Supplementary Material (ESI) for Dalton Transactions This journal is (C) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Shinzi Kato' _publ_contact_author_email KSHINZI@NIFTY.COM loop_ _publ_author_name S.Kato F.Ando M.Ebihara S.Hayashi M.Ishida J.Koketsu ; W.Nakanishi ; J.Nonogaki K.Tani data_tani43 _database_code_depnum_ccdc_archive 'CCDC 709226' #TrackingRef '- comd-(2e).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H14 O2 S4 Se' _chemical_formula_sum 'C16 H14 O2 S4 Se' _chemical_formula_weight 445.47 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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall '-P 2yn' 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 7.779(1) _cell_length_b 12.907(1) _cell_length_c 17.537(1) _cell_angle_alpha 90 _cell_angle_beta 96.942(8) _cell_angle_gamma 90 _cell_volume 1747.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.0 _cell_measurement_theta_max 12.5 _exptl_crystal_description prismatic _exptl_crystal_colour reddish _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.693 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 2.631 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.540 _exptl_absorpt_correction_T_max 0.692 _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.46 _diffrn_reflns_number 4302 _diffrn_reflns_av_R_equivalents 0.0829 _diffrn_reflns_av_sigmaI/netI 0.0882 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4013 _reflns_number_gt 2512 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0216P)^2^+1.3750P] 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 4013 _refine_ls_number_parameters 210 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1021 _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_ref 0.0836 _refine_ls_wR_factor_gt 0.0675 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _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 Se1 Se 0.19137(5) 0.53438(3) 0.43805(2) 0.02655(11) Uani 1 1 d . . . S11 S 0.18145(16) 0.74961(8) 0.47806(6) 0.0379(3) Uani 1 1 d . . . S12 S 0.02138(14) 0.62946(8) 0.34870(6) 0.0289(2) Uani 1 1 d . . . C11 C 0.0471(5) 0.7451(3) 0.3972(2) 0.0221(8) Uani 1 1 d . . . C12 C -0.0557(5) 0.8356(3) 0.3665(2) 0.0223(8) Uani 1 1 d . . . C13 C -0.1169(5) 0.8502(3) 0.2878(2) 0.0213(8) Uani 1 1 d . . . C14 C -0.2112(5) 0.9386(3) 0.2648(2) 0.0267(9) Uani 1 1 d . . . H14 H -0.2505 0.9488 0.2119 0.032 Uiso 1 1 calc R . . C15 C -0.2484(5) 1.0116(3) 0.3176(2) 0.0310(10) Uani 1 1 d . . . H15 H -0.3158 1.0707 0.3012 0.037 Uiso 1 1 calc R . . C16 C -0.1881(5) 0.9991(3) 0.3945(2) 0.0342(11) Uani 1 1 d . . . H16 H -0.2121 1.0501 0.4308 0.041 Uiso 1 1 calc R . . C17 C -0.0929(5) 0.9124(3) 0.4182(2) 0.0274(9) Uani 1 1 d . . . H17 H -0.0515 0.9046 0.4711 0.033 Uiso 1 1 calc R . . O11 O -0.0763(4) 0.7758(2) 0.23832(14) 0.0314(7) Uani 1 1 d . . . C18 C -0.1412(6) 0.7878(3) 0.1591(2) 0.0317(10) Uani 1 1 d . . . H18A H -0.2681 0.7881 0.1534 0.048 Uiso 1 1 calc R . . H18B H -0.1006 0.7301 0.1296 0.048 Uiso 1 1 calc R . . H18C H -0.0994 0.8533 0.1400 0.048 Uiso 1 1 calc R . . S21 S 0.33191(16) 0.34783(9) 0.49697(6) 0.0378(3) Uani 1 1 d . . . S22 S 0.12299(14) 0.40264(7) 0.35558(6) 0.0279(2) Uani 1 1 d . . . C21 C 0.2322(5) 0.3096(3) 0.4128(2) 0.0223(8) Uani 1 1 d . . . C22 C 0.2378(5) 0.2018(3) 0.3845(2) 0.0248(9) Uani 1 1 d . . . C23 C 0.1639(5) 0.1696(3) 0.3106(2) 0.0254(9) Uani 1 1 d . . . C24 C 0.1839(5) 0.0687(3) 0.2865(2) 0.0290(9) Uani 1 1 d . . . H24 H 0.1361 0.0485 0.2362 0.035 Uiso 1 1 calc R . . C25 C 0.2727(5) -0.0031(3) 0.3349(2) 0.0332(10) Uani 1 1 d . . . H25 H 0.2854 -0.0723 0.3179 0.040 Uiso 1 1 calc R . . C26 C 0.3433(6) 0.0262(3) 0.4082(2) 0.0345(10) Uani 1 1 d . . . H26 H 0.4034 -0.0230 0.4417 0.041 Uiso 1 1 calc R . . C27 C 0.3260(5) 0.1264(3) 0.4321(2) 0.0307(10) Uani 1 1 d . . . H27 H 0.3753 0.1455 0.4823 0.037 Uiso 1 1 calc R . . O21 O 0.0749(4) 0.2422(2) 0.26622(16) 0.0370(8) Uani 1 1 d . . . C28 C 0.0030(5) 0.2162(3) 0.1895(2) 0.0324(10) Uani 1 1 d . . . H28A H 0.0951 0.1910 0.1608 0.049 Uiso 1 1 calc R . . H28B H -0.0507 0.2778 0.1641 0.049 Uiso 1 1 calc R . . H28C H -0.0847 0.1620 0.1912 0.049 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 Se1 0.0319(2) 0.0250(2) 0.02098(19) 0.00008(18) -0.00394(16) 0.0012(2) S11 0.0528(8) 0.0293(6) 0.0257(6) -0.0074(5) -0.0187(5) 0.0084(5) S12 0.0368(6) 0.0217(5) 0.0249(5) -0.0045(4) -0.0097(5) 0.0048(4) C11 0.026(2) 0.0219(19) 0.0171(19) -0.0027(15) -0.0005(16) -0.0014(17) C12 0.022(2) 0.025(2) 0.0194(19) -0.0036(16) -0.0027(16) 0.0006(17) C13 0.023(2) 0.0215(19) 0.0186(19) -0.0035(15) -0.0007(16) 0.0014(17) C14 0.027(2) 0.025(2) 0.026(2) 0.0004(16) -0.0055(17) 0.0012(17) C15 0.031(2) 0.026(2) 0.034(2) -0.0015(18) -0.0049(19) 0.0085(18) C16 0.035(3) 0.029(2) 0.037(2) -0.0115(18) -0.003(2) 0.0095(19) C17 0.030(2) 0.030(2) 0.021(2) -0.0034(17) -0.0028(17) 0.0032(19) O11 0.0464(19) 0.0295(15) 0.0157(14) -0.0032(12) -0.0071(13) 0.0113(14) C18 0.040(3) 0.037(2) 0.016(2) -0.0022(18) -0.0032(18) 0.011(2) S21 0.0510(7) 0.0326(6) 0.0251(6) -0.0010(5) -0.0142(5) 0.0057(5) S22 0.0354(6) 0.0211(5) 0.0242(5) 0.0001(4) -0.0086(4) 0.0025(4) C21 0.023(2) 0.024(2) 0.0188(19) 0.0041(15) -0.0030(16) -0.0013(16) C22 0.023(2) 0.021(2) 0.030(2) 0.0020(17) 0.0036(17) -0.0003(17) C23 0.024(2) 0.025(2) 0.026(2) 0.0025(17) -0.0008(17) 0.0006(17) C24 0.027(2) 0.031(2) 0.029(2) -0.0023(18) 0.0049(18) -0.0013(18) C25 0.031(2) 0.023(2) 0.046(3) -0.0010(19) 0.009(2) 0.0005(18) C26 0.044(3) 0.023(2) 0.037(2) 0.0093(19) 0.006(2) 0.007(2) C27 0.032(2) 0.026(2) 0.032(2) 0.0050(18) -0.0014(19) -0.0012(19) O21 0.050(2) 0.0299(16) 0.0270(16) -0.0067(13) -0.0140(14) 0.0131(14) C28 0.034(3) 0.038(2) 0.023(2) -0.0023(19) -0.0044(18) 0.005(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 Se1 S22 2.2539(10) . ? Se1 S12 2.2824(10) . ? S11 C11 1.658(4) . ? S12 C11 1.717(4) . ? C11 C12 1.480(5) . ? C12 C17 1.397(5) . ? C12 C13 1.416(5) . ? C13 O11 1.357(4) . ? C13 C14 1.390(5) . ? C14 C15 1.376(5) . ? C14 H14 0.9500 . ? C15 C16 1.382(5) . ? C15 H15 0.9500 . ? C16 C17 1.379(5) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? O11 C18 1.427(4) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? S21 C21 1.657(4) . ? S22 C21 1.722(4) . ? C21 C22 1.480(5) . ? C22 C27 1.405(5) . ? C22 C23 1.415(5) . ? C23 O21 1.355(4) . ? C23 C24 1.385(5) . ? C24 C25 1.384(5) . ? C24 H24 0.9500 . ? C25 C26 1.388(5) . ? C25 H25 0.9500 . ? C26 C27 1.371(5) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? O21 C28 1.433(4) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? 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 S22 Se1 S12 83.85(4) . . ? C11 S12 Se1 95.98(13) . . ? C12 C11 S11 122.7(3) . . ? C12 C11 S12 118.7(3) . . ? S11 C11 S12 118.5(2) . . ? C17 C12 C13 117.8(3) . . ? C17 C12 C11 117.9(3) . . ? C13 C12 C11 124.2(3) . . ? O11 C13 C14 123.4(3) . . ? O11 C13 C12 116.9(3) . . ? C14 C13 C12 119.7(3) . . ? C15 C14 C13 120.9(4) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C14 C15 C16 120.2(4) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C17 C16 C15 119.7(4) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? C16 C17 C12 121.7(4) . . ? C16 C17 H17 119.1 . . ? C12 C17 H17 119.1 . . ? C13 O11 C18 117.6(3) . . ? O11 C18 H18A 109.5 . . ? O11 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O11 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C21 S22 Se1 95.19(13) . . ? C22 C21 S21 123.3(3) . . ? C22 C21 S22 119.5(3) . . ? S21 C21 S22 117.1(2) . . ? C27 C22 C23 117.1(4) . . ? C27 C22 C21 118.9(3) . . ? C23 C22 C21 123.9(3) . . ? O21 C23 C24 122.9(4) . . ? O21 C23 C22 116.5(3) . . ? C24 C23 C22 120.6(4) . . ? C25 C24 C23 120.6(4) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C24 C25 C26 119.9(4) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? C27 C26 C25 119.8(4) . . ? C27 C26 H26 120.1 . . ? C25 C26 H26 120.1 . . ? C26 C27 C22 122.1(4) . . ? C26 C27 H27 119.0 . . ? C22 C27 H27 119.0 . . ? C23 O21 C28 119.5(3) . . ? O21 C28 H28A 109.5 . . ? O21 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? O21 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S22 Se1 S12 C11 -179.78(14) . . . . ? Se1 S12 C11 C12 -173.6(3) . . . . ? Se1 S12 C11 S11 4.3(3) . . . . ? S11 C11 C12 C17 -24.7(5) . . . . ? S12 C11 C12 C17 153.2(3) . . . . ? S11 C11 C12 C13 154.4(3) . . . . ? S12 C11 C12 C13 -27.7(5) . . . . ? C17 C12 C13 O11 178.7(3) . . . . ? C11 C12 C13 O11 -0.4(6) . . . . ? C17 C12 C13 C14 -0.3(6) . . . . ? C11 C12 C13 C14 -179.4(4) . . . . ? O11 C13 C14 C15 -179.9(4) . . . . ? C12 C13 C14 C15 -1.0(6) . . . . ? C13 C14 C15 C16 1.8(6) . . . . ? C14 C15 C16 C17 -1.1(6) . . . . ? C15 C16 C17 C12 -0.3(7) . . . . ? C13 C12 C17 C16 1.0(6) . . . . ? C11 C12 C17 C16 -179.9(4) . . . . ? C14 C13 O11 C18 -2.9(6) . . . . ? C12 C13 O11 C18 178.2(3) . . . . ? S12 Se1 S22 C21 -177.15(14) . . . . ? Se1 S22 C21 C22 -177.5(3) . . . . ? Se1 S22 C21 S21 0.6(2) . . . . ? S21 C21 C22 C27 2.6(5) . . . . ? S22 C21 C22 C27 -179.5(3) . . . . ? S21 C21 C22 C23 -175.2(3) . . . . ? S22 C21 C22 C23 2.7(5) . . . . ? C27 C22 C23 O21 178.1(4) . . . . ? C21 C22 C23 O21 -4.0(6) . . . . ? C27 C22 C23 C24 -1.9(6) . . . . ? C21 C22 C23 C24 175.9(4) . . . . ? O21 C23 C24 C25 -178.5(4) . . . . ? C22 C23 C24 C25 1.6(6) . . . . ? C23 C24 C25 C26 -0.3(6) . . . . ? C24 C25 C26 C27 -0.6(7) . . . . ? C25 C26 C27 C22 0.2(7) . . . . ? C23 C22 C27 C26 1.0(6) . . . . ? C21 C22 C27 C26 -176.9(4) . . . . ? C24 C23 O21 C28 -2.6(6) . . . . ? C22 C23 O21 C28 177.4(4) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.448 _refine_diff_density_min -0.437 _refine_diff_density_rms 0.104 # Attachment '- compd-(3e).cif' data_tani29 _database_code_depnum_ccdc_archive 'CCDC 709227' #TrackingRef '- compd-(3e).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H14 O2 S4 Te' _chemical_formula_sum 'C16 H14 O2 S4 Te' _chemical_formula_weight 494.11 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' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall '-P 2yn' 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 7.8898(6) _cell_length_b 13.0661(9) _cell_length_c 17.7214(7) _cell_angle_alpha 90.00 _cell_angle_beta 97.790(5) _cell_angle_gamma 90.00 _cell_volume 1810.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.1 _cell_measurement_theta_max 12.3 _exptl_crystal_description prismatic _exptl_crystal_colour deep _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.813 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 968 _exptl_absorpt_coefficient_mu 2.110 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.601 _exptl_absorpt_correction_T_max 0.881 _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.94 _diffrn_reflns_number 4449 _diffrn_reflns_av_R_equivalents 0.0371 _diffrn_reflns_av_sigmaI/netI 0.0570 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4156 _reflns_number_gt 2604 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0174P)^2^+5.2379P] 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 4156 _refine_ls_number_parameters 210 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0912 _refine_ls_R_factor_gt 0.0396 _refine_ls_wR_factor_ref 0.0950 _refine_ls_wR_factor_gt 0.0774 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _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 Te1 Te 0.78399(5) 0.46377(3) 0.04985(2) 0.04569(12) Uani 1 1 d . . . S11 S 0.8106(2) 0.24346(14) 0.02508(9) 0.0641(5) Uani 1 1 d . . . S12 S 0.9813(2) 0.36880(12) 0.14726(9) 0.0539(4) Uani 1 1 d . . . C11 C 0.9519(7) 0.2527(4) 0.1032(3) 0.0382(12) Uani 1 1 d . . . C12 C 1.0554(7) 0.1636(4) 0.1336(3) 0.0400(13) Uani 1 1 d . . . C13 C 1.1176(7) 0.1499(4) 0.2113(3) 0.0398(12) Uani 1 1 d . . . C14 C 1.2138(7) 0.0633(4) 0.2347(3) 0.0482(15) Uani 1 1 d . . . H14 H 1.2532 0.0538 0.2861 0.058 Uiso 1 1 calc R . . C15 C 1.2507(8) -0.0079(5) 0.1826(4) 0.0604(18) Uani 1 1 d . . . H15 H 1.3157 -0.0651 0.1989 0.072 Uiso 1 1 calc R . . C16 C 1.1922(9) 0.0044(5) 0.1062(4) 0.0654(19) Uani 1 1 d . . . H16 H 1.2182 -0.0438 0.0709 0.078 Uiso 1 1 calc R . . C17 C 1.0948(8) 0.0893(5) 0.0829(3) 0.0521(16) Uani 1 1 d . . . H17 H 1.0541 0.0969 0.0314 0.063 Uiso 1 1 calc R . . O11 O 1.0749(6) 0.2220(3) 0.2602(2) 0.0573(12) Uani 1 1 d . . . C18 C 1.1388(9) 0.2117(6) 0.3385(3) 0.0629(19) Uani 1 1 d . . . H18A H 1.0972 0.1491 0.3576 0.094 Uiso 1 1 calc R . . H18B H 1.1010 0.2685 0.3662 0.094 Uiso 1 1 calc R . . H18C H 1.2616 0.2105 0.3446 0.094 Uiso 1 1 calc R . . S21 S 0.6564(2) 0.66164(14) 0.00478(9) 0.0643(5) Uani 1 1 d . . . S22 S 0.8781(2) 0.60211(12) 0.14010(8) 0.0511(4) Uani 1 1 d . . . C21 C 0.7676(7) 0.6966(5) 0.0882(3) 0.0448(14) Uani 1 1 d . . . C22 C 0.7643(7) 0.8019(4) 0.1167(3) 0.0417(13) Uani 1 1 d . . . C23 C 0.8376(7) 0.8331(5) 0.1899(3) 0.0429(13) Uani 1 1 d . . . C24 C 0.8186(8) 0.9320(5) 0.2145(4) 0.0525(15) Uani 1 1 d . . . H24 H 0.8668 0.9509 0.2633 0.063 Uiso 1 1 calc R . . C25 C 0.7300(8) 1.0021(5) 0.1680(4) 0.0622(18) Uani 1 1 d . . . H25 H 0.7173 1.0684 0.1855 0.075 Uiso 1 1 calc R . . C26 C 0.6586(9) 0.9758(5) 0.0950(4) 0.0649(18) Uani 1 1 d . . . H26 H 0.6007 1.0244 0.0629 0.078 Uiso 1 1 calc R . . C27 C 0.6744(8) 0.8769(5) 0.0705(4) 0.0542(16) Uani 1 1 d . . . H27 H 0.6241 0.8590 0.0218 0.065 Uiso 1 1 calc R . . O21 O 0.9285(6) 0.7605(3) 0.2338(2) 0.0620(12) Uani 1 1 d . . . C28 C 0.9990(8) 0.7837(5) 0.3098(3) 0.0599(18) Uani 1 1 d . . . H28A H 1.0865 0.8346 0.3095 0.090 Uiso 1 1 calc R . . H28B H 1.0475 0.7228 0.3343 0.090 Uiso 1 1 calc R . . H28C H 0.9106 0.8092 0.3370 0.090 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 Te1 0.0508(2) 0.0488(2) 0.03480(18) -0.00054(19) -0.00390(14) -0.0024(2) S11 0.0834(12) 0.0522(10) 0.0467(9) -0.0108(7) -0.0270(8) 0.0069(9) S12 0.0626(10) 0.0460(9) 0.0462(8) -0.0093(7) -0.0180(7) 0.0055(7) C11 0.039(3) 0.037(3) 0.037(3) -0.003(2) -0.002(2) 0.000(2) C12 0.040(3) 0.043(3) 0.036(3) -0.007(2) 0.001(2) -0.001(2) C13 0.041(3) 0.043(3) 0.034(3) -0.004(2) 0.002(2) 0.001(3) C14 0.052(3) 0.048(4) 0.042(3) 0.005(3) -0.006(3) 0.006(3) C15 0.058(4) 0.053(4) 0.066(4) -0.006(3) -0.006(3) 0.009(3) C16 0.075(5) 0.059(4) 0.058(4) -0.018(3) -0.003(3) 0.017(4) C17 0.056(4) 0.058(4) 0.039(3) -0.008(3) -0.003(3) 0.008(3) O11 0.078(3) 0.057(3) 0.034(2) -0.005(2) -0.002(2) 0.020(2) C18 0.074(4) 0.085(5) 0.027(3) -0.005(3) -0.003(3) 0.017(4) S21 0.0832(12) 0.0571(11) 0.0438(9) 0.0015(8) -0.0238(8) 0.0065(9) S22 0.0597(9) 0.0425(8) 0.0445(8) -0.0010(7) -0.0169(7) 0.0024(7) C21 0.040(3) 0.054(4) 0.038(3) 0.002(3) -0.001(2) -0.003(3) C22 0.040(3) 0.040(3) 0.044(3) 0.006(3) 0.003(2) 0.000(3) C23 0.040(3) 0.045(3) 0.044(3) -0.002(3) 0.003(2) 0.002(3) C24 0.052(4) 0.052(4) 0.053(4) -0.007(3) 0.008(3) -0.005(3) C25 0.063(4) 0.048(4) 0.077(5) 0.001(4) 0.012(4) 0.006(3) C26 0.068(4) 0.053(4) 0.071(5) 0.018(4) 0.002(4) 0.004(4) C27 0.056(4) 0.050(4) 0.054(4) 0.011(3) -0.001(3) -0.002(3) O21 0.078(3) 0.052(3) 0.049(2) -0.012(2) -0.021(2) 0.013(2) C28 0.065(4) 0.068(5) 0.044(3) -0.010(3) -0.006(3) 0.011(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 Te1 S22 2.4606(15) . ? Te1 S12 2.4931(15) . ? Te1 S21 2.8492(18) . ? S11 C11 1.660(5) . ? S12 C11 1.708(5) . ? C11 C12 1.481(7) . ? C12 C17 1.387(7) . ? C12 C13 1.408(7) . ? C13 O11 1.354(6) . ? C13 C14 1.394(7) . ? C14 C15 1.369(8) . ? C14 H14 0.9300 . ? C15 C16 1.380(8) . ? C15 H15 0.9300 . ? C16 C17 1.381(8) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? O11 C18 1.416(6) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? S21 C21 1.677(5) . ? S22 C21 1.707(6) . ? C21 C22 1.467(8) . ? C22 C27 1.405(8) . ? C22 C23 1.407(7) . ? C23 O21 1.367(6) . ? C23 C24 1.378(8) . ? C24 C25 1.361(8) . ? C24 H24 0.9300 . ? C25 C26 1.382(9) . ? C25 H25 0.9300 . ? C26 C27 1.376(9) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? O21 C28 1.418(6) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? 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 S22 Te1 S12 79.07(5) . . ? S22 Te1 S21 65.15(5) . . ? S12 Te1 S21 144.06(5) . . ? C11 S12 Te1 95.30(18) . . ? C12 C11 S11 121.4(4) . . ? C12 C11 S12 119.9(4) . . ? S11 C11 S12 118.7(3) . . ? C17 C12 C13 117.8(5) . . ? C17 C12 C11 118.4(5) . . ? C13 C12 C11 123.9(5) . . ? O11 C13 C14 123.1(5) . . ? O11 C13 C12 117.0(5) . . ? C14 C13 C12 119.9(5) . . ? C15 C14 C13 120.4(5) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C16 120.6(6) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C15 C16 C17 119.1(6) . . ? C15 C16 H16 120.5 . . ? C17 C16 H16 120.5 . . ? C16 C17 C12 122.2(5) . . ? C16 C17 H17 118.9 . . ? C12 C17 H17 118.9 . . ? C13 O11 C18 118.3(5) . . ? O11 C18 H18A 109.5 . . ? O11 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O11 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C21 S21 Te1 82.9(2) . . ? C21 S22 Te1 95.4(2) . . ? C22 C21 S21 121.8(4) . . ? C22 C21 S22 121.7(4) . . ? S21 C21 S22 116.5(4) . . ? C27 C22 C23 116.6(5) . . ? C27 C22 C21 119.0(5) . . ? C23 C22 C21 124.3(5) . . ? O21 C23 C24 122.8(5) . . ? O21 C23 C22 116.3(5) . . ? C24 C23 C22 120.9(5) . . ? C25 C24 C23 120.6(6) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C24 C25 C26 120.7(6) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C27 C26 C25 119.1(6) . . ? C27 C26 H26 120.4 . . ? C25 C26 H26 120.4 . . ? C26 C27 C22 122.1(6) . . ? C26 C27 H27 119.0 . . ? C22 C27 H27 119.0 . . ? C23 O21 C28 120.0(5) . . ? O21 C28 H28A 109.5 . . ? O21 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? O21 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S22 Te1 S12 C11 179.4(2) . . . . ? S21 Te1 S12 C11 -175.12(19) . . . . ? Te1 S12 C11 C12 174.2(4) . . . . ? Te1 S12 C11 S11 -3.9(3) . . . . ? S11 C11 C12 C17 29.2(7) . . . . ? S12 C11 C12 C17 -148.9(5) . . . . ? S11 C11 C12 C13 -151.2(5) . . . . ? S12 C11 C12 C13 30.8(8) . . . . ? C17 C12 C13 O11 -178.6(5) . . . . ? C11 C12 C13 O11 1.8(8) . . . . ? C17 C12 C13 C14 -0.6(8) . . . . ? C11 C12 C13 C14 179.8(5) . . . . ? O11 C13 C14 C15 179.0(6) . . . . ? C12 C13 C14 C15 1.1(9) . . . . ? C13 C14 C15 C16 -0.5(10) . . . . ? C14 C15 C16 C17 -0.5(11) . . . . ? C15 C16 C17 C12 0.9(11) . . . . ? C13 C12 C17 C16 -0.4(9) . . . . ? C11 C12 C17 C16 179.2(6) . . . . ? C14 C13 O11 C18 3.5(8) . . . . ? C12 C13 O11 C18 -178.5(5) . . . . ? S22 Te1 S21 C21 -0.9(2) . . . . ? S12 Te1 S21 C21 -6.8(2) . . . . ? S12 Te1 S22 C21 177.4(2) . . . . ? S21 Te1 S22 C21 0.9(2) . . . . ? Te1 S21 C21 C22 -176.1(5) . . . . ? Te1 S21 C21 S22 1.3(3) . . . . ? Te1 S22 C21 C22 175.9(4) . . . . ? Te1 S22 C21 S21 -1.5(3) . . . . ? S21 C21 C22 C27 -4.3(8) . . . . ? S22 C21 C22 C27 178.5(4) . . . . ? S21 C21 C22 C23 172.0(5) . . . . ? S22 C21 C22 C23 -5.3(8) . . . . ? C27 C22 C23 O21 -178.4(5) . . . . ? C21 C22 C23 O21 5.3(8) . . . . ? C27 C22 C23 C24 1.0(8) . . . . ? C21 C22 C23 C24 -175.3(5) . . . . ? O21 C23 C24 C25 178.6(6) . . . . ? C22 C23 C24 C25 -0.8(9) . . . . ? C23 C24 C25 C26 -0.6(10) . . . . ? C24 C25 C26 C27 1.7(10) . . . . ? C25 C26 C27 C22 -1.5(10) . . . . ? C23 C22 C27 C26 0.1(9) . . . . ? C21 C22 C27 C26 176.6(6) . . . . ? C24 C23 O21 C28 4.0(9) . . . . ? C22 C23 O21 C28 -176.6(5) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.905 _refine_diff_density_min -1.266 _refine_diff_density_rms 0.115 # Attachment '- compd-(3g).cif' data_nonogaki1 _database_code_depnum_ccdc_archive 'CCDC 709228' #TrackingRef '- compd-(3g).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H14 S4 Te' _chemical_formula_sum 'C16 H14 S4 Te' _chemical_formula_weight 462.11 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.696(5) _cell_length_b 18.810(10) _cell_length_c 12.268(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.51(4) _cell_angle_gamma 90.00 _cell_volume 1751.5(16) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11.3 _cell_measurement_theta_max 14.2 _exptl_crystal_description prismatic _exptl_crystal_colour red _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.752 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 2.165 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.731 _exptl_absorpt_correction_T_max 0.820 _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.23 _diffrn_reflns_number 4057 _diffrn_reflns_av_R_equivalents 0.0911 _diffrn_reflns_av_sigmaI/netI 0.2623 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 27.49 _reflns_number_total 3768 _reflns_number_gt 1227 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0185P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3768 _refine_ls_number_parameters 192 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2550 _refine_ls_R_factor_gt 0.0558 _refine_ls_wR_factor_ref 0.1351 _refine_ls_wR_factor_gt 0.0908 _refine_ls_goodness_of_fit_ref 0.932 _refine_ls_restrained_S_all 0.932 _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 Te1 Te 0.69998(11) 0.11976(5) 0.10566(6) 0.0576(3) Uani 1 1 d . . . S11 S 0.6505(5) 0.25750(17) 0.0013(2) 0.0690(10) Uani 1 1 d . . . S12 S 0.7779(5) 0.22257(17) 0.2306(2) 0.0652(10) Uani 1 1 d . . . C11 C 0.7203(16) 0.2846(6) 0.1324(9) 0.061(4) Uani 1 1 d . . . C12 C 0.7282(15) 0.3595(6) 0.1635(10) 0.051(3) Uani 1 1 d . . . C13 C 0.6728(15) 0.4140(7) 0.0865(9) 0.065(4) Uani 1 1 d . . . H13 H 0.6318 0.4031 0.0128 0.078 Uiso 1 1 calc R . . C14 C 0.6801(18) 0.4838(6) 0.1222(11) 0.077(4) Uani 1 1 d . . . H14 H 0.6388 0.5189 0.0710 0.093 Uiso 1 1 calc R . . C15 C 0.7442(17) 0.5044(7) 0.2275(12) 0.068(4) Uani 1 1 d . . . C16 C 0.7967(17) 0.4504(7) 0.3004(10) 0.068(4) Uani 1 1 d . . . H16 H 0.8366 0.4620 0.3739 0.081 Uiso 1 1 calc R . . C17 C 0.7938(15) 0.3805(7) 0.2711(9) 0.068(3) Uani 1 1 d . . . H17 H 0.8361 0.3464 0.3237 0.081 Uiso 1 1 calc R . . C18 C 0.7450(18) 0.5806(6) 0.2590(11) 0.091(5) Uani 1 1 d . . . H18A H 0.6861 0.5863 0.3216 0.137 Uiso 1 1 calc R . . H18B H 0.6851 0.6079 0.1981 0.137 Uiso 1 1 calc R . . H18C H 0.8645 0.5969 0.2777 0.137 Uiso 1 1 calc R . . S21 S 0.6740(5) -0.03151(17) 0.0891(3) 0.0774(11) Uani 1 1 d . . . S22 S 0.7776(4) 0.05535(17) 0.2840(2) 0.0605(9) Uani 1 1 d . . . C21 C 0.7415(13) -0.0257(5) 0.2240(8) 0.045(3) Uani 1 1 d . . . C22 C 0.7645(14) -0.0897(6) 0.2960(9) 0.047(3) Uani 1 1 d . . . C23 C 0.6922(15) -0.1556(6) 0.2602(9) 0.053(3) Uani 1 1 d . . . H23 H 0.6235 -0.1595 0.1906 0.064 Uiso 1 1 calc R . . C24 C 0.7219(16) -0.2145(6) 0.3267(10) 0.065(4) Uani 1 1 d . . . H24 H 0.6782 -0.2582 0.2996 0.078 Uiso 1 1 calc R . . C25 C 0.8154(16) -0.2103(7) 0.4335(10) 0.065(4) Uani 1 1 d . . . C26 C 0.8855(17) -0.1460(6) 0.4673(9) 0.068(4) Uani 1 1 d . . . H26 H 0.9551 -0.1427 0.5368 0.081 Uiso 1 1 calc R . . C27 C 0.8580(15) -0.0859(7) 0.4034(10) 0.066(4) Uani 1 1 d . . . H27 H 0.9018 -0.0424 0.4318 0.079 Uiso 1 1 calc R . . C28 C 0.8465(16) -0.2766(6) 0.5036(9) 0.078(4) Uani 1 1 d . . . H28A H 0.9458 -0.3020 0.4851 0.117 Uiso 1 1 calc R . . H28B H 0.7438 -0.3063 0.4900 0.117 Uiso 1 1 calc R . . H28C H 0.8696 -0.2635 0.5803 0.117 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 Te1 0.0654(5) 0.0604(5) 0.0468(4) -0.0008(5) 0.0081(3) 0.0012(6) S11 0.099(3) 0.069(2) 0.0393(18) -0.0022(17) 0.0126(19) 0.005(2) S12 0.091(3) 0.057(2) 0.0452(19) 0.0063(17) 0.0023(18) -0.004(2) C11 0.070(9) 0.063(9) 0.060(9) -0.001(7) 0.042(7) -0.004(8) C12 0.055(8) 0.047(8) 0.058(8) 0.008(6) 0.027(7) 0.009(6) C13 0.069(10) 0.076(10) 0.051(8) -0.006(7) 0.009(7) 0.004(8) C14 0.104(12) 0.034(8) 0.087(11) 0.003(8) -0.003(9) 0.010(8) C15 0.057(9) 0.061(10) 0.087(11) -0.006(9) 0.013(8) -0.010(8) C16 0.097(11) 0.058(9) 0.050(8) -0.014(8) 0.020(7) -0.013(9) C17 0.084(9) 0.066(9) 0.050(8) 0.004(8) 0.003(7) -0.006(9) C18 0.101(12) 0.072(11) 0.113(12) -0.017(9) 0.051(10) -0.010(9) S21 0.117(3) 0.063(2) 0.047(2) -0.0036(17) -0.004(2) 0.000(2) S22 0.076(2) 0.053(2) 0.0508(19) -0.0030(16) 0.0060(17) -0.0089(19) C21 0.042(7) 0.043(7) 0.049(7) -0.008(6) 0.004(6) 0.007(6) C22 0.039(7) 0.057(8) 0.045(7) -0.001(6) 0.006(6) -0.002(6) C23 0.056(9) 0.054(8) 0.045(7) -0.016(7) -0.007(6) 0.012(7) C24 0.082(10) 0.052(9) 0.062(9) 0.000(7) 0.013(8) -0.003(8) C25 0.057(9) 0.074(10) 0.067(9) 0.009(8) 0.016(7) -0.011(8) C26 0.086(11) 0.056(9) 0.052(8) 0.010(7) -0.014(7) -0.011(8) C27 0.076(10) 0.058(9) 0.061(8) -0.014(7) 0.007(8) -0.008(7) C28 0.091(11) 0.056(9) 0.088(10) 0.015(8) 0.016(8) 0.006(8) _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 Te1 S12 2.479(3) . ? Te1 S22 2.486(3) . ? Te1 S21 2.857(4) . ? Te1 S11 2.887(3) . ? S11 C11 1.688(11) . ? S12 C11 1.683(11) . ? C11 C12 1.459(14) . ? C12 C17 1.391(14) . ? C12 C13 1.411(14) . ? C13 C14 1.382(15) . ? C13 H13 0.9300 . ? C14 C15 1.361(15) . ? C14 H14 0.9300 . ? C15 C16 1.370(15) . ? C15 C18 1.485(15) . ? C16 C17 1.362(15) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? S21 C21 1.654(10) . ? S22 C21 1.696(10) . ? C21 C22 1.486(13) . ? C22 C27 1.395(14) . ? C22 C23 1.399(13) . ? C23 C24 1.373(14) . ? C23 H23 0.9300 . ? C24 C25 1.389(15) . ? C24 H24 0.9300 . ? C25 C26 1.361(15) . ? C25 C28 1.511(14) . ? C26 C27 1.373(14) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? 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 S12 Te1 S22 80.65(11) . . ? S12 Te1 S21 145.86(10) . . ? S22 Te1 S21 65.22(10) . . ? S12 Te1 S11 64.84(10) . . ? S22 Te1 S11 145.35(10) . . ? S21 Te1 S11 149.27(9) . . ? C11 S11 Te1 81.4(4) . . ? C11 S12 Te1 95.2(4) . . ? C12 C11 S12 119.2(9) . . ? C12 C11 S11 122.3(9) . . ? S12 C11 S11 118.5(7) . . ? C17 C12 C13 116.8(11) . . ? C17 C12 C11 121.0(11) . . ? C13 C12 C11 122.2(12) . . ? C14 C13 C12 119.1(12) . . ? C14 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? C15 C14 C13 124.1(12) . . ? C15 C14 H14 118.0 . . ? C13 C14 H14 118.0 . . ? C14 C15 C16 115.4(12) . . ? C14 C15 C18 120.5(13) . . ? C16 C15 C18 124.0(13) . . ? C17 C16 C15 123.6(12) . . ? C17 C16 H16 118.2 . . ? C15 C16 H16 118.2 . . ? C16 C17 C12 120.8(12) . . ? C16 C17 H17 119.6 . . ? C12 C17 H17 119.6 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C21 S21 Te1 81.8(4) . . ? C21 S22 Te1 93.3(4) . . ? C22 C21 S21 121.9(8) . . ? C22 C21 S22 118.4(8) . . ? S21 C21 S22 119.7(6) . . ? C27 C22 C23 117.3(10) . . ? C27 C22 C21 120.8(11) . . ? C23 C22 C21 121.9(10) . . ? C24 C23 C22 120.6(10) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C23 C24 C25 121.7(12) . . ? C23 C24 H24 119.2 . . ? C25 C24 H24 119.2 . . ? C26 C25 C24 117.1(12) . . ? C26 C25 C28 122.8(12) . . ? C24 C25 C28 120.0(13) . . ? C25 C26 C27 122.8(11) . . ? C25 C26 H26 118.6 . . ? C27 C26 H26 118.6 . . ? C26 C27 C22 120.3(11) . . ? C26 C27 H27 119.9 . . ? C22 C27 H27 119.9 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S12 Te1 S11 C11 -1.6(4) . . . . ? S22 Te1 S11 C11 4.1(5) . . . . ? S21 Te1 S11 C11 176.6(4) . . . . ? S22 Te1 S12 C11 -175.1(4) . . . . ? S21 Te1 S12 C11 -176.7(4) . . . . ? S11 Te1 S12 C11 1.6(4) . . . . ? Te1 S12 C11 C12 175.7(9) . . . . ? Te1 S12 C11 S11 -2.9(7) . . . . ? Te1 S11 C11 C12 -176.0(10) . . . . ? Te1 S11 C11 S12 2.5(6) . . . . ? S12 C11 C12 C17 4.5(16) . . . . ? S11 C11 C12 C17 -177.1(9) . . . . ? S12 C11 C12 C13 -176.5(9) . . . . ? S11 C11 C12 C13 2.0(17) . . . . ? C17 C12 C13 C14 -2.3(18) . . . . ? C11 C12 C13 C14 178.6(11) . . . . ? C12 C13 C14 C15 2(2) . . . . ? C13 C14 C15 C16 -3(2) . . . . ? C13 C14 C15 C18 -179.2(13) . . . . ? C14 C15 C16 C17 3(2) . . . . ? C18 C15 C16 C17 179.3(13) . . . . ? C15 C16 C17 C12 -3(2) . . . . ? C13 C12 C17 C16 2.6(18) . . . . ? C11 C12 C17 C16 -178.3(12) . . . . ? S12 Te1 S21 C21 1.2(5) . . . . ? S22 Te1 S21 C21 -0.6(4) . . . . ? S11 Te1 S21 C21 -175.9(4) . . . . ? S12 Te1 S22 C21 -178.4(4) . . . . ? S21 Te1 S22 C21 0.6(4) . . . . ? S11 Te1 S22 C21 176.3(4) . . . . ? Te1 S21 C21 C22 178.2(9) . . . . ? Te1 S21 C21 S22 0.9(6) . . . . ? Te1 S22 C21 C22 -178.4(8) . . . . ? Te1 S22 C21 S21 -1.0(7) . . . . ? S21 C21 C22 C27 165.3(9) . . . . ? S22 C21 C22 C27 -17.3(14) . . . . ? S21 C21 C22 C23 -15.5(15) . . . . ? S22 C21 C22 C23 161.8(9) . . . . ? C27 C22 C23 C24 -3.6(18) . . . . ? C21 C22 C23 C24 177.2(10) . . . . ? C22 C23 C24 C25 3.6(19) . . . . ? C23 C24 C25 C26 -3.7(19) . . . . ? C23 C24 C25 C28 -179.5(11) . . . . ? C24 C25 C26 C27 4(2) . . . . ? C28 C25 C26 C27 179.7(12) . . . . ? C25 C26 C27 C22 -4(2) . . . . ? C23 C22 C27 C26 3.9(18) . . . . ? C21 C22 C27 C26 -176.9(11) . . . . ? _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.941 _refine_diff_density_max 0.497 _refine_diff_density_min -0.702 _refine_diff_density_rms 0.130