scans' _diffrn_standards_number 3 _diffrn_standards_interval_time 9000 _diffrn_standards_decay_% 0 _diffrn_reflns_number 10214 _diffrn_reflns_av_R_equivalents 0.0212 _diffrn_reflns_av_sigmaI/netI 0.0292 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 30.01 _reflns_number_total 5134 _reflns_number_gt 5031 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0392P)^2^+0.1655P] 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 SHELXL _refine_ls_extinction_coef 0.0031(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5134 _refine_ls_number_parameters 215 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0258 _refine_ls_R_factor_gt 0.0247 _refine_ls_wR_factor_ref 0.0633 _refine_ls_wR_factor_gt 0.0630 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.000 _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 0.0000 0.0000 0.0000 0.02431(5) Uani 1 2 d S . . Cl1 Cl 0.18543(9) 0.02682(8) 0.19303(7) 0.04111(15) Uani 1 1 d . . . Cl2 Cl 0.18007(10) 0.21811(8) 0.00991(8) 0.04422(15) Uani 1 1 d . . . Cl3 Cl 0.1380(3) -0.1313(3) -0.1374(3) 0.0286(6) Uani 0.50 1 d P . . O1 O -0.1628(16) 0.1521(14) 0.1640(12) 0.050(2) Uani 0.50 1 d P . . N1 N -0.1183(17) 0.1034(11) 0.1057(10) 0.043(3) Uani 0.50 1 d P . . S1 S 0.28993(9) 0.65808(8) 0.59243(7) 0.03507(13) Uani 1 1 d . . . S2 S 0.18747(8) 0.39091(7) 0.35347(6) 0.03203(12) Uani 1 1 d . . . S3 S 0.47699(9) 0.51445(7) 0.75258(6) 0.03436(13) Uani 1 1 d . . . S4 S 0.36957(8) 0.24005(7) 0.52058(6) 0.03128(12) Uani 1 1 d . . . S5 S 0.08428(12) 0.80232(9) 0.48862(10) 0.05029(19) Uani 1 1 d . . . S6 S -0.02643(10) 0.49423(9) 0.19812(9) 0.04730(18) Uani 1 1 d . . . S7 S 0.63720(10) 0.40622(9) 0.93387(7) 0.04026(15) Uani 1 1 d . . . S8 S 0.51612(10) 0.08493(8) 0.66568(7) 0.03971(15) Uani 1 1 d . . . C1 C 0.2930(3) 0.4821(3) 0.5182(2) 0.0280(4) Uani 1 1 d . . . C2 C 0.3722(3) 0.4183(3) 0.5880(2) 0.0281(4) Uani 1 1 d . . . C3 C 0.1488(3) 0.6497(3) 0.4591(3) 0.0336(5) Uani 1 1 d . . . C4 C 0.1032(3) 0.5257(3) 0.3481(3) 0.0330(5) Uani 1 1 d . . . C5 C 0.5286(3) 0.3707(3) 0.7752(2) 0.0291(4) Uani 1 1 d . . . C6 C 0.4809(3) 0.2441(3) 0.6661(2) 0.0300(4) Uani 1 1 d . . . C7 C -0.0146(5) 0.7803(4) 0.3224(4) 0.0519(8) Uani 1 1 d . . . H7A H -0.1318 0.7453 0.3095 0.062 Uiso 1 1 calc R . . H7B H 0.0118 0.8750 0.3182 0.062 Uiso 1 1 calc R . . C8 C 0.0311(4) 0.6790(4) 0.2104(4) 0.0451(7) Uani 1 1 d . . . H8A H 0.1482 0.7135 0.2224 0.054 Uiso 1 1 calc R . . H8B H -0.0210 0.6804 0.1276 0.054 Uiso 1 1 calc R . . C9 C 0.6047(5) 0.2277(4) 0.9390(3) 0.0513(8) Uani 1 1 d . . . H9A H 0.7077 0.2071 0.9432 0.062 Uiso 1 1 calc R . . H9B H 0.5744 0.2322 1.0208 0.062 Uiso 1 1 calc R . . C10 C 0.4786(4) 0.1031(4) 0.8259(4) 0.0464(7) Uani 1 1 d . . . H10A H 0.3724 0.1163 0.8276 0.056 Uiso 1 1 calc R . . H10B H 0.4759 0.0140 0.8377 0.056 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 0.02752(7) 0.02250(7) 0.02172(7) 0.00838(5) 0.00122(4) 0.00942(4) Cl1 0.0486(4) 0.0411(3) 0.0317(3) 0.0138(3) -0.0032(3) 0.0199(3) Cl2 0.0492(4) 0.0354(3) 0.0450(4) 0.0177(3) 0.0050(3) 0.0095(3) Cl3 0.0336(7) 0.0272(16) 0.0222(18) 0.0032(13) 0.0067(10) 0.0148(9) O1 0.067(6) 0.038(4) 0.037(5) 0.010(4) 0.004(3) 0.013(3) N1 0.066(7) 0.020(4) 0.019(4) 0.002(3) -0.011(3) -0.010(3) S1 0.0396(3) 0.0335(3) 0.0298(3) 0.0096(2) 0.0036(2) 0.0150(2) S2 0.0348(3) 0.0306(3) 0.0275(3) 0.0116(2) -0.0018(2) 0.0104(2) S3 0.0429(3) 0.0342(3) 0.0240(3) 0.0071(2) 0.0003(2) 0.0203(3) S4 0.0328(3) 0.0321(3) 0.0243(3) 0.0075(2) -0.0002(2) 0.0121(2) S5 0.0559(4) 0.0404(4) 0.0581(5) 0.0191(4) 0.0075(4) 0.0262(3) S6 0.0442(4) 0.0425(4) 0.0489(4) 0.0249(3) -0.0127(3) 0.0073(3) S7 0.0483(4) 0.0423(4) 0.0268(3) 0.0106(3) -0.0039(3) 0.0210(3) S8 0.0524(4) 0.0335(3) 0.0319(3) 0.0095(3) 0.0034(3) 0.0209(3) C1 0.0277(10) 0.0312(11) 0.0237(10) 0.0112(8) 0.0021(8) 0.0095(8) C2 0.0262(10) 0.0339(11) 0.0239(10) 0.0107(9) 0.0024(8) 0.0122(8) C3 0.0299(11) 0.0349(12) 0.0411(13) 0.0196(11) 0.0072(10) 0.0134(9) C4 0.0290(10) 0.0354(12) 0.0354(12) 0.0190(10) -0.0004(9) 0.0093(9) C5 0.0294(10) 0.0334(11) 0.0249(10) 0.0104(9) 0.0026(8) 0.0148(9) C6 0.0280(10) 0.0338(12) 0.0283(11) 0.0116(9) 0.0022(8) 0.0139(9) C7 0.0578(19) 0.062(2) 0.065(2) 0.0441(19) 0.0248(17) 0.0356(17) C8 0.0459(15) 0.0492(17) 0.0554(18) 0.0349(15) 0.0141(13) 0.0195(13) C9 0.085(3) 0.0529(18) 0.0307(13) 0.0221(13) 0.0161(15) 0.0378(18) C10 0.0507(16) 0.0487(17) 0.0545(18) 0.0295(15) 0.0252(14) 0.0207(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Os1 N1 1.895(11) 2 ? Os1 N1 1.895(11) . ? Os1 Cl3 2.343(2) 2 ? Os1 Cl3 2.343(2) . ? Os1 Cl1 2.3743(6) 2 ? Os1 Cl1 2.3743(6) . ? Os1 Cl2 2.3763(8) . ? Os1 Cl2 2.3763(8) 2 ? Cl3 N1 0.455(9) 2 ? O1 Cl3 0.421(8) 2 ? O1 N1 0.873(12) . ? N1 Cl3 0.455(9) 2 ? S1 C1 1.724(3) . ? S1 C3 1.743(3) . ? S2 C1 1.723(2) . ? S2 C4 1.738(3) . ? S3 C2 1.723(2) . ? S3 C5 1.738(3) . ? S4 C2 1.723(3) . ? S4 C6 1.740(2) . ? S5 C3 1.741(3) . ? S5 C7 1.828(4) . ? S6 C4 1.746(3) . ? S6 C8 1.805(3) . ? S7 C5 1.740(2) . ? S7 C9 1.822(4) . ? S8 C6 1.743(3) . ? S8 C10 1.808(3) . ? C1 C2 1.389(3) . ? C3 C4 1.353(4) . ? C5 C6 1.356(3) . ? C7 C8 1.496(5) . ? C9 C10 1.495(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Os1 N1 180.0(6) 2 . ? N1 Os1 Cl3 177.9(4) 2 2 ? N1 Os1 Cl3 2.1(4) . 2 ? N1 Os1 Cl3 2.1(4) 2 . ? N1 Os1 Cl3 177.9(4) . . ? Cl3 Os1 Cl3 180.00(12) 2 . ? N1 Os1 Cl1 90.9(4) 2 2 ? N1 Os1 Cl1 89.1(4) . 2 ? Cl3 Os1 Cl1 91.04(7) 2 2 ? Cl3 Os1 Cl1 88.96(7) . 2 ? N1 Os1 Cl1 89.1(4) 2 . ? N1 Os1 Cl1 90.9(4) . . ? Cl3 Os1 Cl1 88.96(7) 2 . ? Cl3 Os1 Cl1 91.04(7) . . ? Cl1 Os1 Cl1 180.0 2 . ? N1 Os1 Cl2 88.2(4) 2 . ? N1 Os1 Cl2 91.8(4) . . ? Cl3 Os1 Cl2 91.09(8) 2 . ? Cl3 Os1 Cl2 88.91(8) . . ? Cl1 Os1 Cl2 92.17(3) 2 . ? Cl1 Os1 Cl2 87.83(3) . . ? N1 Os1 Cl2 91.8(4) 2 2 ? N1 Os1 Cl2 88.2(4) . 2 ? Cl3 Os1 Cl2 88.91(8) 2 2 ? Cl3 Os1 Cl2 91.09(8) . 2 ? Cl1 Os1 Cl2 87.83(3) 2 2 ? Cl1 Os1 Cl2 92.17(3) . 2 ? Cl2 Os1 Cl2 180.00(3) . 2 ? N1 Cl3 Os1 8.8(18) 2 . ? Cl3 O1 N1 4.4(11) 2 . ? Cl3 N1 O1 4.1(11) 2 . ? Cl3 N1 Os1 169(2) 2 . ? O1 N1 Os1 172(2) . . ? C1 S1 C3 95.71(12) . . ? C1 S2 C4 95.30(12) . . ? C2 S3 C5 96.04(12) . . ? C2 S4 C6 95.40(12) . . ? C3 S5 C7 103.58(16) . . ? C4 S6 C8 97.43(15) . . ? C5 S7 C9 104.42(14) . . ? C6 S8 C10 96.90(14) . . ? C2 C1 S2 122.7(2) . . ? C2 C1 S1 121.98(19) . . ? S2 C1 S1 115.25(14) . . ? C1 C2 S4 123.65(19) . . ? C1 C2 S3 121.0(2) . . ? S4 C2 S3 115.36(14) . . ? C4 C3 S5 129.0(2) . . ? C4 C3 S1 115.9(2) . . ? S5 C3 S1 115.09(17) . . ? C3 C4 S2 117.27(19) . . ? C3 C4 S6 125.0(2) . . ? S2 C4 S6 117.67(16) . . ? C6 C5 S3 115.95(18) . . ? C6 C5 S7 127.5(2) . . ? S3 C5 S7 116.51(14) . . ? C5 C6 S4 117.19(19) . . ? C5 C6 S8 124.06(19) . . ? S4 C6 S8 118.68(15) . . ? C8 C7 S5 115.3(2) . . ? C7 C8 S6 113.2(2) . . ? C10 C9 S7 116.6(2) . . ? C9 C10 S8 113.0(2) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C7 H7B Cl1 0.97 2.77 3.572(4) 140.2 1_565 C8 H8A Cl1 0.97 3.31 3.609(3) 100.0 1_565 C8 H8B Cl2 0.97 2.56 3.455(3) 153.6 2_565 C8 H8A S7 0.97 2.93 3.647(3) 131.3 2_666 C9 H9A O1 0.97 2.84 3.405(15) 117.9 1_656 C9 H9A N1 0.97 2.83 3.570(14) 133.3 1_656 C9 H9A Cl1 0.97 2.82 3.581(4) 136.1 2_656 C9 H9A Cl3 0.97 2.81 3.468(4) 125.7 2_656 C10 H10B Cl1 0.97 3.13 3.508(3) 104.8 2_656 C10 H10A Cl3 0.97 3.05 3.530(4) 112.0 1_556 C10 H10B O1 0.97 2.85 3.373(14) 114.7 2_556 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.01 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.411 _refine_diff_density_min -1.130 _refine_diff_density_rms 0.121 data_delta-(BEDT-TTF)4[OsNOCl5]1.33(C6H5NO2)0.67 _database_code_depnum_ccdc_archive 'CCDC 258889' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C10 H8 S8)4, (OsNOCl5)1.33, (C6H5NO2)0.67' _chemical_formula_sum 'C44 H35.33 Cl6.66 N2 O2.67 Os1.33 S32' _chemical_formula_weight 2150.83 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' Cl Cl 0.1484 0.1585 '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' Os Os -1.2165 7.6030 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M I2/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 15.034(3) _cell_length_b 6.728(2) _cell_length_c 35.211(6) _cell_angle_alpha 90.00 _cell_angle_beta 92.980(10) _cell_angle_gamma 90.00 _cell_volume 3556.7(14) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 18 _cell_measurement_theta_max 20 _exptl_crystal_description 'not distinctly faced' _exptl_crystal_colour black _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.008 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2123 _exptl_absorpt_coefficient_mu 3.620 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.4305 _exptl_absorpt_correction_T_max 0.6705 _exptl_absorpt_process_details ; aplication absorption correction procedure based on psi-scans data using WinGX facilities ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type Mok\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'Enraf Nonius FR590' _diffrn_radiation_monochromator graphite _diffrn_detector 'scintillation LiI' _diffrn_detector_dtime 1.195 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Enraf Nonius CAD4' _diffrn_measurement_method 'non-profiled omega scans' _diffrn_standards_number 3 _diffrn_standards_interval_time 9000 _diffrn_standards_decay_% 0 _diffrn_reflns_number 6222 _diffrn_reflns_av_R_equivalents 0.1140 _diffrn_reflns_av_sigmaI/netI 0.1191 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 24.97 _reflns_number_total 3100 _reflns_number_gt 2070 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0721P)^2^+16.0858P] 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 3100 _refine_ls_number_parameters 210 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0836 _refine_ls_R_factor_gt 0.0493 _refine_ls_wR_factor_ref 0.1563 _refine_ls_wR_factor_gt 0.1389 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.100 _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 S1 S 0.87333(16) 0.5431(3) -0.01270(5) 0.0513(6) Uani 1 1 d . A . S2 S 0.84769(15) 0.9624(3) -0.03216(5) 0.0508(6) Uani 1 1 d . A . S6 S 0.77463(16) 0.8884(3) -0.10989(5) 0.0550(6) Uani 1 1 d . . . S4 S 0.91161(16) 1.0859(3) 0.05330(5) 0.0539(6) Uani 1 1 d . . . S7 S 1.01088(19) 0.7435(4) 0.15058(6) 0.0690(7) Uani 1 1 d . . . S3 S 0.95329(15) 0.6716(3) 0.07052(5) 0.0507(6) Uani 1 1 d . . . S5 S 0.7980(2) 0.3882(4) -0.08493(7) 0.0830(10) Uani 1 1 d . . . S8 S 0.96039(19) 1.2375(4) 0.12921(7) 0.0693(7) Uani 1 1 d . . . C1 C 0.8816(5) 0.7899(10) 0.00180(19) 0.0400(16) Uani 1 1 d . . . C2 C 0.9131(5) 0.8429(12) 0.0372(2) 0.0440(17) Uani 1 1 d . A . C3 C 0.8248(5) 0.5948(12) -0.05716(19) 0.0467(19) Uani 1 1 d . A . C4 C 0.8145(5) 0.7885(11) -0.06698(19) 0.0441(18) Uani 1 1 d . A . C5 C 0.9726(5) 0.8419(12) 0.1071(2) 0.0445(18) Uani 1 1 d . A . C6 C 0.9531(5) 1.0308(12) 0.0990(2) 0.0461(18) Uani 1 1 d . A . C7A C 0.7486(13) 0.484(3) -0.1267(4) 0.049(4) Uiso 0.53(2) 1 d P A 1 H7A1 H 0.7483 0.3818 -0.1462 0.059 Uiso 0.53(2) 1 calc PR A 1 H7A2 H 0.6872 0.5173 -0.1224 0.059 Uiso 0.53(2) 1 calc PR A 1 C8A C 0.7973(12) 0.676(2) -0.1419(4) 0.051(5) Uiso 0.53(2) 1 d P A 1 H8A1 H 0.7752 0.7054 -0.1676 0.062 Uiso 0.53(2) 1 calc PR A 1 H8A2 H 0.8609 0.6520 -0.1421 0.062 Uiso 0.53(2) 1 calc PR A 1 C7B C 0.7941(15) 0.498(3) -0.1319(5) 0.049(5) Uiso 0.47(2) 1 d P A 2 H7B1 H 0.8538 0.5379 -0.1378 0.058 Uiso 0.47(2) 1 calc PR A 2 H7B2 H 0.7743 0.3977 -0.1503 0.058 Uiso 0.47(2) 1 calc PR A 2 C8B C 0.7363(14) 0.666(3) -0.1357(5) 0.055(6) Uiso 0.47(2) 1 d P A 2 H8B1 H 0.6786 0.6288 -0.1269 0.066 Uiso 0.47(2) 1 calc PR A 2 H8B2 H 0.7283 0.6988 -0.1625 0.066 Uiso 0.47(2) 1 calc PR A 2 C9A C 0.9917(15) 0.938(3) 0.1826(5) 0.052(5) Uiso 0.53(2) 1 d P A 1 H9A1 H 0.9283 0.9431 0.1865 0.062 Uiso 0.53(2) 1 calc PR A 1 H9A2 H 1.0217 0.9053 0.2069 0.062 Uiso 0.53(2) 1 calc PR A 1 C10A C 1.0195(13) 1.126(2) 0.1716(4) 0.044(4) Uiso 0.53(2) 1 d P A 1 H10A H 1.0824 1.1184 0.1667 0.052 Uiso 0.53(2) 1 calc PR A 1 H10B H 1.0137 1.2157 0.1928 0.052 Uiso 0.53(2) 1 calc PR A 1 C9B C 0.9515(18) 0.924(3) 0.1817(6) 0.062(6) Uiso 0.47(2) 1 d P A 2 H9B1 H 0.8877 0.9098 0.1768 0.074 Uiso 0.47(2) 1 calc PR A 2 H9B2 H 0.9650 0.8903 0.2082 0.074 Uiso 0.47(2) 1 calc PR A 2 C10B C 0.9777(19) 1.137(3) 0.1750(6) 0.064(6) Uiso 0.47(2) 1 d P A 2 H10C H 1.0406 1.1503 0.1822 0.076 Uiso 0.47(2) 1 calc PR A 2 H10D H 0.9457 1.2198 0.1923 0.076 Uiso 0.47(2) 1 calc PR A 2 Os1 Os 0.2500 0.7500 0.2500 0.0528(3) Uani 0.702(3) 2 d SPD . . Cl1 Cl 0.3730(4) 0.9521(11) 0.27144(14) 0.0711(13) Uani 0.526(2) 1 d PD . . N1 N 0.333(2) 0.911(5) 0.2663(11) 0.042(11) Uiso 0.1755(8) 1 d PD . . O1 O 0.388(4) 1.033(8) 0.2700(19) 0.09(2) Uiso 0.1755(8) 1 d PD . . Cl2 Cl 0.3530(5) 0.5196(10) 0.22566(14) 0.0835(17) Uani 0.526(2) 1 d PD . . N2 N 0.3244(11) 0.579(2) 0.2308(4) 0.069(18) Uiso 0.1755(8) 1 d PD . . O2 O 0.3737(14) 0.466(3) 0.2177(5) 0.10(2) Uiso 0.1755(8) 1 d PD . . Cl3 Cl 0.2397(3) 0.9245(6) 0.19194(8) 0.0750(10) Uani 0.702(3) 1 d PD . . 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 S1 0.0803(14) 0.0381(11) 0.0339(9) 0.0003(8) -0.0115(9) 0.0073(10) S2 0.0804(14) 0.0389(11) 0.0316(9) 0.0011(8) -0.0134(9) 0.0048(10) S6 0.0812(15) 0.0456(12) 0.0359(9) -0.0016(8) -0.0181(9) 0.0093(11) S4 0.0818(15) 0.0399(11) 0.0386(10) -0.0011(8) -0.0111(9) 0.0088(10) S7 0.1093(19) 0.0609(14) 0.0340(10) -0.0008(10) -0.0216(11) 0.0153(14) S3 0.0778(14) 0.0402(11) 0.0327(9) -0.0013(8) -0.0100(9) 0.0101(10) S5 0.149(3) 0.0375(12) 0.0570(13) -0.0050(10) -0.0407(15) 0.0006(14) S8 0.1022(18) 0.0466(13) 0.0560(13) -0.0150(10) -0.0251(12) 0.0109(13) C1 0.052(4) 0.033(4) 0.035(3) 0.000(3) -0.003(3) 0.011(3) C2 0.053(4) 0.045(4) 0.033(3) 0.000(3) -0.005(3) 0.001(4) C3 0.061(5) 0.046(5) 0.032(3) -0.003(3) -0.014(3) 0.004(4) C4 0.060(4) 0.044(5) 0.027(3) -0.002(3) -0.009(3) 0.009(4) C5 0.059(5) 0.042(4) 0.031(3) -0.002(3) -0.009(3) 0.004(4) C6 0.054(4) 0.050(5) 0.033(4) -0.009(3) -0.007(3) 0.002(4) Os1 0.0720(5) 0.0610(5) 0.0240(3) 0.0013(3) -0.0103(2) 0.0122(4) Cl1 0.077(4) 0.087(5) 0.047(2) 0.011(3) -0.012(2) -0.013(4) Cl2 0.111(4) 0.086(4) 0.052(2) -0.006(3) -0.003(3) 0.041(4) Cl3 0.103(3) 0.087(3) 0.0334(14) 0.0138(15) -0.0126(15) 0.012(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 S1 C3 1.728(7) . ? S1 C1 1.739(7) . ? S2 C1 1.724(7) . ? S2 C4 1.749(7) . ? S6 C4 1.732(7) . ? S6 C8B 1.829(19) . ? S6 C8A 1.865(16) . ? S4 C2 1.732(8) . ? S4 C6 1.734(7) . ? S7 C5 1.737(7) . ? S7 C9A 1.758(17) . ? S7 C9B 1.89(2) . ? S3 C2 1.732(7) . ? S3 C5 1.738(8) . ? S5 C3 1.735(8) . ? S5 C7A 1.737(15) . ? S5 C7B 1.809(17) . ? S8 C6 1.751(8) . ? S8 C10B 1.75(2) . ? S8 C10A 1.855(15) . ? C1 C2 1.357(10) . ? C3 C4 1.355(11) . ? C5 C6 1.332(11) . ? C7A C8A 1.59(3) . ? C7B C8B 1.43(3) . ? C9A C10A 1.40(2) . ? C9B C10B 1.51(3) . ? Os1 N1 1.726(19) . ? Os1 N2 1.762(19) . ? Os1 Cl3 2.356(3) . ? Os1 Cl2 2.382(7) . ? Os1 Cl1 2.387(6) . ? N1 O1 1.17(2) . ? N2 O2 1.18(2) . ? 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 C3 S1 C1 95.4(3) . . ? C1 S2 C4 95.7(3) . . ? C4 S6 C8B 101.6(7) . . ? C4 S6 C8A 99.4(6) . . ? C8B S6 C8A 29.9(7) . . ? C2 S4 C6 95.3(4) . . ? C5 S7 C9A 102.9(7) . . ? C5 S7 C9B 97.0(8) . . ? C2 S3 C5 95.9(4) . . ? C3 S5 C7A 104.9(6) . . ? C3 S5 C7B 100.7(7) . . ? C6 S8 C10B 104.8(8) . . ? C6 S8 C10A 100.4(6) . . ? C2 C1 S2 122.4(6) . . ? C2 C1 S1 122.4(6) . . ? S2 C1 S1 115.1(4) . . ? C1 C2 S3 122.7(6) . . ? C1 C2 S4 122.6(6) . . ? S3 C2 S4 114.6(4) . . ? C4 C3 S1 117.5(5) . . ? C4 C3 S5 127.3(5) . . ? S1 C3 S5 115.1(5) . . ? C3 C4 S6 128.7(6) . . ? C3 C4 S2 116.1(5) . . ? S6 C4 S2 115.2(4) . . ? C6 C5 S7 127.8(6) . . ? C6 C5 S3 116.2(5) . . ? S7 C5 S3 115.9(5) . . ? C5 C6 S4 118.0(5) . . ? C5 C6 S8 128.3(6) . . ? S4 C6 S8 113.7(5) . . ? C8A C7A S5 113.7(12) . . ? C7A C8A S6 108.6(12) . . ? C8B C7B S5 113.5(15) . . ? C7B C8B S6 115.4(15) . . ? C10A C9A S7 115.8(13) . . ? C9A C10A S8 116.9(12) . . ? C10B C9B S7 112.6(16) . . ? C9B C10B S8 118.8(15) . . ? N1 Os1 N2 94.2(15) . . ? N1 Os1 Cl3 89.5(14) . . ? N2 Os1 Cl3 90.3(4) . . ? N1 Os1 Cl2 93.1(14) . . ? Cl3 Os1 Cl2 91.54(16) . . ? N2 Os1 Cl1 89.7(4) . . ? Cl3 Os1 Cl1 90.32(16) . . ? Cl2 Os1 Cl1 88.7(2) . . ? O1 N1 Os1 167(5) . . ? O2 N2 Os1 179.5(14) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C7A H7A2 S8 0.97 2.91 3.55(2) 124.4 2_645 C8A H8A1 Cl3 0.97 2.64 3.248(17) 121.2 5_675 C8A H8A2 C10A 0.97 2.59 3.28(3) 127.8 5_775 C8A H8A1 O1 0.97 3.07 3.58(7) 114.5 3_544 C8A H8A1 Cl1 0.97 3.16 3.637(17) 112.0 3_544 C8A H8A2 S8 0.97 2.80 3.694(18) 153.2 5_775 C7B H7B1 S7 0.97 2.83 3.44(2) 121.9 5_765 C7B H7B2 Cl3 0.97 2.62 3.561(19) 163.9 5_665 C7B H7B2 Cl1 0.97 3.22 3.67(2) 110.8 3_544 C8B H8B2 O2 0.97 2.65 3.37(3) 130.9 5_665 C8B H8B2 Cl3 0.97 2.79 3.42(2) 123.6 5_675 C8B H8B1 C5 0.97 2.81 3.55(2) 134.3 2_655 C8B H8B2 Cl2 0.97 2.88 3.599(19) 131.3 5_665 C8B H8B2 C9B 0.97 3.14 3.62(3) 112.5 2_655 C9A H9A1 O2 0.97 3.09 3.50(3) 107.3 6_665 C9A H9A1 O1 0.97 3.04 3.53(7) 112.7 6_675 C9A H9A2 Cl1 0.97 2.96 3.65(2) 128.9 7_665 C10A H10B O1 0.97 2.56 3.34(5) 137.1 7_675 C10A H10A C8A 0.97 2.47 3.28(3) 140.3 5_775 C10A H10A Cl3 0.97 2.80 3.613(19) 141.4 1_655 C9B H9B1 Cl3 0.97 2.57 3.38(3) 141.2 6_675 C9B H9B1 C8B 0.97 2.82 3.62(3) 140.2 2_655 C9B H9B2 O1 0.97 2.57 3.31(7) 133.3 6_675 C9B H9B2 Cl1 0.97 2.88 3.53(2) 124.9 6_675 C9B H9B2 O2 0.97 2.79 3.16(4) 103.6 6_665 C10B H10D Cl2 0.97 2.56 3.52(3) 168.1 6_675 C10B H10D N2 0.97 2.69 3.64(3) 167.1 6_675 C10B H10C O1 0.97 2.89 3.51(4) 123.1 7_675 C10B H10D Cl3 0.97 3.25 3.68(3) 109.4 6_675 C10B H10D O2 0.97 2.56 3.48(3) 157.7 6_675 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.408 _refine_diff_density_min -1.226 _refine_diff_density_rms 0.130 data_alfa'-(BEDT-TTF)4[OsNOCl5]C6H5NO2 _database_code_depnum_ccdc_archive 'CCDC 258890' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C10 H8 S8)4, OsNOCl5, C6H5NO2' _chemical_formula_sum 'C46 H37 Cl5 N2 O3 Os S32' _chemical_formula_weight 2059.15 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' Cl Cl 0.1484 0.1585 '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' Os Os -1.2165 7.6030 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6275(6) _cell_length_b 11.1599(6) _cell_length_c 18.0640(10) _cell_angle_alpha 101.478(5) _cell_angle_beta 91.926(6) _cell_angle_gamma 110.894(5) _cell_volume 1765.31(18) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 18 _cell_measurement_theta_max 20 _exptl_crystal_description parallelepiped _exptl_crystal_colour black _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.937 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 2.985 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.3814 _exptl_absorpt_correction_T_max 0.5866 _exptl_absorpt_process_details ;aplication absorption correction procedure based on psi-scans data using WinGX facilities ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 292(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type Mok\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'Enraf Nonius FR590' _diffrn_radiation_monochromator graphite _diffrn_detector 'scintillation LiI' _diffrn_detector_dtime 1.195 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Enraf Nonius CAD4' _diffrn_measurement_method 'non-profiled omega scans' _diffrn_standards_number 3 _diffrn_standards_interval_time 9000 _diffrn_standards_decay_% 0 _diffrn_reflns_number 10582 _diffrn_reflns_av_R_equivalents 0.0160 _diffrn_reflns_av_sigmaI/netI 0.0236 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 30.03 _reflns_number_total 10278 _reflns_number_gt 9343 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0409P)^2^+1.9900P] 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 SHELXL _refine_ls_extinction_coef 0.0071(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10278 _refine_ls_number_parameters 399 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0390 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0941 _refine_ls_wR_factor_gt 0.0793 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _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 S1 S 0.11740(11) -0.09880(9) 0.52126(5) 0.0498(2) Uani 1 1 d . . . S2 S 0.38007(10) 0.14456(9) 0.57403(4) 0.04581(18) Uani 1 1 d . . . S3 S 0.21939(10) -0.13052(9) 0.35391(4) 0.04437(18) Uani 1 1 d . . . S4 S 0.47572(11) 0.11833(9) 0.40233(5) 0.04762(19) Uani 1 1 d . . . S5 S -0.00735(12) -0.09591(10) 0.66674(5) 0.0549(2) Uani 1 1 d . . . S6 S 0.31328(12) 0.19167(10) 0.73270(5) 0.0524(2) Uani 1 1 d . . . S7 S 0.27207(12) -0.17664(10) 0.19319(5) 0.0545(2) Uani 1 1 d . . . S8 S 0.57454(11) 0.12118(10) 0.24946(5) 0.0510(2) Uani 1 1 d . . . C1 C 0.2786(4) 0.0143(3) 0.49960(17) 0.0423(7) Uani 1 1 d . . . C2 C 0.3213(4) 0.0020(3) 0.42724(17) 0.0409(6) Uani 1 1 d . . . C3 C 0.1378(4) -0.0184(3) 0.61666(17) 0.0401(6) Uani 1 1 d . . . C4 C 0.2597(4) 0.0918(3) 0.64132(17) 0.0392(6) Uani 1 1 d . . . C5 C 0.3306(4) -0.0765(3) 0.28396(17) 0.0391(6) Uani 1 1 d . A . C6 C 0.4483(4) 0.0388(3) 0.30629(17) 0.0390(6) Uani 1 1 d . A . C7 C 0.0305(5) 0.0286(4) 0.7532(2) 0.0554(9) Uani 1 1 d . . . H7A H 0.0003 0.0985 0.7431 0.066 Uiso 1 1 calc R . . H7B H -0.0301 -0.0096 0.7906 0.066 Uiso 1 1 calc R . . C8 C 0.1903(5) 0.0867(4) 0.7861(2) 0.0543(9) Uani 1 1 d . . . H8A H 0.2244 0.0158 0.7895 0.065 Uiso 1 1 calc R . . H8B H 0.1976 0.1373 0.8374 0.065 Uiso 1 1 calc R . . C9A C 0.4011(6) -0.0885(5) 0.1343(3) 0.0496(15) Uiso 0.722(12) 1 d P A 1 H9A H 0.4868 -0.1150 0.1337 0.060 Uiso 0.722(12) 1 calc PR A 1 H9B H 0.3523 -0.1149 0.0826 0.060 Uiso 0.722(12) 1 calc PR A 1 C10A C 0.4566(7) 0.0597(6) 0.1591(3) 0.0524(14) Uiso 0.722(12) 1 d P A 1 H10A H 0.3716 0.0869 0.1635 0.063 Uiso 0.722(12) 1 calc PR A 1 H10B H 0.5130 0.0982 0.1206 0.063 Uiso 0.722(12) 1 calc PR A 1 C9B C 0.3385(17) -0.0520(14) 0.1390(8) 0.052(4) Uiso 0.278(12) 1 d P A 2 H9C H 0.3173 -0.0937 0.0852 0.062 Uiso 0.278(12) 1 calc PR A 2 H9D H 0.2849 0.0073 0.1491 0.062 Uiso 0.278(12) 1 calc PR A 2 C10B C 0.500(2) 0.0239(18) 0.1573(9) 0.059(4) Uiso 0.278(12) 1 d P A 2 H10C H 0.5282 0.0817 0.1223 0.070 Uiso 0.278(12) 1 calc PR A 2 H10D H 0.5498 -0.0380 0.1459 0.070 Uiso 0.278(12) 1 calc PR A 2 S11 S 0.17463(11) 0.39137(9) 0.63060(5) 0.04769(19) Uani 1 1 d . . . S12 S 0.13286(12) 0.63700(10) 0.62029(5) 0.0495(2) Uani 1 1 d . . . S13 S 0.28560(13) 0.36939(10) 0.46354(5) 0.0527(2) Uani 1 1 d . . . S14 S 0.24291(12) 0.61365(9) 0.45181(5) 0.0505(2) Uani 1 1 d . . . S15 S 0.11344(14) 0.40333(11) 0.78964(6) 0.0584(3) Uani 1 1 d . . . S16 S 0.05934(12) 0.69571(9) 0.77708(5) 0.0512(2) Uani 1 1 d . . . S17 S 0.37366(18) 0.31790(12) 0.30969(6) 0.0730(4) Uani 1 1 d . . . S18 S 0.32527(12) 0.60958(9) 0.29691(5) 0.0480(2) Uani 1 1 d . . . C11 C 0.1856(4) 0.5076(3) 0.57662(17) 0.0415(7) Uani 1 1 d . . . C12 C 0.2323(4) 0.4987(3) 0.50644(17) 0.0411(6) Uani 1 1 d . . . C13 C 0.1290(4) 0.4781(3) 0.71226(18) 0.0427(7) Uani 1 1 d . . . C14 C 0.1096(4) 0.5894(3) 0.70753(18) 0.0419(7) Uani 1 1 d . . . C15 C 0.3170(4) 0.4199(4) 0.37781(18) 0.0447(7) Uani 1 1 d . . . C16 C 0.2983(4) 0.5311(3) 0.37254(17) 0.0393(6) Uani 1 1 d . . . C17 C 0.0277(5) 0.4956(4) 0.8527(2) 0.0505(8) Uani 1 1 d . . . H17A H -0.0774 0.4663 0.8340 0.061 Uiso 1 1 calc R . . H17B H 0.0334 0.4763 0.9025 0.061 Uiso 1 1 calc R . . C18 C 0.0981(5) 0.6426(4) 0.8610(2) 0.0567(9) Uani 1 1 d . . . H18A H 0.2056 0.6703 0.8723 0.068 Uiso 1 1 calc R . . H18B H 0.0617 0.6857 0.9037 0.068 Uiso 1 1 calc R . . C19 C 0.4523(4) 0.4246(4) 0.2472(2) 0.0511(8) Uani 1 1 d . . . H19A H 0.5453 0.4928 0.2727 0.061 Uiso 1 1 calc R . . H19B H 0.4758 0.3741 0.2025 0.061 Uiso 1 1 calc R . . C20 C 0.3518(5) 0.4884(4) 0.22222(19) 0.0476(8) Uani 1 1 d . . . H20A H 0.2549 0.4206 0.2017 0.057 Uiso 1 1 calc R . . H20B H 0.3933 0.5303 0.1816 0.057 Uiso 1 1 calc R . . C1S C 0.3452(9) 0.6201(8) 0.0085(6) 0.091(4) Uiso 0.498(4) 1 d PG . . H1S H 0.2840 0.6688 0.0115 0.109 Uiso 0.498(4) 1 calc PR . . C2S C 0.4929(10) 0.6758(6) -0.0059(5) 0.107(4) Uiso 0.498(4) 1 d PG . . H2S H 0.5304 0.7617 -0.0125 0.129 Uiso 0.498(4) 1 calc PR . . C3S C 0.5844(7) 0.6030(7) -0.0104(5) 0.070(3) Uiso 0.498(4) 1 d PG . . H3S H 0.6832 0.6403 -0.0200 0.084 Uiso 0.498(4) 1 calc PR . . C4S C 0.5284(7) 0.4746(7) -0.0006(5) 0.073(3) Uiso 0.498(4) 1 d PG . . C5S C 0.3808(7) 0.4190(6) 0.0137(4) 0.060(2) Uiso 0.498(4) 1 d PG . . H5S H 0.3433 0.3331 0.0203 0.072 Uiso 0.498(4) 1 calc PR . . C6S C 0.2892(6) 0.4917(8) 0.0183(5) 0.076(3) Uiso 0.498(4) 1 d PG . . H6S H 0.1904 0.4545 0.0279 0.092 Uiso 0.498(4) 1 calc PR . . N1S N 0.6204(14) 0.3970(12) -0.0016(7) 0.093(3) Uiso 0.498(4) 1 d PD . . O1S O 0.7356(14) 0.4299(14) -0.0291(8) 0.143(4) Uiso 0.498(4) 1 d PD . . O2S O 0.5859(15) 0.3011(12) 0.0247(8) 0.146(5) Uiso 0.498(4) 1 d PD . . Os1 Os 0.0000 0.0000 0.0000 0.03907(6) Uani 1 2 d SD . . Cl1 Cl -0.00640(17) -0.17714(11) 0.05608(7) 0.0530(3) Uani 0.75 1 d PD B 1 N1 N -0.0184(16) -0.1380(12) 0.0454(8) 0.040(3) Uiso 0.25 1 d PD B 2 O1 O -0.026(2) -0.2249(14) 0.0691(10) 0.080(5) Uiso 0.25 1 d PD B 2 Cl2 Cl 0.22579(13) -0.00982(15) -0.04496(8) 0.0556(3) Uani 0.75 1 d PD B 1 N2 N 0.1715(15) 0.0052(15) -0.0391(9) 0.047(3) Uiso 0.25 1 d PD B 2 O2 O 0.2866(17) 0.011(2) -0.0538(13) 0.098(6) Uiso 0.25 1 d PD B 2 Cl3 Cl 0.14264(10) 0.15888(8) 0.11022(4) 0.0527(2) Uani 1 1 d D B . 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 S1 0.0626(5) 0.0500(5) 0.0321(4) 0.0050(3) 0.0144(3) 0.0169(4) S2 0.0562(5) 0.0522(5) 0.0286(3) 0.0094(3) 0.0152(3) 0.0186(4) S3 0.0581(5) 0.0458(4) 0.0294(3) 0.0102(3) 0.0147(3) 0.0177(4) S4 0.0603(5) 0.0488(4) 0.0301(3) 0.0047(3) 0.0109(3) 0.0176(4) S5 0.0659(6) 0.0499(5) 0.0433(4) 0.0091(4) 0.0238(4) 0.0142(4) S6 0.0632(5) 0.0564(5) 0.0297(4) 0.0041(3) 0.0161(3) 0.0147(4) S7 0.0686(6) 0.0530(5) 0.0283(3) 0.0054(3) 0.0123(4) 0.0079(4) S8 0.0512(5) 0.0525(5) 0.0436(4) 0.0063(4) 0.0216(4) 0.0136(4) C1 0.0584(19) 0.0502(17) 0.0264(13) 0.0104(12) 0.0112(12) 0.0283(15) C2 0.0550(18) 0.0475(17) 0.0276(13) 0.0115(12) 0.0119(12) 0.0255(14) C3 0.0522(17) 0.0433(16) 0.0295(13) 0.0102(11) 0.0147(12) 0.0214(14) C4 0.0525(17) 0.0434(15) 0.0275(12) 0.0107(11) 0.0138(12) 0.0225(14) C5 0.0525(17) 0.0437(16) 0.0280(13) 0.0081(11) 0.0119(12) 0.0255(14) C6 0.0480(16) 0.0447(16) 0.0300(13) 0.0085(11) 0.0109(11) 0.0234(13) C7 0.060(2) 0.067(2) 0.0427(18) 0.0134(17) 0.0263(16) 0.0254(19) C8 0.066(2) 0.072(2) 0.0355(16) 0.0198(16) 0.0201(16) 0.032(2) S11 0.0621(5) 0.0552(5) 0.0305(3) 0.0080(3) 0.0122(3) 0.0276(4) S12 0.0688(6) 0.0532(5) 0.0307(4) 0.0084(3) 0.0132(3) 0.0273(4) S13 0.0784(6) 0.0604(5) 0.0337(4) 0.0164(4) 0.0191(4) 0.0384(5) S14 0.0769(6) 0.0463(4) 0.0315(4) 0.0052(3) 0.0170(4) 0.0278(4) S15 0.0842(7) 0.0629(6) 0.0442(5) 0.0229(4) 0.0322(5) 0.0383(5) S16 0.0708(6) 0.0460(4) 0.0387(4) 0.0102(3) 0.0257(4) 0.0218(4) S17 0.1319(11) 0.0711(7) 0.0534(6) 0.0293(5) 0.0507(7) 0.0701(8) S18 0.0734(6) 0.0424(4) 0.0320(4) 0.0093(3) 0.0151(4) 0.0246(4) C11 0.0433(16) 0.0508(18) 0.0294(13) 0.0071(12) 0.0068(11) 0.0172(14) C12 0.0465(16) 0.0483(17) 0.0275(13) 0.0071(12) 0.0069(11) 0.0169(14) C13 0.0437(16) 0.0487(17) 0.0310(14) 0.0083(12) 0.0129(12) 0.0114(13) C14 0.0436(16) 0.0459(16) 0.0314(13) 0.0049(12) 0.0134(12) 0.0119(13) C15 0.0592(19) 0.0538(19) 0.0302(14) 0.0111(13) 0.0155(13) 0.0299(16) C16 0.0469(16) 0.0431(16) 0.0279(13) 0.0057(11) 0.0086(11) 0.0174(13) C17 0.063(2) 0.058(2) 0.0344(15) 0.0133(14) 0.0184(15) 0.0254(17) C18 0.070(2) 0.057(2) 0.0356(16) 0.0010(15) 0.0049(16) 0.0198(19) C19 0.055(2) 0.062(2) 0.0393(16) 0.0094(15) 0.0182(15) 0.0254(17) C20 0.064(2) 0.0466(18) 0.0310(14) 0.0034(13) 0.0074(14) 0.0220(16) Os1 0.04645(10) 0.03977(10) 0.02516(8) -0.00093(6) 0.00397(6) 0.01349(7) Cl1 0.0686(9) 0.0517(8) 0.0358(6) 0.0115(6) 0.0101(5) 0.0178(7) Cl2 0.0585(9) 0.0637(8) 0.0417(6) 0.0128(5) 0.0137(6) 0.0180(7) Cl3 0.0628(5) 0.0496(4) 0.0303(3) -0.0027(3) 0.0008(3) 0.0094(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 S1 C1 1.731(4) . ? S1 C3 1.746(3) . ? S2 C1 1.731(4) . ? S2 C4 1.749(3) . ? S3 C2 1.733(4) . ? S3 C5 1.744(3) . ? S4 C2 1.732(4) . ? S4 C6 1.748(3) . ? S5 C3 1.747(3) . ? S5 C7 1.800(4) . ? S6 C4 1.742(3) . ? S6 C8 1.800(4) . ? S7 C5 1.736(3) . ? S7 C9B 1.803(14) . ? S7 C9A 1.810(5) . ? S8 C6 1.743(3) . ? S8 C10B 1.764(16) . ? S8 C10A 1.816(6) . ? C1 C2 1.379(4) . ? C3 C4 1.344(5) . ? C5 C6 1.351(5) . ? C7 C8 1.488(6) . ? C9A C10A 1.510(8) . ? C9B C10B 1.47(2) . ? S11 C11 1.748(4) . ? S11 C13 1.757(3) . ? S12 C11 1.750(4) . ? S12 C14 1.757(3) . ? S13 C12 1.748(3) . ? S13 C15 1.751(3) . ? S14 C12 1.746(3) . ? S14 C16 1.749(3) . ? S15 C13 1.750(3) . ? S15 C17 1.801(4) . ? S16 C14 1.754(3) . ? S16 C18 1.807(4) . ? S17 C15 1.743(3) . ? S17 C19 1.794(4) . ? S18 C16 1.743(3) . ? S18 C20 1.805(3) . ? C11 C12 1.356(4) . ? C13 C14 1.338(5) . ? C15 C16 1.337(5) . ? C17 C18 1.508(6) . ? C19 C20 1.495(5) . ? C1S C2S 1.3900 . ? C1S C6S 1.3900 . ? C2S C3S 1.3900 . ? C3S C4S 1.3900 . ? C4S C5S 1.3900 . ? C4S N1S 1.442(14) . ? C5S C6S 1.3900 . ? N1S O1S 1.196(9) . ? N1S O2S 1.200(9) . ? Os1 N2 1.804(13) 2 ? Os1 N2 1.804(13) . ? Os1 N1 1.842(11) 2 ? Os1 N1 1.842(11) . ? Os1 Cl2 2.3770(9) . ? Os1 Cl2 2.3770(9) 2 ? Os1 Cl1 2.3774(9) . ? Os1 Cl1 2.3774(9) 2 ? Os1 Cl3 2.3808(7) . ? Os1 Cl3 2.3808(7) 2 ? N1 O1 1.116(9) . ? N2 O2 1.131(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 S1 C3 95.18(16) . . ? C1 S2 C4 95.12(16) . . ? C2 S3 C5 95.70(16) . . ? C2 S4 C6 95.31(16) . . ? C3 S5 C7 100.78(17) . . ? C4 S6 C8 100.68(18) . . ? C5 S7 C9B 98.8(5) . . ? C5 S7 C9A 104.2(2) . . ? C9B S7 C9A 26.8(5) . . ? C6 S8 C10B 102.5(5) . . ? C6 S8 C10A 99.5(2) . . ? C10B S8 C10A 21.4(6) . . ? C2 C1 S1 121.8(3) . . ? C2 C1 S2 122.5(3) . . ? S1 C1 S2 115.69(17) . . ? C1 C2 S4 123.0(3) . . ? C1 C2 S3 121.7(3) . . ? S4 C2 S3 115.31(17) . . ? C4 C3 S1 117.1(2) . . ? C4 C3 S5 129.2(2) . . ? S1 C3 S5 113.71(19) . . ? C3 C4 S6 128.1(2) . . ? C3 C4 S2 116.9(2) . . ? S6 C4 S2 115.00(19) . . ? C6 C5 S7 128.1(2) . . ? C6 C5 S3 116.6(2) . . ? S7 C5 S3 115.3(2) . . ? C5 C6 S8 127.3(2) . . ? C5 C6 S4 117.1(2) . . ? S8 C6 S4 115.53(19) . . ? C8 C7 S5 114.0(3) . . ? C7 C8 S6 114.3(3) . . ? C10A C9A S7 115.1(4) . . ? C9A C10A S8 112.0(5) . . ? C10B C9B S7 112.2(12) . . ? C9B C10B S8 120.9(13) . . ? C11 S11 C13 95.15(16) . . ? C11 S12 C14 95.06(16) . . ? C12 S13 C15 95.07(16) . . ? C12 S14 C16 95.32(15) . . ? C13 S15 C17 101.22(17) . . ? C14 S16 C18 100.14(18) . . ? C15 S17 C19 101.25(17) . . ? C16 S18 C20 102.14(16) . . ? C12 C11 S11 122.6(3) . . ? C12 C11 S12 122.5(3) . . ? S11 C11 S12 114.90(17) . . ? C11 C12 S14 123.1(3) . . ? C11 C12 S13 122.1(3) . . ? S14 C12 S13 114.85(17) . . ? C14 C13 S15 128.8(3) . . ? C14 C13 S11 117.3(2) . . ? S15 C13 S11 113.9(2) . . ? C13 C14 S16 128.6(3) . . ? C13 C14 S12 117.3(2) . . ? S16 C14 S12 114.0(2) . . ? C16 C15 S17 127.9(3) . . ? C16 C15 S13 117.5(2) . . ? S17 C15 S13 114.6(2) . . ? C15 C16 S18 128.7(2) . . ? C15 C16 S14 117.2(2) . . ? S18 C16 S14 114.07(19) . . ? C18 C17 S15 114.1(3) . . ? C17 C18 S16 113.4(3) . . ? C20 C19 S17 113.8(3) . . ? C19 C20 S18 114.1(2) . . ? C2S C1S C6S 120.0 . . ? C3S C2S C1S 120.0 . . ? C2S C3S C4S 120.0 . . ? C5S C4S C3S 120.0 . . ? C5S C4S N1S 117.8(7) . . ? C3S C4S N1S 122.1(7) . . ? C6S C5S C4S 120.0 . . ? C5S C6S C1S 120.0 . . ? O1S N1S O2S 119.0(15) . . ? O1S N1S C4S 118.8(12) . . ? O2S N1S C4S 122.2(12) . . ? N2 Os1 N2 180.0(14) 2 . ? N2 Os1 N1 95.7(6) 2 2 ? N2 Os1 N1 84.3(6) . 2 ? N2 Os1 N1 84.3(6) 2 . ? N2 Os1 N1 95.7(6) . . ? N1 Os1 N1 180.0(10) 2 . ? N2 Os1 Cl2 174.2(5) 2 . ? N2 Os1 Cl2 5.8(5) . . ? N1 Os1 Cl2 90.1(4) 2 . ? N1 Os1 Cl2 89.9(4) . . ? N2 Os1 Cl2 5.8(5) 2 2 ? N2 Os1 Cl2 174.2(5) . 2 ? N1 Os1 Cl2 89.9(4) 2 2 ? N1 Os1 Cl2 90.1(4) . 2 ? Cl2 Os1 Cl2 180.00(6) . 2 ? N2 Os1 Cl1 88.5(5) 2 . ? N2 Os1 Cl1 91.5(5) . . ? N1 Os1 Cl1 175.8(5) 2 . ? N1 Os1 Cl1 4.2(5) . . ? Cl2 Os1 Cl1 85.77(5) . . ? Cl2 Os1 Cl1 94.23(5) 2 . ? N2 Os1 Cl1 91.5(5) 2 2 ? N2 Os1 Cl1 88.5(5) . 2 ? N1 Os1 Cl1 4.2(5) 2 2 ? N1 Os1 Cl1 175.8(5) . 2 ? Cl2 Os1 Cl1 94.23(5) . 2 ? Cl2 Os1 Cl1 85.77(5) 2 2 ? Cl1 Os1 Cl1 180.00(8) . 2 ? N2 Os1 Cl3 90.5(5) 2 . ? N2 Os1 Cl3 89.5(5) . . ? N1 Os1 Cl3 87.7(4) 2 . ? N1 Os1 Cl3 92.3(4) . . ? Cl2 Os1 Cl3 89.24(4) . . ? Cl2 Os1 Cl3 90.76(4) 2 . ? Cl1 Os1 Cl3 91.85(4) . . ? Cl1 Os1 Cl3 88.15(4) 2 . ? N2 Os1 Cl3 89.5(5) 2 2 ? N2 Os1 Cl3 90.5(5) . 2 ? N1 Os1 Cl3 92.3(4) 2 2 ? N1 Os1 Cl3 87.7(4) . 2 ? Cl2 Os1 Cl3 90.76(4) . 2 ? Cl2 Os1 Cl3 89.24(4) 2 2 ? Cl1 Os1 Cl3 88.15(4) . 2 ? Cl1 Os1 Cl3 91.85(4) 2 2 ? Cl3 Os1 Cl3 180.00(3) . 2 ? O1 N1 Os1 175.6(16) . . ? O2 N2 Os1 170.8(18) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C17 H17A S7 0.97 3.03 3.609(4) 119.5 2_556 C18 H18A O2S 0.97 2.58 3.407(15) 143.6 2_666 C20 H20A Cl3 0.97 2.85 3.627(4) 137.4 . C7 H7B Cl1 0.97 3.04 3.567(4) 115.4 2_556 C7 H7B Cl3 0.97 2.68 3.617(4) 162.1 2_556 C7 H7A S3 0.97 2.87 3.652(5) 138.9 2_556 C8 H8B Cl2 0.97 2.99 3.477(4) 112.2 1_556 C8 H8B Cl1 0.97 2.79 3.571(4) 138.3 2_556 C9B H9D Cl3 0.97 2.70 3.599(16) 154.3 . C10B H10D O2 0.97 2.32 2.90(2) 118.0 2_655 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.030 _refine_diff_density_min -0.866 _refine_diff_density_rms 0.103