Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Konrad Seppelt' _publ_contact_author_email SEPPELT@CHEMIE.FU-BERLIN.DE loop_ _publ_author_name K.Seppelt B.Mueller H.Poleschner # Attachment 'IBUT4TE4.CIF' data_ibut4te4 _database_code_depnum_ccdc_archive 'CCDC 670385' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; 1,2,3,4-Tetra(2-methylpropyl)-tetratelluretanediylium-bis- (trifluormethanesulfonate) ; _chemical_melting_point ? _chemical_formula_moiety (C4H9Te)4,(CF3SO3)2 _chemical_formula_sum 'C18 H36 F6 O6 S2 Te4' _chemical_formula_weight 1036.99 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' F F 0.0171 0.0103 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.904(4) _cell_length_b 9.750(5) _cell_length_c 10.916(5) _cell_angle_alpha 85.046(10) _cell_angle_beta 88.275(12) _cell_angle_gamma 68.728(9) _cell_volume 781.0(6) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 999 _cell_measurement_theta_min 2. _cell_measurement_theta_max 25. _exptl_crystal_description irregular _exptl_crystal_colour dark_red _exptl_crystal_size_max 0.0 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.205 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 486 _exptl_absorpt_coefficient_mu 3.897 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.862 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details Bruker_2000_NT_Software_Reference_Manual _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Bruker_CCD _diffrn_measurement_method omega_scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 6266 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0576 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 25.08 _reflns_number_total 6266 _reflns_number_gt 5217 _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^)+(0.0372P)^2^+32.6481P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0023(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6266 _refine_ls_number_parameters 169 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0743 _refine_ls_R_factor_gt 0.0626 _refine_ls_wR_factor_ref 0.1887 _refine_ls_wR_factor_gt 0.1804 _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 Te1 Te 0.56501(10) 0.69154(8) 0.99070(7) 0.0227(2) Uani 1 1 d . . . Te2 Te 0.27310(10) 0.64913(8) 1.08553(7) 0.0231(2) Uani 1 1 d . . . C4 C 0.2146(19) 1.0310(14) 0.8959(14) 0.043(4) Uani 1 1 d . . . H4A H 0.1628 1.1383 0.8780 0.065 Uiso 1 1 calc R . . H4B H 0.2583 1.0079 0.9811 0.065 Uiso 1 1 calc R . . H4C H 0.1214 0.9889 0.8846 0.065 Uiso 1 1 calc R . . C7 C 0.4098(17) 0.7376(12) 1.3224(11) 0.028(3) Uani 1 1 d . . . H7 H 0.5068 0.7569 1.2708 0.034 Uiso 1 1 calc R . . C6 C 0.3706(16) 0.6097(12) 1.2721(10) 0.021(2) Uani 1 1 d . . . H6A H 0.2794 0.5870 1.3259 0.026 Uiso 1 1 calc R . . H6B H 0.4835 0.5211 1.2775 0.026 Uiso 1 1 calc R . . C3 C 0.3725(17) 0.9653(13) 0.8090(12) 0.032(3) Uani 1 1 d . . . H3 H 0.4737 0.9972 0.8310 0.038 Uiso 1 1 calc R . . C2 C 0.4447(17) 0.7964(12) 0.8169(10) 0.025(3) Uani 1 1 d . . . H2A H 0.5364 0.7625 0.7515 0.030 Uiso 1 1 calc R . . H2B H 0.3433 0.7637 0.8003 0.030 Uiso 1 1 calc R . . C5 C 0.319(2) 1.0212(14) 0.6775(12) 0.037(3) Uani 1 1 d . . . H5A H 0.2244 0.9867 0.6525 0.056 Uiso 1 1 calc R . . H5B H 0.4254 0.9840 0.6243 0.056 Uiso 1 1 calc R . . H5C H 0.2729 1.1295 0.6702 0.056 Uiso 1 1 calc R . . C9 C 0.479(2) 0.6920(14) 1.4523(12) 0.038(3) Uani 1 1 d . . . H9A H 0.3836 0.6773 1.5048 0.057 Uiso 1 1 calc R . . H9B H 0.5147 0.7694 1.4828 0.057 Uiso 1 1 calc R . . H9C H 0.5849 0.5997 1.4538 0.057 Uiso 1 1 calc R . . C8 C 0.243(2) 0.8789(14) 1.3191(13) 0.045(4) Uani 1 1 d . . . H8A H 0.1411 0.8580 1.3584 0.067 Uiso 1 1 calc R . . H8B H 0.2120 0.9173 1.2335 0.067 Uiso 1 1 calc R . . H8C H 0.2691 0.9524 1.3633 0.067 Uiso 1 1 calc R . . S3 S 0.0272(4) 0.5921(4) 0.7876(3) 0.0317(7) Uani 1 1 d . . . O1 O 0.2133(12) 0.5679(10) 0.8100(8) 0.036(2) Uani 1 1 d . . . O2 O -0.0133(14) 0.4606(11) 0.7780(9) 0.047(3) Uani 1 1 d . . . O3 O -0.0994(15) 0.6990(14) 0.8587(9) 0.061(3) Uani 1 1 d . . . F3 F 0.0892(12) 0.5929(9) 0.5520(7) 0.050(2) Uani 1 1 d . . . F2 F 0.0358(12) 0.7995(8) 0.6234(8) 0.054(2) Uani 1 1 d . . . F1 F -0.1806(12) 0.7215(12) 0.5999(8) 0.066(3) Uani 1 1 d . . . C1 C -0.0072(19) 0.6791(15) 0.6331(13) 0.039(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Te1 0.0194(5) 0.0231(4) 0.0278(4) -0.0026(3) 0.0011(3) -0.0104(3) Te2 0.0175(5) 0.0264(4) 0.0257(4) -0.0041(3) 0.0022(3) -0.0079(3) C4 0.034(8) 0.031(7) 0.075(10) 0.000(7) -0.004(8) -0.024(6) C7 0.028(7) 0.026(6) 0.031(6) -0.006(5) 0.003(5) -0.010(5) C6 0.019(6) 0.023(5) 0.028(6) -0.003(5) 0.000(5) -0.013(5) C3 0.014(7) 0.036(7) 0.052(8) -0.005(6) 0.000(6) -0.016(5) C2 0.030(7) 0.025(6) 0.026(6) -0.003(5) -0.004(5) -0.018(5) C5 0.045(9) 0.032(7) 0.041(8) 0.001(6) -0.003(6) -0.021(6) C9 0.045(9) 0.030(7) 0.038(7) -0.005(5) -0.003(6) -0.012(6) C8 0.047(10) 0.031(7) 0.048(8) -0.020(6) -0.015(7) 0.001(6) S3 0.0237(18) 0.0484(19) 0.0303(16) -0.0009(14) 0.0011(13) -0.0225(15) O1 0.020(5) 0.046(5) 0.041(5) 0.003(4) -0.006(4) -0.011(4) O2 0.056(7) 0.057(6) 0.053(6) 0.006(5) 0.003(5) -0.052(6) O3 0.049(7) 0.092(9) 0.041(6) -0.013(6) 0.013(5) -0.024(6) F3 0.053(6) 0.062(5) 0.037(4) -0.018(4) 0.013(4) -0.019(4) F2 0.060(6) 0.033(4) 0.062(5) 0.008(4) 0.002(5) -0.013(4) F1 0.028(5) 0.111(8) 0.046(5) 0.011(5) -0.013(4) -0.012(5) C1 0.026(8) 0.041(7) 0.051(8) -0.011(6) 0.006(6) -0.012(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 Te1 C2 2.149(11) . ? Te1 Te2 2.6535(15) . ? Te2 C6 2.153(11) . ? C4 C3 1.524(19) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C7 C9 1.507(17) . ? C7 C8 1.520(17) . ? C7 C6 1.536(15) . ? C7 H7 1.0000 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C3 C5 1.506(18) . ? C3 C2 1.530(15) . ? C3 H3 1.0000 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? S3 O3 1.423(11) . ? S3 O1 1.428(9) . ? S3 O2 1.443(9) . ? S3 C1 1.803(15) . ? F3 C1 1.302(15) . ? F2 C1 1.330(15) . ? F1 C1 1.332(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Te1 Te2 96.5(3) . . ? C6 Te2 Te1 94.7(3) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C9 C7 C8 110.1(11) . . ? C9 C7 C6 108.8(9) . . ? C8 C7 C6 112.4(11) . . ? C9 C7 H7 108.5 . . ? C8 C7 H7 108.5 . . ? C6 C7 H7 108.5 . . ? C7 C6 Te2 115.3(7) . . ? C7 C6 H6A 108.4 . . ? Te2 C6 H6A 108.4 . . ? C7 C6 H6B 108.4 . . ? Te2 C6 H6B 108.4 . . ? H6A C6 H6B 107.5 . . ? C5 C3 C4 111.1(11) . . ? C5 C3 C2 108.1(10) . . ? C4 C3 C2 113.3(10) . . ? C5 C3 H3 108.1 . . ? C4 C3 H3 108.1 . . ? C2 C3 H3 108.1 . . ? C3 C2 Te1 114.6(8) . . ? C3 C2 H2A 108.6 . . ? Te1 C2 H2A 108.6 . . ? C3 C2 H2B 108.6 . . ? Te1 C2 H2B 108.6 . . ? H2A C2 H2B 107.6 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O3 S3 O1 114.8(6) . . ? O3 S3 O2 114.5(7) . . ? O1 S3 O2 115.4(6) . . ? O3 S3 C1 103.9(6) . . ? O1 S3 C1 102.6(6) . . ? O2 S3 C1 103.3(6) . . ? F3 C1 F2 107.0(11) . . ? F3 C1 F1 107.3(12) . . ? F2 C1 F1 106.9(12) . . ? F3 C1 S3 113.0(10) . . ? F2 C1 S3 111.4(10) . . ? F1 C1 S3 110.9(9) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 25.08 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 3.294 _refine_diff_density_min -3.185 _refine_diff_density_rms 0.366 data_et4te4 _database_code_depnum_ccdc_archive 'CCDC 670386' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ;1,2,3,4-Tetraethyl-tetratelluretanediylium-bis- (trifluormethanesulfonate) ; _chemical_melting_point ? _chemical_formula_moiety (C2H5Te)4,(CF3SO3)2 _chemical_formula_sum 'C10 H20 F6 O6 S2 Te4' _chemical_formula_weight 924.78 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.411(2) _cell_length_b 7.6856(17) _cell_length_c 15.241(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.854(5) _cell_angle_gamma 90.00 _cell_volume 1184.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 999 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 30.0 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.594 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 844 _exptl_absorpt_coefficient_mu 5.124 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.725 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details Bruker_2000_NT_Software_Reference_Manual _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Bruker_CCD _diffrn_measurement_method omega_scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 17112 _diffrn_reflns_av_R_equivalents 0.0591 _diffrn_reflns_av_sigmaI/netI 0.0473 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 29.13 _reflns_number_total 3180 _reflns_number_gt 2099 _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^)+(0.0410P)^2^+2.2899P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3180 _refine_ls_number_parameters 130 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0736 _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_ref 0.0924 _refine_ls_wR_factor_gt 0.0794 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 C1 C 0.7092(6) 0.5833(9) 0.1950(5) 0.0342(16) Uani 1 1 d . . . H1A H 0.7585 0.5305 0.1555 0.057(8) Uiso 1 1 calc R . . H1B H 0.7574 0.6859 0.2217 0.057(8) Uiso 1 1 calc R . . C2 C 0.7029(7) 0.4575(9) 0.2687(5) 0.0367(16) Uani 1 1 d . . . H2A H 0.6388 0.4970 0.3003 0.057(8) Uiso 1 1 calc R . . H2B H 0.7881 0.4499 0.3102 0.057(8) Uiso 1 1 calc R . . H2C H 0.6776 0.3450 0.2431 0.057(8) Uiso 1 1 calc R . . C3 C 0.2120(6) 0.4234(9) 0.0442(5) 0.0310(15) Uani 1 1 d . . . H3A H 0.2011 0.4981 -0.0083 0.057(8) Uiso 1 1 calc R . . H3B H 0.1585 0.3203 0.0259 0.057(8) Uiso 1 1 calc R . . C4 C 0.1605(8) 0.5157(12) 0.1137(6) 0.059(2) Uani 1 1 d . . . H4A H 0.1682 0.4420 0.1655 0.057(8) Uiso 1 1 calc R . . H4B H 0.0692 0.5447 0.0895 0.057(8) Uiso 1 1 calc R . . H4C H 0.2106 0.6202 0.1310 0.057(8) Uiso 1 1 calc R . . Te1 Te 0.51763(4) 0.66337(5) 0.11469(3) 0.02539(12) Uani 1 1 d . . . Te2 Te 0.41599(4) 0.34606(5) 0.08534(3) 0.02611(12) Uani 1 1 d . . . C5 C 0.9092(7) 0.0589(10) 0.1262(6) 0.0413(18) Uani 1 1 d . . . F1 F 0.9757(5) 0.1289(7) 0.0717(4) 0.0653(14) Uani 1 1 d . . . F2 F 0.9458(5) -0.1045(7) 0.1400(4) 0.0794(18) Uani 1 1 d . . . F3 F 0.9442(5) 0.1434(7) 0.2034(3) 0.0696(16) Uani 1 1 d . . . O1 O 0.7086(5) 0.2542(6) 0.0670(3) 0.0390(12) Uani 1 1 d . . . O2 O 0.6762(4) -0.0054(6) 0.1461(3) 0.0408(12) Uani 1 1 d . . . O3 O 0.7136(5) -0.0236(6) -0.0043(4) 0.0483(13) Uani 1 1 d . . . S1 S 0.73196(15) 0.07232(19) 0.07863(12) 0.0273(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.030(3) 0.034(3) 0.033(4) 0.000(3) -0.003(3) -0.005(3) C2 0.039(4) 0.038(4) 0.030(4) 0.004(3) 0.003(3) -0.008(3) C3 0.020(3) 0.038(4) 0.035(4) -0.007(3) 0.008(3) -0.005(3) C4 0.041(4) 0.082(7) 0.049(5) -0.017(5) 0.001(4) 0.011(5) Te1 0.0242(2) 0.0210(2) 0.0305(2) -0.00252(18) 0.00559(16) -0.00192(16) Te2 0.0241(2) 0.0221(2) 0.0321(3) 0.00124(18) 0.00670(17) -0.00413(16) C5 0.024(3) 0.041(4) 0.056(5) 0.003(4) 0.003(3) -0.005(3) F1 0.044(3) 0.080(4) 0.080(4) -0.002(3) 0.031(3) -0.014(3) F2 0.041(3) 0.056(3) 0.130(5) 0.022(3) 0.000(3) 0.018(2) F3 0.046(3) 0.108(4) 0.046(3) -0.018(3) -0.007(2) -0.024(3) O1 0.039(3) 0.025(2) 0.052(3) 0.005(2) 0.008(2) 0.001(2) O2 0.036(2) 0.038(3) 0.048(3) 0.011(2) 0.011(2) -0.010(2) O3 0.054(3) 0.041(3) 0.045(3) -0.014(2) 0.001(3) -0.014(3) S1 0.0245(7) 0.0211(7) 0.0333(9) 0.0003(7) 0.0012(6) -0.0030(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 C1 C2 1.496(9) . ? C1 Te1 2.164(6) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 C4 1.477(10) . ? C3 Te2 2.149(6) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? Te1 Te2 2.6534(7) . ? C5 F2 1.314(8) . ? C5 F1 1.317(9) . ? C5 F3 1.317(9) . ? C5 S1 1.817(7) . ? O1 S1 1.423(5) . ? O2 S1 1.428(5) . ? O3 S1 1.436(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 C2 C1 Te1 114.1(5) . . ? C2 C1 H1A 108.7 . . ? Te1 C1 H1A 108.7 . . ? C2 C1 H1B 108.7 . . ? Te1 C1 H1B 108.7 . . ? H1A C1 H1B 107.6 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 Te2 115.3(5) . . ? C4 C3 H3A 108.5 . . ? Te2 C3 H3A 108.5 . . ? C4 C3 H3B 108.5 . . ? Te2 C3 H3B 108.5 . . ? H3A C3 H3B 107.5 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C1 Te1 Te2 96.34(18) . . ? C3 Te2 Te1 96.96(18) . . ? F2 C5 F1 108.4(7) . . ? F2 C5 F3 108.7(7) . . ? F1 C5 F3 106.7(6) . . ? F2 C5 S1 110.3(5) . . ? F1 C5 S1 111.2(5) . . ? F3 C5 S1 111.4(5) . . ? O1 S1 O2 114.5(3) . . ? O1 S1 O3 114.3(3) . . ? O2 S1 O3 115.4(3) . . ? O1 S1 C5 103.5(3) . . ? O2 S1 C5 103.8(3) . . ? O3 S1 C5 103.3(4) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 29.13 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.531 _refine_diff_density_min -0.778 _refine_diff_density_rms 0.201 # Attachment 'MESE4.CIF' data_mese4 _database_code_depnum_ccdc_archive 'CCDC 670387' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ;1,2,3,4-Tetramethyl-tetraselenetanediylium-bis- (trifluormethanesulfonate) ; _chemical_melting_point ? _chemical_formula_moiety (CH3Se)4,(CF3SO3)2 _chemical_formula_sum 'C6 H12 F6 O6 S2 Se4' _chemical_formula_weight 674.12 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' H H 0.0000 0.0000 '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 7.173(5) _cell_length_b 7.455(5) _cell_length_c 9.880(5) _cell_angle_alpha 76.932(5) _cell_angle_beta 75.714(5) _cell_angle_gamma 64.608(5) _cell_volume 458.1(5) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 999 _cell_measurement_theta_min 2. _cell_measurement_theta_max 60. _exptl_crystal_description brick _exptl_crystal_colour red _exptl_crystal_size_max .3 _exptl_crystal_size_mid .2 _exptl_crystal_size_min .1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.443 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 318 _exptl_absorpt_coefficient_mu 8.313 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3556 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details Bruker_2000_NT_Software_Reference_Manual _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Bruker_CCD _diffrn_measurement_method omega-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 3840 _diffrn_reflns_av_R_equivalents 0.0249 _diffrn_reflns_av_sigmaI/netI 0.0438 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 27.54 _reflns_number_total 2088 _reflns_number_gt 1551 _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^)+(0.0517P)^2^+0.0924P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2088 _refine_ls_number_parameters 128 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0588 _refine_ls_R_factor_gt 0.0362 _refine_ls_wR_factor_ref 0.0944 _refine_ls_wR_factor_gt 0.0822 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.043 _refine_ls_shift/su_mean 0.003 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 C1 C 0.1322(8) 0.1679(8) 0.5769(5) 0.0345(12) Uani 1 1 d . . . Se1 Se 0.28111(7) 0.53716(7) 0.91276(5) 0.02907(16) Uani 1 1 d . . . Se2 Se 0.50126(8) 0.24401(7) 1.01575(5) 0.02754(16) Uani 1 1 d . . . S3 S 0.06841(19) 0.12530(17) 0.76916(13) 0.0284(3) Uani 1 1 d . . . O1 O 0.2496(6) 0.1125(6) 0.8142(4) 0.0428(9) Uani 1 1 d . . . F2 F 0.1951(6) 0.3181(5) 0.5346(4) 0.0532(9) Uani 1 1 d . . . F3 F 0.2865(6) 0.0043(5) 0.5296(4) 0.0528(9) Uani 1 1 d . . . O2 O -0.1167(7) 0.2992(6) 0.7993(4) 0.0553(12) Uani 1 1 d . . . C3 C 0.4159(11) 0.5048(11) 0.7182(6) 0.0415(14) Uani 1 1 d . . . H8A H 0.558(11) 0.487(9) 0.716(7) 0.053(8) Uiso 1 1 d . . . H8B H 0.368(11) 0.597(11) 0.676(7) 0.053(8) Uiso 1 1 d . . . H8C H 0.381(9) 0.402(10) 0.707(6) 0.053(8) Uiso 1 1 d . . . O3 O 0.0375(6) -0.0587(6) 0.7960(4) 0.0435(10) Uani 1 1 d . . . C2 C 0.3128(10) 0.2302(10) 1.1924(7) 0.0395(14) Uani 1 1 d . . . H10A H 0.218(10) 0.345(10) 1.211(7) 0.053(8) Uiso 1 1 d . . . H10B H 0.391(10) 0.159(10) 1.240(7) 0.053(8) Uiso 1 1 d . . . H10C H 0.236(9) 0.151(9) 1.161(6) 0.053(8) Uiso 1 1 d . . . F1 F -0.0294(6) 0.2111(5) 0.5175(4) 0.0538(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.037(3) 0.031(3) 0.030(3) 0.001(2) -0.008(2) -0.009(2) Se1 0.0255(3) 0.0324(3) 0.0306(3) 0.0004(2) -0.0086(2) -0.0129(2) Se2 0.0331(3) 0.0236(3) 0.0273(3) -0.00150(19) -0.0060(2) -0.0131(2) S3 0.0261(6) 0.0252(6) 0.0282(6) -0.0014(5) -0.0040(5) -0.0064(5) O1 0.046(2) 0.049(2) 0.043(2) 0.0016(18) -0.0172(19) -0.0254(19) F2 0.074(2) 0.052(2) 0.043(2) 0.0089(16) -0.0084(17) -0.0416(19) F3 0.052(2) 0.048(2) 0.0418(19) -0.0114(16) 0.0078(16) -0.0112(17) O2 0.052(3) 0.042(2) 0.041(2) -0.0026(19) 0.001(2) 0.004(2) C3 0.052(4) 0.047(4) 0.027(3) -0.003(2) -0.014(3) -0.017(3) O3 0.045(2) 0.041(2) 0.048(2) 0.0075(18) -0.0117(19) -0.0252(19) C2 0.032(3) 0.041(3) 0.039(3) 0.003(3) 0.002(3) -0.017(3) F1 0.061(2) 0.064(2) 0.045(2) -0.0033(17) -0.0273(18) -0.0244(19) _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 C1 F1 1.312(6) . ? C1 F2 1.326(6) . ? C1 F3 1.332(6) . ? C1 S3 1.828(5) . ? Se1 C3 1.945(6) . ? Se1 Se2 2.2656(12) . ? Se2 C2 1.939(6) . ? S3 O2 1.427(4) . ? S3 O1 1.434(4) . ? S3 O3 1.438(4) . ? C3 H8A 0.96(7) . ? C3 H8B 0.71(7) . ? C3 H8C 0.94(7) . ? C2 H10A 0.86(6) . ? C2 H10B 0.76(7) . ? C2 H10C 1.10(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F1 C1 F2 107.9(4) . . ? F1 C1 F3 108.1(4) . . ? F2 C1 F3 107.9(4) . . ? F1 C1 S3 111.7(4) . . ? F2 C1 S3 111.0(4) . . ? F3 C1 S3 110.1(3) . . ? C3 Se1 Se2 97.6(2) . . ? C2 Se2 Se1 96.77(19) . . ? O2 S3 O1 115.1(3) . . ? O2 S3 O3 114.9(3) . . ? O1 S3 O3 115.2(2) . . ? O2 S3 C1 102.6(2) . . ? O1 S3 C1 103.4(2) . . ? O3 S3 C1 103.2(2) . . ? Se1 C3 H8A 104(4) . . ? Se1 C3 H8B 107(6) . . ? H8A C3 H8B 108(7) . . ? Se1 C3 H8C 99(4) . . ? H8A C3 H8C 123(5) . . ? H8B C3 H8C 113(7) . . ? Se2 C2 H10A 114(4) . . ? Se2 C2 H10B 100(5) . . ? H10A C2 H10B 125(7) . . ? Se2 C2 H10C 97(3) . . ? H10A C2 H10C 107(5) . . ? H10B C2 H10C 110(6) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.043 _refine_diff_density_min -0.572 _refine_diff_density_rms 0.157 # Attachment 'PR4TE4.CIF' data_pr4te4 _database_code_depnum_ccdc_archive 'CCDC 670388' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ;1,2,3,4-Tetrapropyl-tetratelluretanediylium-bis- (trifluorsulfonate) ; _chemical_melting_point ? _chemical_formula_moiety (C3H7Te)4,(CF3SO3)2 _chemical_formula_sum 'C14 H28 F6 O6 S2 Te4' _chemical_formula_weight 980.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.8167(14) _cell_length_b 8.4933(15) _cell_length_c 11.623(2) _cell_angle_alpha 81.367(4) _cell_angle_beta 89.475(4) _cell_angle_gamma 64.800(3) _cell_volume 689.0(2) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 999 _cell_measurement_theta_min 2. _cell_measurement_theta_max 3. _exptl_crystal_description flat_needle _exptl_crystal_colour black _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.364 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 454 _exptl_absorpt_coefficient_mu 4.410 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.856 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details Bruker_2000_NT_Software_Reference_Manual _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Bruker_CCD _diffrn_measurement_method omega_scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 11507 _diffrn_reflns_av_R_equivalents 0.0319 _diffrn_reflns_av_sigmaI/netI 0.0408 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 30.54 _reflns_number_total 4108 _reflns_number_gt 3071 _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^)+(0.0323P)^2^+0.9000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4108 _refine_ls_number_parameters 188 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0514 _refine_ls_R_factor_gt 0.0292 _refine_ls_wR_factor_ref 0.0700 _refine_ls_wR_factor_gt 0.0603 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 0.988 _refine_ls_shift/su_max 0.027 _refine_ls_shift/su_mean 0.001 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 C1 C 0.0734(6) 0.1510(6) 1.1932(3) 0.0239(8) Uani 1 1 d . . . H1A H 0.088(8) 0.229(8) 1.221(5) 0.043(4) Uiso 1 1 d . . . H1B H -0.030(8) 0.132(7) 1.224(5) 0.043(4) Uiso 1 1 d . . . C2 C 0.2610(6) -0.0099(6) 1.1988(4) 0.0303(9) Uani 1 1 d . . . H2A H 0.361(7) 0.023(7) 1.159(5) 0.043(4) Uiso 1 1 d . . . H2B H 0.256(8) -0.085(7) 1.161(5) 0.043(4) Uiso 1 1 d . . . C3 C 0.3225(7) -0.0959(7) 1.3248(4) 0.0338(10) Uani 1 1 d . . . H3A H 0.331(8) -0.025(7) 1.367(5) 0.043(4) Uiso 1 1 d . . . H3B H 0.439(8) -0.205(7) 1.326(5) 0.043(4) Uiso 1 1 d . . . H3C H 0.248(8) -0.137(7) 1.363(5) 0.043(4) Uiso 1 1 d . . . C4 C 0.1417(6) 0.3648(6) 0.7522(4) 0.0257(9) Uani 1 1 d . . . H4A H 0.029(8) 0.446(7) 0.747(5) 0.043(4) Uiso 1 1 d . . . H4B H 0.228(8) 0.388(7) 0.712(5) 0.043(4) Uiso 1 1 d . . . C5 C 0.1363(8) 0.2064(7) 0.7105(4) 0.0340(10) Uani 1 1 d . . . H5A H 0.064(8) 0.170(7) 0.752(5) 0.043(4) Uiso 1 1 d . . . H5B H 0.247(8) 0.105(8) 0.733(5) 0.043(4) Uiso 1 1 d . . . C6 C 0.0927(8) 0.2410(8) 0.5797(4) 0.0372(11) Uani 1 1 d . . . H6A H -0.027(8) 0.346(7) 0.560(5) 0.043(4) Uiso 1 1 d . . . H6B H 0.090(7) 0.138(7) 0.554(5) 0.043(4) Uiso 1 1 d . . . H6C H 0.182(8) 0.279(7) 0.542(5) 0.043(4) Uiso 1 1 d . . . Te1 Te -0.05520(3) 0.27279(3) 1.01924(2) 0.02140(7) Uani 1 1 d . . . Te2 Te 0.24199(3) 0.31518(4) 0.93267(2) 0.02143(7) Uani 1 1 d . . . C7 C 0.5325(6) 0.3204(7) 0.3594(4) 0.0303(10) Uani 1 1 d . . . F1 F 0.5290(5) 0.1665(4) 0.3958(2) 0.0460(7) Uani 1 1 d . . . F2 F 0.4074(4) 0.4376(4) 0.4174(2) 0.0477(7) Uani 1 1 d . . . F3 F 0.7029(4) 0.3063(5) 0.3899(3) 0.0538(9) Uani 1 1 d . . . O1 O 0.2926(4) 0.3992(5) 0.1871(3) 0.0325(7) Uani 1 1 d . . . O2 O 0.6260(4) 0.2442(4) 0.1558(3) 0.0335(7) Uani 1 1 d . . . O3 O 0.4944(5) 0.5514(5) 0.1800(3) 0.0389(8) Uani 1 1 d . . . S S 0.48116(13) 0.38613(14) 0.20276(8) 0.0220(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0243(18) 0.027(2) 0.0204(19) -0.0018(17) 0.0013(15) -0.0116(17) C2 0.031(2) 0.027(3) 0.026(2) -0.0054(18) -0.0018(17) -0.0059(19) C3 0.036(2) 0.033(3) 0.028(2) 0.001(2) -0.0049(19) -0.011(2) C4 0.0263(19) 0.029(2) 0.0222(19) -0.0048(17) 0.0038(16) -0.0125(18) C5 0.047(3) 0.030(3) 0.029(2) -0.008(2) 0.003(2) -0.020(2) C6 0.041(3) 0.046(3) 0.030(2) -0.016(2) 0.004(2) -0.021(2) Te1 0.01989(12) 0.02393(16) 0.02112(13) -0.00086(10) -0.00077(9) -0.01098(11) Te2 0.01809(12) 0.02469(16) 0.02112(13) -0.00387(11) 0.00182(9) -0.00878(11) C7 0.027(2) 0.043(3) 0.024(2) -0.0031(19) -0.0006(16) -0.019(2) F1 0.066(2) 0.0418(18) 0.0288(14) 0.0084(13) -0.0026(13) -0.0265(16) F2 0.0554(18) 0.061(2) 0.0312(15) -0.0212(15) 0.0105(13) -0.0244(16) F3 0.0388(15) 0.090(3) 0.0362(16) -0.0022(17) -0.0152(13) -0.0338(17) O1 0.0203(13) 0.050(2) 0.0290(16) -0.0009(14) -0.0050(11) -0.0189(14) O2 0.0282(15) 0.0364(19) 0.0319(17) -0.0081(14) 0.0056(13) -0.0094(14) O3 0.0431(18) 0.036(2) 0.044(2) -0.0020(16) 0.0050(15) -0.0240(16) S 0.0183(4) 0.0281(6) 0.0203(4) -0.0006(4) -0.0009(3) -0.0117(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 C1 C2 1.514(6) . ? C1 Te1 2.166(4) . ? C1 H1A 0.83(6) . ? C1 H1B 0.94(5) . ? C2 C3 1.517(6) . ? C2 H2A 1.02(5) . ? C2 H2B 0.84(6) . ? C3 H3A 0.86(6) . ? C3 H3B 0.98(6) . ? C3 H3C 0.88(6) . ? C4 C5 1.514(7) . ? C4 Te2 2.162(4) . ? C4 H4A 0.85(6) . ? C4 H4B 0.89(5) . ? C5 C6 1.518(7) . ? C5 H5A 0.87(5) . ? C5 H5B 0.93(6) . ? C6 H6A 0.98(6) . ? C6 H6B 0.98(6) . ? C6 H6C 0.96(5) . ? Te1 Te2 2.6644(5) . ? C7 F1 1.324(5) . ? C7 F2 1.327(5) . ? C7 F3 1.332(5) . ? C7 S 1.818(4) . ? O1 S 1.442(3) . ? O2 S 1.434(3) . ? O3 S 1.436(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 Te1 115.1(3) . . ? C2 C1 H1A 110(4) . . ? Te1 C1 H1A 105(4) . . ? C2 C1 H1B 117(3) . . ? Te1 C1 H1B 97(3) . . ? H1A C1 H1B 112(5) . . ? C1 C2 C3 109.8(4) . . ? C1 C2 H2A 111(3) . . ? C3 C2 H2A 112(3) . . ? C1 C2 H2B 113(4) . . ? C3 C2 H2B 109(4) . . ? H2A C2 H2B 103(5) . . ? C2 C3 H3A 112(4) . . ? C2 C3 H3B 108(3) . . ? H3A C3 H3B 114(5) . . ? C2 C3 H3C 117(4) . . ? H3A C3 H3C 103(5) . . ? H3B C3 H3C 101(5) . . ? C5 C4 Te2 113.8(3) . . ? C5 C4 H4A 108(4) . . ? Te2 C4 H4A 106(4) . . ? C5 C4 H4B 107(3) . . ? Te2 C4 H4B 105(4) . . ? H4A C4 H4B 117(5) . . ? C4 C5 C6 111.3(4) . . ? C4 C5 H5A 111(4) . . ? C6 C5 H5A 115(4) . . ? C4 C5 H5B 112(4) . . ? C6 C5 H5B 111(3) . . ? H5A C5 H5B 95(5) . . ? C5 C6 H6A 109(3) . . ? C5 C6 H6B 110(3) . . ? H6A C6 H6B 112(5) . . ? C5 C6 H6C 108(3) . . ? H6A C6 H6C 102(4) . . ? H6B C6 H6C 114(4) . . ? C1 Te1 Te2 96.37(11) . . ? C4 Te2 Te1 95.21(11) . . ? F1 C7 F2 107.6(3) . . ? F1 C7 F3 107.9(4) . . ? F2 C7 F3 107.2(4) . . ? F1 C7 S 111.5(3) . . ? F2 C7 S 111.5(3) . . ? F3 C7 S 111.1(3) . . ? O2 S O3 115.2(2) . . ? O2 S O1 114.7(2) . . ? O3 S O1 114.7(2) . . ? O2 S C7 103.5(2) . . ? O3 S C7 103.3(2) . . ? O1 S C7 103.14(18) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 30.54 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 1.223 _refine_diff_density_min -0.804 _refine_diff_density_rms 0.173