# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'G Reid' _publ_contact_author_email GR@SOTON.AC.UK _publ_section_title ; Preparations and structures of tellurium(IV) halide complexes with thioether coordination ; loop_ _publ_author_name 'G. Reid' 'Chitra Gurnani' 'Marek Jura' 'W. Levason' 'Raju Ratnani' 'Michael Webster' # Attachment 'Te_all8atest.txt' # 08mj41 data_08mj41 _database_code_depnum_ccdc_archive 'CCDC 711707' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2008-09-29 _audit_author_name 'Webster, M.' _audit_update_record ' 2009-02-01 Updated atom labelling for C2/C4.' _chemical_name_systematic ; Tetrachloro(2,5-dithiahexane-S,S')tellurium(IV) ; # I-Lab software gives S ligand as 1,2-bis(methylthio)ethane _chemical_name_common Tetrachloro(2,5-dithiahexane-S,S')tellurium(IV) _chemical_melting_point ? _chemical_formula_moiety 'C4 H10 Cl4 S2 Te' _chemical_formula_sum 'C4 H10 Cl4 S2 Te' _chemical_formula_weight 391.64 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' Cl Cl 0.1484 0.1585 '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' _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 7.400(3) _cell_length_b 11.512(5) _cell_length_c 8.051(3) _cell_angle_alpha 90.00 _cell_angle_beta 117.05(2) _cell_angle_gamma 90.00 _cell_volume 610.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 36893 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.129 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 372 _exptl_absorpt_coefficient_mu 3.598 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5725 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13481 _diffrn_reflns_av_R_equivalents 0.0700 _diffrn_reflns_av_sigmaI/netI 0.0590 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 27.55 _reflns_number_total 2794 _reflns_number_gt 2494 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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 'w=1/[\s^2^(Fo^2^)+(0.0274P)^2^+0.7863P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(3) _chemical_absolute_configuration ad _refine_ls_number_reflns 2794 _refine_ls_number_parameters 100 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0462 _refine_ls_R_factor_gt 0.0362 _refine_ls_wR_factor_ref 0.0745 _refine_ls_wR_factor_gt 0.0705 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 0.31098(5) 0.42319(3) 0.25305(5) 0.02039(10) Uani 1 1 d . . . Cl1 Cl 0.3039(2) 0.55203(13) 0.0132(2) 0.0281(4) Uani 1 1 d . . . Cl2 Cl 0.5500(2) 0.27995(13) 0.2253(2) 0.0298(4) Uani 1 1 d . . . Cl3 Cl 0.0035(2) 0.32149(14) 0.0212(2) 0.0339(4) Uani 1 1 d . . . Cl4 Cl 0.5929(2) 0.53980(13) 0.5043(2) 0.0261(3) Uani 1 1 d . . . S1 S 0.2202(2) 0.30901(13) 0.5258(2) 0.0246(3) Uani 1 1 d . . . S2 S 0.0883(2) 0.59136(13) 0.3179(2) 0.0226(3) Uani 1 1 d . . . C1 C 0.4529(10) 0.3292(6) 0.7388(9) 0.0329(16) Uani 1 1 d . . . H1A H 0.5564 0.2754 0.7407 0.049 Uiso 1 1 calc R . . H1B H 0.4278 0.3139 0.8463 0.049 Uiso 1 1 calc R . . H1C H 0.5005 0.4093 0.7449 0.049 Uiso 1 1 calc R . . C2 C 0.0528(8) 0.4155(7) 0.5500(7) 0.0238(11) Uani 1 1 d . . . H2A H -0.0868 0.4015 0.4509 0.029 Uiso 1 1 calc R . . H2B H 0.0523 0.4029 0.6714 0.029 Uiso 1 1 calc R . . C3 C 0.1076(9) 0.5423(5) 0.5393(8) 0.0217(13) Uani 1 1 d . . . H3A H 0.2488 0.5552 0.6361 0.026 Uiso 1 1 calc R . . H3B H 0.0186 0.5919 0.5711 0.026 Uiso 1 1 calc R . . C4 C -0.1747(9) 0.5627(6) 0.1585(9) 0.0313(15) Uani 1 1 d . . . H4A H -0.2020 0.5861 0.0322 0.047 Uiso 1 1 calc R . . H4B H -0.2623 0.6070 0.1973 0.047 Uiso 1 1 calc R . . H4C H -0.2024 0.4796 0.1598 0.047 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 0.01907(16) 0.02068(17) 0.01924(17) -0.00160(18) 0.00682(13) -0.00134(17) Cl1 0.0312(8) 0.0291(8) 0.0228(8) 0.0018(6) 0.0113(7) 0.0008(7) Cl2 0.0297(8) 0.0241(8) 0.0316(8) -0.0001(6) 0.0104(7) 0.0053(6) Cl3 0.0258(8) 0.0312(9) 0.0357(9) -0.0113(7) 0.0062(7) -0.0058(7) Cl4 0.0230(7) 0.0267(8) 0.0245(7) -0.0023(6) 0.0071(6) -0.0044(6) S1 0.0239(8) 0.0197(8) 0.0265(8) 0.0004(6) 0.0082(6) -0.0016(6) S2 0.0217(7) 0.0207(7) 0.0226(8) 0.0022(6) 0.0076(6) 0.0005(6) C1 0.031(3) 0.031(4) 0.027(3) 0.009(3) 0.005(3) 0.005(3) C2 0.028(3) 0.022(3) 0.024(3) 0.005(3) 0.014(2) 0.001(3) C3 0.024(3) 0.019(3) 0.021(3) -0.001(2) 0.009(3) 0.004(2) C4 0.022(3) 0.043(4) 0.022(3) -0.004(3) 0.004(3) 0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Te1 Cl1 2.4166(17) . ? Te1 Cl3 2.4839(17) . ? Te1 Cl2 2.5016(17) . ? Te1 Cl4 2.5313(16) . ? Te1 S2 2.7420(17) . ? Te1 S1 2.8880(18) . ? S1 C1 1.810(6) . ? S1 C2 1.816(7) . ? S2 C4 1.809(6) . ? S2 C3 1.812(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.528(10) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 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 Cl1 Te1 Cl3 90.53(6) . . ? Cl1 Te1 Cl2 95.30(6) . . ? Cl3 Te1 Cl2 93.75(6) . . ? Cl1 Te1 Cl4 91.35(6) . . ? Cl3 Te1 Cl4 172.27(6) . . ? Cl2 Te1 Cl4 93.54(6) . . ? Cl1 Te1 S2 85.54(6) . . ? Cl3 Te1 S2 92.95(6) . . ? Cl2 Te1 S2 173.23(5) . . ? Cl4 Te1 S2 79.72(6) . . ? Cl1 Te1 S1 163.50(5) . . ? Cl3 Te1 S1 84.64(6) . . ? Cl2 Te1 S1 100.74(6) . . ? Cl4 Te1 S1 91.48(5) . . ? S2 Te1 S1 78.99(5) . . ? C1 S1 C2 102.3(3) . . ? C1 S1 Te1 102.3(2) . . ? C2 S1 Te1 100.4(2) . . ? C4 S2 C3 102.7(3) . . ? C4 S2 Te1 106.4(2) . . ? C3 S2 Te1 100.5(2) . . ? S1 C1 H1A 109.5 . . ? S1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? S1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 S1 115.3(4) . . ? C3 C2 H2A 108.5 . . ? S1 C2 H2A 108.5 . . ? C3 C2 H2B 108.5 . . ? S1 C2 H2B 108.5 . . ? H2A C2 H2B 107.5 . . ? C2 C3 S2 116.7(4) . . ? C2 C3 H3A 108.1 . . ? S2 C3 H3A 108.1 . . ? C2 C3 H3B 108.1 . . ? S2 C3 H3B 108.1 . . ? H3A C3 H3B 107.3 . . ? S2 C4 H4A 109.5 . . ? S2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? S2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 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 # Cl2 Te1 S2 C4 -176.1(5) . . . . ? # Cl2 Te1 S2 C3 -69.4(5) . . . . ? Cl1 Te1 S1 C1 -120.5(3) . . . . ? Cl3 Te1 S1 C1 166.1(2) . . . . ? Cl2 Te1 S1 C1 73.2(2) . . . . ? Cl4 Te1 S1 C1 -20.6(2) . . . . ? S2 Te1 S1 C1 -99.9(2) . . . . ? Cl1 Te1 S1 C2 -15.3(3) . . . . ? Cl3 Te1 S1 C2 -88.8(2) . . . . ? Cl2 Te1 S1 C2 178.4(2) . . . . ? Cl4 Te1 S1 C2 84.5(2) . . . . ? S2 Te1 S1 C2 5.3(2) . . . . ? Cl1 Te1 S2 C4 86.5(3) . . . . ? Cl3 Te1 S2 C4 -3.8(3) . . . . ? Cl4 Te1 S2 C4 178.7(3) . . . . ? S1 Te1 S2 C4 -87.8(3) . . . . ? Cl1 Te1 S2 C3 -166.8(2) . . . . ? Cl3 Te1 S2 C3 102.9(2) . . . . ? Cl4 Te1 S2 C3 -74.7(2) . . . . ? S1 Te1 S2 C3 18.9(2) . . . . ? C1 S1 C2 C3 68.6(5) . . . . ? Te1 S1 C2 C3 -36.5(4) . . . . ? S1 C2 C3 S2 65.5(5) . . . . ? C4 S2 C3 C2 58.1(5) . . . . ? Te1 S2 C3 C2 -51.5(5) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.599 _refine_diff_density_min -1.119 _refine_diff_density_rms 0.151 #===END OF CIF ============================================================== # 08mj51 data_08mj51 _database_code_depnum_ccdc_archive 'CCDC 711708' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2008-11-13 _audit_author_name 'Webster, M.' _chemical_name_systematic ; chloro(1,2-bis(isopropylthio)ethane)tellurium(II) nonachloroditellurium(IV) ; # C8H18S2 = 1,2-bis(isopropylthio)ethane # 2-{[2-(isopropylthio)ethyl]thio}propane i-Lab IUPAC name of S2 ligand # 2,7-dimethyl-3,6-dithiaoctane # 2-(2-isopropylsulfanylethylsulfanyl)propane (from chemspider) # SMILES: S(C(C)C)CCSC(C)C CC(C)SCCSC(C)C _chemical_name_common ;chloro(1,2-bis(isopropylthio)ethane)tellurium(ii) nonachloroditellurium(IV) ; _chemical_melting_point ? _chemical_formula_moiety 'C8 H18 Cl S2 Te 1+, Cl9 Te2 1-' _chemical_formula_sum 'C8 H18 Cl10 S2 Te3' _chemical_formula_structural '((C8 H18 S2) Te Cl) (Cl9 Te2)' _chemical_formula_weight 915.64 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' Cl Cl 0.1484 0.1585 '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' _space_group_IT_number 2 _space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6256(10) _cell_length_b 13.7668(10) _cell_length_c 18.1851(15) _cell_angle_alpha 98.143(5) _cell_angle_beta 98.110(5) _cell_angle_gamma 100.759(5) _cell_volume 2548.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 45929 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 # _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.387 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1696 _exptl_absorpt_coefficient_mu 4.619 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8593 # _exptl_absorpt_correction_T_max 1.0000 # _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48243 _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_av_sigmaI/netI 0.0405 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 27.52 _reflns_number_total 11643 _reflns_number_gt 9651 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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 'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+10.7512P] 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 11643 _refine_ls_number_parameters 423 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0509 _refine_ls_R_factor_gt 0.0356 _refine_ls_wR_factor_ref 0.0688 _refine_ls_wR_factor_gt 0.0625 _refine_ls_goodness_of_fit_ref 1.153 _refine_ls_restrained_S_all 1.170 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Te1 Te 0.25198(3) 0.82649(2) 0.235963(18) 0.01692(7) Uani 1 1 d . . . Te2 Te 0.73185(3) 0.68594(2) 0.275854(17) 0.01673(7) Uani 1 1 d . . . Te3 Te 0.18289(3) 0.48839(2) 0.319637(18) 0.01841(7) Uani 1 1 d . . . Te4 Te 0.32117(3) 0.77162(2) 0.446057(17) 0.01620(7) Uani 1 1 d . . . Te5 Te 0.71676(3) 0.71694(2) 0.054850(17) 0.01584(7) Uani 1 1 d . . . Te6 Te 0.76473(3) 1.00318(2) 0.168418(17) 0.01543(7) Uani 1 1 d . . . Cl1 Cl 0.15740(12) 0.87963(10) 0.36000(7) 0.0246(3) Uani 1 1 d . . . Cl2 Cl 0.55236(12) 0.63123(9) 0.15479(7) 0.0220(3) Uani 1 1 d . . . Cl3 Cl 0.02222(12) 0.57025(10) 0.25632(8) 0.0295(3) Uani 1 1 d . . . Cl4 Cl 0.01537(14) 0.35607(11) 0.33138(10) 0.0418(4) Uani 1 1 d . . . Cl5 Cl 0.21565(18) 0.41151(11) 0.20257(8) 0.0415(4) Uani 1 1 d . . . Cl6 Cl 0.34521(12) 0.40078(10) 0.38422(8) 0.0289(3) Uani 1 1 d D . . Cl7 Cl 0.47434(12) 0.70208(10) 0.51495(7) 0.0227(3) Uani 1 1 d . . . Cl8 Cl 0.49201(12) 0.90016(9) 0.43178(7) 0.0255(3) Uani 1 1 d . . . Cl9 Cl 0.28017(14) 0.85924(10) 0.55853(7) 0.0275(3) Uani 1 1 d . . . Cl10 Cl 0.37420(11) 0.66472(9) 0.31543(7) 0.0206(2) Uani 1 1 d . . . Cl11 Cl 0.15043(12) 0.59922(10) 0.46175(7) 0.0252(3) Uani 1 1 d . . . Cl12 Cl 0.57272(14) 0.61231(11) -0.04710(8) 0.0321(3) Uani 1 1 d . . . Cl13 Cl 0.86555(12) 0.77567(10) -0.02084(7) 0.0249(3) Uani 1 1 d . . . Cl14 Cl 0.83411(13) 0.59010(9) 0.07736(7) 0.0261(3) Uani 1 1 d . . . Cl15 Cl 0.60251(12) 0.93199(10) 0.24184(8) 0.0265(3) Uani 1 1 d . . . Cl16 Cl 0.93330(12) 1.08102(10) 0.09792(7) 0.0263(3) Uani 1 1 d . . . Cl17 Cl 0.89353(14) 1.09442(10) 0.28073(7) 0.0310(3) Uani 1 1 d . . . Cl18 Cl 0.64681(13) 1.13081(10) 0.14720(8) 0.0273(3) Uani 1 1 d . . . Cl19 Cl 0.61166(12) 0.87752(10) 0.02730(7) 0.0244(3) Uani 1 1 d . . . Cl20 Cl 0.88625(11) 0.84079(9) 0.18345(7) 0.0218(3) Uani 1 1 d . . . S1 S 0.19365(11) 0.97914(9) 0.19676(7) 0.0172(2) Uani 1 1 d . . . S2 S 0.32290(12) 0.79529(9) 0.10463(7) 0.0185(2) Uani 1 1 d . . . S3 S 0.88142(11) 0.71488(9) 0.40885(7) 0.0170(2) Uani 1 1 d . . . S4 S 0.62240(11) 0.53167(9) 0.31416(7) 0.0166(2) Uani 1 1 d . . . C1 C 0.3664(6) 1.1022(4) 0.3130(3) 0.0341(14) Uani 1 1 d . . . H1A H 0.4466 1.1532 0.3312 0.051 Uiso 1 1 calc R . . H1B H 0.3742 1.0411 0.3336 0.051 Uiso 1 1 calc R . . H1C H 0.2928 1.1275 0.3293 0.051 Uiso 1 1 calc R . . C2 C 0.3240(6) 1.1673(4) 0.1902(3) 0.0334(14) Uani 1 1 d . . . H2A H 0.2425 1.1856 0.2001 0.050 Uiso 1 1 calc R . . H2B H 0.3200 1.1492 0.1357 0.050 Uiso 1 1 calc R . . H2C H 0.3966 1.2244 0.2106 0.050 Uiso 1 1 calc R . . C3 C 0.3442(5) 1.0784(4) 0.2278(3) 0.0197(10) Uani 1 1 d . . . H3 H 0.4195 1.0528 0.2111 0.024 Uiso 1 1 calc R . . C4 C 0.1852(5) 0.9483(4) 0.0951(3) 0.0185(10) Uani 1 1 d . . . H4A H 0.1051 0.8969 0.0738 0.022 Uiso 1 1 calc R . . H4B H 0.1781 1.0091 0.0729 0.022 Uiso 1 1 calc R . . C5 C 0.2999(5) 0.9097(4) 0.0716(3) 0.0207(11) Uani 1 1 d . . . H5A H 0.3797 0.9623 0.0909 0.025 Uiso 1 1 calc R . . H5B H 0.2885 0.8977 0.0158 0.025 Uiso 1 1 calc R . . C6 C 0.1809(5) 0.6992(4) 0.0527(3) 0.0213(11) Uani 1 1 d . . . H6 H 0.0991 0.7213 0.0620 0.026 Uiso 1 1 calc R . . C7 C 0.1890(5) 0.6048(4) 0.0862(3) 0.0244(11) Uani 1 1 d . . . H7A H 0.1139 0.5513 0.0623 0.037 Uiso 1 1 calc R . . H7B H 0.1891 0.6190 0.1406 0.037 Uiso 1 1 calc R . . H7C H 0.2693 0.5833 0.0774 0.037 Uiso 1 1 calc R . . C8 C 0.1848(6) 0.6853(4) -0.0315(3) 0.0293(13) Uani 1 1 d . . . H8A H 0.2674 0.6679 -0.0404 0.044 Uiso 1 1 calc R . . H8B H 0.1771 0.7478 -0.0500 0.044 Uiso 1 1 calc R . . H8C H 0.1125 0.6312 -0.0584 0.044 Uiso 1 1 calc R . . C9 C 0.8459(5) 0.9065(4) 0.4260(3) 0.0265(12) Uani 1 1 d . . . H9A H 0.9403 0.9271 0.4295 0.040 Uiso 1 1 calc R . . H9B H 0.8132 0.9607 0.4530 0.040 Uiso 1 1 calc R . . H9C H 0.8042 0.8920 0.3729 0.040 Uiso 1 1 calc R . . C10 C 0.8768(7) 0.8314(4) 0.5448(3) 0.0356(14) Uani 1 1 d . . . H10A H 0.8488 0.8883 0.5718 0.053 Uiso 1 1 calc R . . H10B H 0.9717 0.8465 0.5497 0.053 Uiso 1 1 calc R . . H10C H 0.8491 0.7713 0.5665 0.053 Uiso 1 1 calc R . . C11 C 0.8151(5) 0.8128(4) 0.4612(3) 0.0192(10) Uani 1 1 d . . . H11 H 0.7187 0.7902 0.4559 0.023 Uiso 1 1 calc R . . C12 C 0.8159(5) 0.6019(4) 0.4426(3) 0.0195(10) Uani 1 1 d . . . H12A H 0.8623 0.5489 0.4258 0.023 Uiso 1 1 calc R . . H12B H 0.8331 0.6153 0.4984 0.023 Uiso 1 1 calc R . . C13 C 0.6695(5) 0.5624(4) 0.4154(3) 0.0193(10) Uani 1 1 d . . . H13A H 0.6229 0.6139 0.4348 0.023 Uiso 1 1 calc R . . H13B H 0.6415 0.5017 0.4372 0.023 Uiso 1 1 calc R . . C14 C 0.7165(5) 0.4358(4) 0.2872(3) 0.0177(10) Uani 1 1 d . . . H14 H 0.8115 0.4651 0.3037 0.021 Uiso 1 1 calc R . . C15 C 0.6867(6) 0.4081(4) 0.2017(3) 0.0286(12) Uani 1 1 d . . . H15A H 0.5934 0.3803 0.1854 0.043 Uiso 1 1 calc R . . H15B H 0.7358 0.3580 0.1851 0.043 Uiso 1 1 calc R . . H15C H 0.7116 0.4682 0.1795 0.043 Uiso 1 1 calc R . . C16 C 0.6782(5) 0.3476(4) 0.3259(3) 0.0231(11) Uani 1 1 d . . . H16A H 0.7175 0.2924 0.3064 0.035 Uiso 1 1 calc R . . H16B H 0.5834 0.3255 0.3162 0.035 Uiso 1 1 calc R . . H16C H 0.7091 0.3675 0.3804 0.035 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 0.01803(15) 0.01583(16) 0.01823(16) 0.00628(13) 0.00427(12) 0.00353(12) Te2 0.01961(16) 0.01495(15) 0.01690(16) 0.00590(12) 0.00415(12) 0.00367(12) Te3 0.01744(16) 0.01641(16) 0.02231(17) 0.00787(13) 0.00143(13) 0.00404(12) Te4 0.01820(15) 0.01677(16) 0.01625(15) 0.00527(12) 0.00533(12) 0.00665(12) Te5 0.01682(15) 0.01519(15) 0.01475(15) 0.00370(12) 0.00169(12) 0.00144(12) Te6 0.01655(15) 0.01398(15) 0.01663(15) 0.00454(12) 0.00427(12) 0.00296(12) Cl1 0.0241(6) 0.0279(7) 0.0277(7) 0.0109(5) 0.0108(5) 0.0109(5) Cl2 0.0202(6) 0.0244(6) 0.0209(6) 0.0066(5) 0.0028(5) 0.0024(5) Cl3 0.0219(6) 0.0301(7) 0.0404(8) 0.0196(6) 0.0019(6) 0.0078(5) Cl4 0.0233(7) 0.0281(7) 0.0721(11) 0.0281(8) -0.0056(7) -0.0040(6) Cl5 0.0720(11) 0.0310(8) 0.0253(7) 0.0025(6) 0.0044(7) 0.0253(8) Cl6 0.0233(6) 0.0348(7) 0.0349(7) 0.0192(6) 0.0057(6) 0.0117(6) Cl7 0.0224(6) 0.0296(7) 0.0202(6) 0.0086(5) 0.0049(5) 0.0120(5) Cl8 0.0257(6) 0.0208(6) 0.0282(7) 0.0052(5) 0.0048(5) -0.0003(5) Cl9 0.0389(7) 0.0259(7) 0.0233(6) 0.0049(5) 0.0122(6) 0.0152(6) Cl10 0.0209(6) 0.0207(6) 0.0230(6) 0.0050(5) 0.0090(5) 0.0066(5) Cl11 0.0222(6) 0.0289(7) 0.0294(7) 0.0137(6) 0.0099(5) 0.0073(5) Cl12 0.0338(7) 0.0306(7) 0.0232(7) -0.0016(6) -0.0049(6) -0.0031(6) Cl13 0.0226(6) 0.0330(7) 0.0222(6) 0.0115(5) 0.0079(5) 0.0053(5) Cl14 0.0330(7) 0.0219(6) 0.0275(7) 0.0073(5) 0.0076(6) 0.0118(5) Cl15 0.0222(6) 0.0307(7) 0.0318(7) 0.0156(6) 0.0110(5) 0.0057(5) Cl16 0.0224(6) 0.0326(7) 0.0296(7) 0.0155(6) 0.0106(5) 0.0077(5) Cl17 0.0334(7) 0.0293(7) 0.0224(7) -0.0032(6) 0.0002(6) -0.0038(6) Cl18 0.0293(7) 0.0216(6) 0.0391(8) 0.0134(6) 0.0144(6) 0.0128(5) Cl19 0.0207(6) 0.0305(7) 0.0240(6) 0.0096(5) 0.0023(5) 0.0078(5) Cl20 0.0168(6) 0.0204(6) 0.0264(6) 0.0061(5) -0.0012(5) 0.0013(5) S1 0.0178(6) 0.0165(6) 0.0187(6) 0.0052(5) 0.0036(5) 0.0052(5) S2 0.0193(6) 0.0177(6) 0.0200(6) 0.0044(5) 0.0050(5) 0.0053(5) S3 0.0167(6) 0.0150(6) 0.0196(6) 0.0049(5) 0.0034(5) 0.0029(5) S4 0.0164(6) 0.0170(6) 0.0173(6) 0.0051(5) 0.0047(5) 0.0029(5) C1 0.042(3) 0.021(3) 0.030(3) 0.001(2) -0.001(3) -0.006(3) C2 0.041(3) 0.019(3) 0.038(3) 0.011(3) -0.002(3) 0.002(2) C3 0.018(2) 0.020(2) 0.018(2) 0.005(2) 0.000(2) -0.002(2) C4 0.021(2) 0.017(2) 0.015(2) 0.001(2) 0.0002(19) 0.002(2) C5 0.026(3) 0.020(3) 0.019(2) 0.005(2) 0.009(2) 0.008(2) C6 0.024(3) 0.019(2) 0.020(3) 0.002(2) 0.003(2) 0.003(2) C7 0.033(3) 0.018(3) 0.020(3) 0.003(2) 0.000(2) 0.004(2) C8 0.047(4) 0.025(3) 0.018(3) 0.006(2) 0.007(2) 0.010(3) C9 0.033(3) 0.014(2) 0.033(3) 0.005(2) 0.008(2) 0.003(2) C10 0.057(4) 0.022(3) 0.023(3) -0.002(2) 0.003(3) 0.005(3) C11 0.020(2) 0.014(2) 0.025(3) 0.005(2) 0.006(2) 0.0048(19) C12 0.024(3) 0.016(2) 0.019(2) 0.008(2) 0.002(2) 0.002(2) C13 0.021(2) 0.021(3) 0.017(2) 0.004(2) 0.007(2) 0.004(2) C14 0.021(2) 0.017(2) 0.018(2) 0.007(2) 0.007(2) 0.006(2) C15 0.050(4) 0.018(3) 0.022(3) 0.006(2) 0.011(3) 0.011(2) C16 0.029(3) 0.015(2) 0.025(3) 0.007(2) 0.004(2) 0.003(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 Te1 S1 2.4688(12) . ? Te1 S2 2.6067(13) . ? Te1 Cl1 2.6608(13) . ? Te2 S4 2.4646(12) . ? Te2 Cl2 2.6193(13) . ? Te2 S3 2.6343(12) . ? Te3 Cl5 2.3414(15) . ? Te3 Cl4 2.3536(14) . ? Te3 Cl3 2.4579(13) . ? Te3 Cl6 2.5329(13) . ? Te3 Cl10 2.8783(13) . ? Te3 Cl11 2.9081(14) . ? Te4 Cl7 2.3412(12) . ? Te4 Cl8 2.3575(13) . ? Te4 Cl9 2.3616(13) . ? Te4 Cl11 2.7814(13) . ? Te4 Cl10 2.7969(12) . ? Te4 Cl1 2.9232(13) . ? Te5 Cl12 2.3398(13) . ? Te5 Cl13 2.3452(13) . ? Te5 Cl14 2.3755(13) . ? Te5 Cl19 2.7319(13) . ? Te5 Cl20 2.8557(13) . ? Te5 Cl2 2.9121(13) . ? Te6 Cl17 2.3378(13) . ? Te6 Cl18 2.3840(13) . ? Te6 Cl15 2.4704(13) . ? Te6 Cl16 2.5141(13) . ? Te6 Cl20 2.8091(13) . ? Te6 Cl19 2.9560(13) . ? S1 C4 1.824(5) . ? S1 C3 1.859(5) . ? S2 C5 1.809(5) . ? S2 C6 1.849(5) . ? S3 C12 1.808(5) . ? S3 C11 1.844(5) . ? S4 C13 1.805(5) . ? S4 C14 1.851(5) . ? C1 C3 1.512(7) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.517(7) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3 1.0000 . ? C4 C5 1.508(7) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.524(7) . ? C6 C8 1.524(7) . ? C6 H6 1.0000 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C11 1.522(7) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.534(7) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11 1.0000 . ? C12 C13 1.533(7) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C16 1.508(7) . ? C14 C15 1.520(7) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 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 S1 Te1 S2 85.35(4) . . ? S1 Te1 Cl1 85.37(4) . . ? S2 Te1 Cl1 170.27(4) . . ? S4 Te2 Cl2 84.64(4) . . ? S4 Te2 S3 84.38(4) . . ? Cl2 Te2 S3 168.59(4) . . ? Cl5 Te3 Cl4 94.60(7) . . ? Cl5 Te3 Cl3 90.35(5) . . ? Cl4 Te3 Cl3 90.35(5) . . ? Cl5 Te3 Cl6 89.34(5) . . ? Cl4 Te3 Cl6 88.59(5) . . ? Cl3 Te3 Cl6 178.87(5) . . ? Cl5 Te3 Cl10 91.02(5) . . ? Cl4 Te3 Cl10 173.62(5) . . ? Cl3 Te3 Cl10 86.60(4) . . ? Cl6 Te3 Cl10 94.49(4) . . ? Cl5 Te3 Cl11 175.42(5) . . ? Cl4 Te3 Cl11 89.53(5) . . ? Cl3 Te3 Cl11 87.64(4) . . ? Cl6 Te3 Cl11 92.74(4) . . ? Cl10 Te3 Cl11 84.75(4) . . ? Cl7 Te4 Cl8 88.84(5) . . ? Cl7 Te4 Cl9 90.78(5) . . ? Cl8 Te4 Cl9 94.74(5) . . ? Cl7 Te4 Cl11 83.04(4) . . ? Cl8 Te4 Cl11 170.23(4) . . ? Cl9 Te4 Cl11 90.81(5) . . ? Cl7 Te4 Cl10 87.53(4) . . ? Cl8 Te4 Cl10 85.49(4) . . ? Cl9 Te4 Cl10 178.28(4) . . ? Cl11 Te4 Cl10 88.72(4) . . ? Cl7 Te4 Cl1 172.70(4) . . ? Cl8 Te4 Cl1 83.89(4) . . ? Cl9 Te4 Cl1 89.12(4) . . ? Cl11 Te4 Cl1 104.26(4) . . ? Cl10 Te4 Cl1 92.60(4) . . ? Cl12 Te5 Cl13 93.43(5) . . ? Cl12 Te5 Cl14 92.85(5) . . ? Cl13 Te5 Cl14 89.11(5) . . ? Cl12 Te5 Cl19 91.22(5) . . ? Cl13 Te5 Cl19 84.53(4) . . ? Cl14 Te5 Cl19 172.64(4) . . ? Cl12 Te5 Cl20 177.60(5) . . ? Cl13 Te5 Cl20 88.94(4) . . ? Cl14 Te5 Cl20 86.79(4) . . ? Cl19 Te5 Cl20 89.39(4) . . ? Cl12 Te5 Cl2 88.38(4) . . ? Cl13 Te5 Cl2 173.70(4) . . ? Cl14 Te5 Cl2 84.77(4) . . ? Cl19 Te5 Cl2 101.48(4) . . ? Cl20 Te5 Cl2 89.23(4) . . ? Cl17 Te6 Cl18 94.68(5) . . ? Cl17 Te6 Cl15 89.24(5) . . ? Cl18 Te6 Cl15 89.85(4) . . ? Cl17 Te6 Cl16 88.68(5) . . ? Cl18 Te6 Cl16 89.57(4) . . ? Cl15 Te6 Cl16 177.80(5) . . ? Cl17 Te6 Cl20 90.36(5) . . ? Cl18 Te6 Cl20 174.80(4) . . ? Cl15 Te6 Cl20 88.92(4) . . ? Cl16 Te6 Cl20 91.84(4) . . ? Cl17 Te6 Cl19 176.28(5) . . ? Cl18 Te6 Cl19 89.03(4) . . ? Cl15 Te6 Cl19 91.01(4) . . ? Cl16 Te6 Cl19 91.11(4) . . ? Cl20 Te6 Cl19 85.94(4) . . ? Te1 Cl1 Te4 91.16(4) . . ? Te2 Cl2 Te5 95.07(4) . . ? Te4 Cl10 Te3 93.23(4) . . ? Te4 Cl11 Te3 92.92(4) . . ? Te5 Cl19 Te6 91.77(4) . . ? Te6 Cl20 Te5 92.34(4) . . ? C4 S1 C3 103.6(2) . . ? C4 S1 Te1 100.31(16) . . ? C3 S1 Te1 105.02(16) . . ? C5 S2 C6 104.3(2) . . ? C5 S2 Te1 99.90(16) . . ? C6 S2 Te1 100.02(17) . . ? C12 S3 C11 104.0(2) . . ? C12 S3 Te2 100.53(16) . . ? C11 S3 Te2 100.50(16) . . ? C13 S4 C14 103.3(2) . . ? C13 S4 Te2 101.08(17) . . ? C14 S4 Te2 105.41(16) . . ? C3 C1 H1A 109.5 . . ? C3 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C3 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 H2A 109.5 . . ? C3 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C3 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 C2 113.5(5) . . ? C1 C3 S1 107.5(4) . . ? C2 C3 S1 107.3(3) . . ? C1 C3 H3 109.5 . . ? C2 C3 H3 109.5 . . ? S1 C3 H3 109.5 . . ? C5 C4 S1 114.5(3) . . ? C5 C4 H4A 108.6 . . ? S1 C4 H4A 108.6 . . ? C5 C4 H4B 108.6 . . ? S1 C4 H4B 108.6 . . ? H4A C4 H4B 107.6 . . ? C4 C5 S2 114.3(3) . . ? C4 C5 H5A 108.7 . . ? S2 C5 H5A 108.7 . . ? C4 C5 H5B 108.7 . . ? S2 C5 H5B 108.7 . . ? H5A C5 H5B 107.6 . . ? C7 C6 C8 113.3(4) . . ? C7 C6 S2 105.4(3) . . ? C8 C6 S2 109.9(4) . . ? C7 C6 H6 109.4 . . ? C8 C6 H6 109.4 . . ? S2 C6 H6 109.4 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C11 C9 H9A 109.5 . . ? C11 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C11 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 H10A 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C11 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 C10 111.8(4) . . ? C9 C11 S3 107.1(3) . . ? C10 C11 S3 109.4(4) . . ? C9 C11 H11 109.5 . . ? C10 C11 H11 109.5 . . ? S3 C11 H11 109.5 . . ? C13 C12 S3 113.9(3) . . ? C13 C12 H12A 108.8 . . ? S3 C12 H12A 108.8 . . ? C13 C12 H12B 108.8 . . ? S3 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? C12 C13 S4 114.2(3) . . ? C12 C13 H13A 108.7 . . ? S4 C13 H13A 108.7 . . ? C12 C13 H13B 108.7 . . ? S4 C13 H13B 108.7 . . ? H13A C13 H13B 107.6 . . ? C16 C14 C15 112.9(4) . . ? C16 C14 S4 108.8(3) . . ? C15 C14 S4 107.0(3) . . ? C16 C14 H14 109.4 . . ? C15 C14 H14 109.4 . . ? S4 C14 H14 109.4 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 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 S1 C4 C5 S2 60.7(5) . . . . ? S3 C12 C13 S4 59.7(4) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.899 _refine_diff_density_min -0.948 _refine_diff_density_rms 0.181 #===END OF CIF ============================================================== # 08mj65 data_08mj65 _database_code_depnum_ccdc_archive 'CCDC 711709' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2008-11-30 _audit_author_name 'Webster, M.' _chemical_name_systematic ; tetrachloro(1,2-bis(isopropylthio)ethane)tellurium(IV) ; # C8H18S2 = 1,2-bis(isopropylthio)ethane # 2-{[2-(isopropylthio)ethyl]thio}propane i-Lab IUPAC name of S2 ligand # 2,7-dimethyl-3,6-dithiaoctane # 2-(2-isopropylsulfanylethylsulfanyl)propane (from chemspider) # SMILES: S(C(C)C)CCSC(C)C CC(C)SCCSC(C)C _chemical_name_common tetrachloro(1,2-bis(isopropylthio)ethane)tellurium(IV) _chemical_melting_point ? _chemical_formula_moiety 'C8 H18 Cl4 S2 Te' _chemical_formula_sum 'C8 H18 Cl4 S2 Te' _chemical_formula_weight 447.74 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _space_group_IT_number 14 _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 9.0486(10) _cell_length_b 9.3392(10) _cell_length_c 19.5796(15) _cell_angle_alpha 90.00 _cell_angle_beta 99.207(6) _cell_angle_gamma 90.00 _cell_volume 1633.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 13941 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.821 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 2.704 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6682 # 0.6418 _exptl_absorpt_correction_T_max 0.7456 # 0.7553 _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18916 _diffrn_reflns_av_R_equivalents 0.0286 _diffrn_reflns_av_sigmaI/netI 0.0324 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.59 _diffrn_reflns_theta_max 27.51 _reflns_number_total 3670 _reflns_number_gt 3521 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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 'w=1/[\s^2^(Fo^2^)+(0.0591P)^2^+0.2517P] 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 3670 _refine_ls_number_parameters 136 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0318 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_ref 0.1099 _refine_ls_wR_factor_gt 0.1086 _refine_ls_goodness_of_fit_ref 1.443 _refine_ls_restrained_S_all 1.443 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Te1 Te 0.813028(18) 0.73671(2) 0.859587(9) 0.01435(11) Uani 1 1 d . . . Cl1 Cl 0.93378(8) 0.81136(9) 0.97285(3) 0.03015(19) Uani 1 1 d . . . Cl2 Cl 0.79741(9) 0.97862(8) 0.81239(4) 0.0329(2) Uani 1 1 d . . . Cl3 Cl 1.05711(7) 0.68339(8) 0.82021(3) 0.02167(17) Uani 1 1 d . . . Cl4 Cl 0.55702(10) 0.74652(8) 0.89357(5) 0.0306(2) Uani 1 1 d . . . S1 S 0.65096(6) 0.62479(7) 0.73351(3) 0.01848(17) Uani 1 1 d . . . S2 S 0.82753(7) 0.43938(7) 0.89006(3) 0.01898(16) Uani 1 1 d . . . C1 C 0.8096(5) 0.7606(3) 0.6488(2) 0.0317(8) Uani 1 1 d . . . H1A H 0.8458 0.8217 0.6886 0.047 Uiso 1 1 calc R . . H1B H 0.7140 0.7977 0.6247 0.047 Uiso 1 1 calc R . . H1C H 0.8831 0.7602 0.6170 0.047 Uiso 1 1 calc R . . C2 C 0.7326(3) 0.5085(3) 0.61365(14) 0.0234(6) Uani 1 1 d . . . H2A H 0.7202 0.4120 0.6316 0.035 Uiso 1 1 calc R . . H2B H 0.8057 0.5060 0.5817 0.035 Uiso 1 1 calc R . . H2C H 0.6362 0.5429 0.5891 0.035 Uiso 1 1 calc R . . C3 C 0.7879(3) 0.6089(3) 0.67342(13) 0.0189(5) Uani 1 1 d . . . H3 H 0.8849 0.5722 0.6991 0.023 Uiso 1 1 calc R . . C4 C 0.6253(3) 0.4438(3) 0.76324(14) 0.0278(6) Uani 1 1 d . . . H4A H 0.5468 0.4456 0.7932 0.033 Uiso 1 1 calc R . . H4B H 0.5877 0.3837 0.7225 0.033 Uiso 1 1 calc R . . C5 C 0.7637(4) 0.3730(3) 0.80300(15) 0.0302(7) Uani 1 1 d . . . H5A H 0.8465 0.3843 0.7759 0.036 Uiso 1 1 calc R . . H5B H 0.7435 0.2692 0.8060 0.036 Uiso 1 1 calc R . . C6 C 0.6745(3) 0.3947(3) 0.93765(13) 0.0180(5) Uani 1 1 d . . . H6 H 0.5799 0.4408 0.9145 0.022 Uiso 1 1 calc R . . C7 C 0.6522(4) 0.2337(3) 0.94037(18) 0.0262(7) Uani 1 1 d . . . H7A H 0.6234 0.1966 0.8933 0.039 Uiso 1 1 calc R . . H7B H 0.5731 0.2123 0.9677 0.039 Uiso 1 1 calc R . . H7C H 0.7458 0.1882 0.9619 0.039 Uiso 1 1 calc R . . C8 C 0.7195(3) 0.4591(3) 1.00938(13) 0.0235(6) Uani 1 1 d . . . H8A H 0.7324 0.5628 1.0053 0.035 Uiso 1 1 calc R . . H8B H 0.8139 0.4162 1.0316 0.035 Uiso 1 1 calc R . . H8C H 0.6412 0.4397 1.0374 0.035 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 0.01822(16) 0.01229(15) 0.01350(16) 0.00056(5) 0.00546(10) 0.00038(5) Cl1 0.0344(4) 0.0385(5) 0.0177(3) -0.0088(3) 0.0047(3) -0.0055(3) Cl2 0.0489(4) 0.0154(4) 0.0379(4) 0.0075(3) 0.0178(3) 0.0034(3) Cl3 0.0197(3) 0.0273(4) 0.0194(3) -0.0006(3) 0.0070(2) -0.0015(2) Cl4 0.0263(4) 0.0355(5) 0.0336(5) 0.0143(3) 0.0157(4) 0.0138(3) S1 0.0178(3) 0.0235(4) 0.0142(3) 0.0035(2) 0.0027(2) -0.0002(2) S2 0.0215(3) 0.0195(3) 0.0178(3) 0.0063(3) 0.0087(2) 0.0062(2) C1 0.046(2) 0.0262(17) 0.0254(17) 0.0019(11) 0.0134(16) -0.0147(12) C2 0.0255(13) 0.0246(14) 0.0204(13) -0.0022(11) 0.0048(10) -0.0007(11) C3 0.0194(11) 0.0236(13) 0.0144(11) 0.0024(10) 0.0049(9) -0.0029(10) C4 0.0420(16) 0.0276(15) 0.0137(11) -0.0008(11) 0.0041(11) -0.0195(13) C5 0.063(2) 0.0120(14) 0.0192(13) -0.0009(10) 0.0184(14) 0.0038(13) C6 0.0189(11) 0.0216(13) 0.0145(11) 0.0008(10) 0.0058(9) 0.0004(10) C7 0.0318(16) 0.0230(15) 0.0246(16) 0.0006(11) 0.0073(14) -0.0073(11) C8 0.0317(14) 0.0240(14) 0.0162(12) -0.0009(10) 0.0076(10) -0.0029(11) _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 Cl1 2.4129(7) . ? Te1 Cl2 2.4365(8) . ? Te1 Cl3 2.5030(7) . ? Te1 Cl4 2.5121(9) . ? Te1 S2 2.8388(7) . ? Te1 S1 2.8598(7) . ? S1 C4 1.814(3) . ? S1 C3 1.846(2) . ? S2 C5 1.819(3) . ? S2 C6 1.836(3) . ? C1 C3 1.520(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.520(4) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3 1.0000 . ? C4 C5 1.517(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.520(4) . ? C6 C8 1.522(4) . ? C6 H6 1.0000 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 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 Cl1 Te1 Cl2 94.06(3) . . ? Cl1 Te1 Cl3 92.77(2) . . ? Cl2 Te1 Cl3 93.91(3) . . ? Cl1 Te1 Cl4 92.70(3) . . ? Cl2 Te1 Cl4 93.82(3) . . ? Cl3 Te1 Cl4 170.18(3) . . ? Cl1 Te1 S2 95.20(2) . . ? Cl2 Te1 S2 169.95(2) . . ? Cl3 Te1 S2 81.76(2) . . ? Cl4 Te1 S2 89.63(2) . . ? Cl1 Te1 S1 173.31(2) . . ? Cl2 Te1 S1 91.20(2) . . ? Cl3 Te1 S1 90.99(2) . . ? Cl4 Te1 S1 82.81(3) . . ? S2 Te1 S1 79.86(2) . . ? C4 S1 C3 105.25(14) . . ? C4 S1 Te1 97.92(9) . . ? C3 S1 Te1 106.01(8) . . ? C5 S2 C6 104.26(14) . . ? C5 S2 Te1 98.00(10) . . ? C6 S2 Te1 108.39(9) . . ? C3 C1 H1A 109.5 . . ? C3 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C3 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 H2A 109.5 . . ? C3 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C3 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 C2 111.9(2) . . ? C1 C3 S1 105.2(2) . . ? C2 C3 S1 111.62(17) . . ? C1 C3 H3 109.3 . . ? C2 C3 H3 109.3 . . ? S1 C3 H3 109.3 . . ? C5 C4 S1 115.7(2) . . ? C5 C4 H4A 108.4 . . ? S1 C4 H4A 108.4 . . ? C5 C4 H4B 108.4 . . ? S1 C4 H4B 108.4 . . ? H4A C4 H4B 107.4 . . ? C4 C5 S2 116.4(2) . . ? C4 C5 H5A 108.2 . . ? S2 C5 H5A 108.2 . . ? C4 C5 H5B 108.2 . . ? S2 C5 H5B 108.2 . . ? H5A C5 H5B 107.3 . . ? C7 C6 C8 112.1(2) . . ? C7 C6 S2 111.0(2) . . ? C8 C6 S2 105.47(17) . . ? C7 C6 H6 109.4 . . ? C8 C6 H6 109.4 . . ? S2 C6 H6 109.4 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 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 S1 C4 C5 S2 72.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.806 _refine_diff_density_min -2.594 _refine_diff_density_rms 0.454 #===END OF CIF ============================================================== # 09mj06 data_09mj06 _database_code_depnum_ccdc_archive 'CCDC 721177' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2009-01-28 _audit_author_name 'Webster, M.' _chemical_name_systematic ; tetrabromo(1,2-bis(methylthio)ethane-S,S')tellurium(IV) ; # C4H10S2 ligand name # 2,5-dithiahexane # 1,2-bis(methylthio)ethane (I-Lab name) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H10 Br4 S2 Te' _chemical_formula_sum 'C4 H10 Br4 S2 Te' _chemical_formula_weight 569.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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' _space_group_IT_number 1 _space_group_name_Hall 'P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 7.0419(15) _cell_length_b 7.612(2) _cell_length_c 7.6259(15) _cell_angle_alpha 111.166(10) _cell_angle_beta 112.450(10) _cell_angle_gamma 98.639(15) _cell_volume 332.03(13) _cell_formula_units_Z 1 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 14156 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.848 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 258 _exptl_absorpt_coefficient_mu 14.540 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5695 # 0.2743 _exptl_absorpt_correction_T_max 1.0000 # 0.7597 _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6307 _diffrn_reflns_av_R_equivalents 0.0492 _diffrn_reflns_av_sigmaI/netI 0.0630 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.25 _diffrn_reflns_theta_max 27.58 _reflns_number_total 2606 _reflns_number_gt 2586 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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 'w=1/[\s^2^(Fo^2^)+(0.0420P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.074(7) _chemical_absolute_configuration ad _refine_ls_number_reflns 2606 _refine_ls_number_parameters 102 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0285 _refine_ls_R_factor_gt 0.0283 _refine_ls_wR_factor_ref 0.0723 _refine_ls_wR_factor_gt 0.0720 _refine_ls_goodness_of_fit_ref 0.968 _refine_ls_restrained_S_all 0.967 _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 0.34048(4) 0.76347(4) 0.61498(4) 0.01699(10) Uani 1 1 d . . . Br1 Br -0.04552(8) 0.79193(9) 0.48743(9) 0.02487(13) Uani 1 1 d . . . Br2 Br 0.48735(9) 0.97819(8) 0.45739(9) 0.02372(13) Uani 1 1 d . . . Br3 Br 0.20115(9) 0.41616(8) 0.26934(9) 0.03034(15) Uani 1 1 d . . . Br4 Br 0.48723(8) 1.07974(7) 0.99513(8) 0.02331(13) Uani 1 1 d . . . S1 S 0.7121(2) 0.6452(2) 0.7692(2) 0.0199(2) Uani 1 1 d . . . S2 S 0.2296(2) 0.5779(2) 0.8296(2) 0.0199(3) Uani 1 1 d . . . C1 C 0.9189(10) 0.8693(9) 1.0034(10) 0.0288(12) Uani 1 1 d . . . H1A H 0.8511 0.9422 1.0829 0.043 Uiso 1 1 calc R . . H1B H 0.9883 0.9545 0.9593 0.043 Uiso 1 1 calc R . . H1C H 1.0291 0.8322 1.0947 0.043 Uiso 1 1 calc R . . C2 C 0.6217(9) 0.4981(8) 0.8812(9) 0.0219(10) Uani 1 1 d . . . H2A H 0.5274 0.3623 0.7643 0.026 Uiso 1 1 calc R . . H2B H 0.7510 0.4847 0.9820 0.026 Uiso 1 1 calc R . . C3 C 0.4965(8) 0.5822(8) 0.9983(8) 0.0217(10) Uani 1 1 d . . . H3A H 0.5857 0.7221 1.1072 0.026 Uiso 1 1 calc R . . H3B H 0.4786 0.5048 1.0744 0.026 Uiso 1 1 calc R . . C4 C 0.0847(10) 0.3158(9) 0.6514(10) 0.0328(13) Uani 1 1 d . . . H4A H 0.1663 0.2607 0.5787 0.049 Uiso 1 1 calc R . . H4B H -0.0599 0.2981 0.5454 0.049 Uiso 1 1 calc R . . H4C H 0.0689 0.2457 0.7332 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 Te1 0.01702(15) 0.01626(16) 0.01652(15) 0.00711(11) 0.00757(11) 0.00458(11) Br1 0.0192(2) 0.0345(3) 0.0238(3) 0.0165(2) 0.0097(2) 0.0097(2) Br2 0.0275(2) 0.0223(3) 0.0241(3) 0.0106(2) 0.0157(2) 0.0058(2) Br3 0.0374(3) 0.0203(3) 0.0245(3) 0.0022(2) 0.0171(2) 0.0009(2) Br4 0.0292(3) 0.0183(2) 0.0203(3) 0.0071(2) 0.0116(2) 0.0073(2) S1 0.0183(5) 0.0216(6) 0.0209(6) 0.0096(5) 0.0106(5) 0.0064(5) S2 0.0183(5) 0.0208(6) 0.0226(6) 0.0114(5) 0.0104(5) 0.0061(5) C1 0.030(3) 0.022(3) 0.024(3) 0.004(2) 0.012(2) 0.002(2) C2 0.023(2) 0.025(3) 0.024(3) 0.016(2) 0.012(2) 0.009(2) C3 0.019(2) 0.025(2) 0.020(2) 0.011(2) 0.007(2) 0.008(2) C4 0.036(3) 0.026(3) 0.036(3) 0.014(3) 0.018(3) 0.007(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Te1 Br1 2.5867(8) . ? Te1 Br2 2.6542(8) . ? Te1 Br3 2.6669(9) . ? Te1 Br4 2.6818(9) . ? Te1 S2 2.7560(14) . ? Te1 S1 2.8571(14) . ? S1 C2 1.811(6) . ? S1 C1 1.813(6) . ? S2 C4 1.800(6) . ? S2 C3 1.815(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.531(8) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 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 Br1 Te1 Br2 97.11(2) . . ? Br1 Te1 Br3 91.76(3) . . ? Br2 Te1 Br3 94.19(3) . . ? Br1 Te1 Br4 91.21(3) . . ? Br2 Te1 Br4 93.58(3) . . ? Br3 Te1 Br4 171.27(2) . . ? Br1 Te1 S2 86.32(3) . . ? Br2 Te1 S2 172.61(3) . . ? Br3 Te1 S2 92.23(4) . . ? Br4 Te1 S2 79.77(4) . . ? Br1 Te1 S1 164.46(3) . . ? Br2 Te1 S1 97.79(3) . . ? Br3 Te1 S1 82.77(4) . . ? Br4 Te1 S1 92.25(4) . . ? S2 Te1 S1 79.40(4) . . ? C2 S1 C1 103.2(3) . . ? C2 S1 Te1 99.85(18) . . ? C1 S1 Te1 104.8(2) . . ? C4 S2 C3 103.2(3) . . ? C4 S2 Te1 109.5(2) . . ? C3 S2 Te1 99.69(18) . . ? S1 C1 H1A 109.5 . . ? S1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? S1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 S1 115.4(4) . . ? C3 C2 H2A 108.4 . . ? S1 C2 H2A 108.4 . . ? C3 C2 H2B 108.4 . . ? S1 C2 H2B 108.4 . . ? H2A C2 H2B 107.5 . . ? C2 C3 S2 115.1(4) . . ? C2 C3 H3A 108.5 . . ? S2 C3 H3A 108.5 . . ? C2 C3 H3B 108.5 . . ? S2 C3 H3B 108.5 . . ? H3A C3 H3B 107.5 . . ? S2 C4 H4A 109.5 . . ? S2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? S2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 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 # Br2 Te1 S2 C4 -157.2(3) . . . . ? # Br2 Te1 S2 C3 -49.4(3) . . . . ? Br1 Te1 S1 C2 -17.0(2) . . . . ? Br2 Te1 S1 C2 179.66(19) . . . . ? Br3 Te1 S1 C2 -87.08(19) . . . . ? Br4 Te1 S1 C2 85.73(19) . . . . ? S2 Te1 S1 C2 6.57(19) . . . . ? Br1 Te1 S1 C1 -123.5(2) . . . . ? Br2 Te1 S1 C1 73.1(2) . . . . ? Br3 Te1 S1 C1 166.4(2) . . . . ? Br4 Te1 S1 C1 -20.8(2) . . . . ? S2 Te1 S1 C1 -100.0(2) . . . . ? Br1 Te1 S2 C4 84.8(2) . . . . ? Br3 Te1 S2 C4 -6.8(2) . . . . ? Br4 Te1 S2 C4 176.7(2) . . . . ? S1 Te1 S2 C4 -89.1(2) . . . . ? Br1 Te1 S2 C3 -167.42(18) . . . . ? Br3 Te1 S2 C3 100.96(18) . . . . ? Br4 Te1 S2 C3 -75.52(18) . . . . ? S1 Te1 S2 C3 18.74(17) . . . . ? C1 S1 C2 C3 68.3(5) . . . . ? Te1 S1 C2 C3 -39.5(4) . . . . ? S1 C2 C3 S2 68.3(5) . . . . ? C4 S2 C3 C2 61.1(5) . . . . ? Te1 S2 C3 C2 -51.8(4) . . . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 1.032 _refine_diff_density_min -0.895 _refine_diff_density_rms 0.156 #===END OF CIF ============================================================== # 09mj05 data_09mj05 _database_code_depnum_ccdc_archive 'CCDC 721178' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2009-01-27 _audit_author_name 'Webster, M.' _chemical_name_systematic ; tetrabromo(1,2-bis(isopropylthio)ethane-S,S')tellurium(IV) ; # Sulphur ligand name: # 1,2-bis(isopropylthio)ethane # 2-{[2-(isopropylthio)ethyl]thio}propane (i-Lab IUPAC name) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H18 Br4 S2 Te' _chemical_formula_sum 'C8 H18 Br4 S2 Te' _chemical_formula_weight 625.58 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' Br Br -0.2901 2.4595 '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' _space_group_IT_number 14 _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 7.535(2) _cell_length_b 15.212(4) _cell_length_c 15.222(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.486(15) _cell_angle_gamma 90.00 _cell_volume 1739.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 38716 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.389 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1160 _exptl_absorpt_coefficient_mu 11.113 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6161 # _exptl_absorpt_correction_T_max 1.0000 # _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17593 _diffrn_reflns_av_R_equivalents 0.0661 _diffrn_reflns_av_sigmaI/netI 0.0541 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.66 _diffrn_reflns_theta_max 27.57 _reflns_number_total 3962 _reflns_number_gt 3081 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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 'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+17.1893P] 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 3962 _refine_ls_number_parameters 140 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0735 _refine_ls_R_factor_gt 0.0472 _refine_ls_wR_factor_ref 0.1003 _refine_ls_wR_factor_gt 0.0882 _refine_ls_goodness_of_fit_ref 1.134 _refine_ls_restrained_S_all 1.134 _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 0.12622(6) 0.17440(3) 0.74400(3) 0.02137(12) Uani 1 1 d . . . Br1 Br -0.04880(13) 0.07524(6) 0.85153(5) 0.0429(2) Uani 1 1 d . . . Br2 Br 0.43112(11) 0.16045(5) 0.83420(5) 0.0352(2) Uani 1 1 d . . . Br3 Br 0.03231(11) 0.32608(5) 0.81587(5) 0.02935(18) Uani 1 1 d . . . Br4 Br 0.19602(10) 0.04269(5) 0.63574(5) 0.02843(18) Uani 1 1 d . . . S1 S 0.3033(2) 0.26547(12) 0.62126(11) 0.0231(4) Uani 1 1 d . . . S2 S -0.1705(2) 0.22024(13) 0.62569(11) 0.0260(4) Uani 1 1 d . . . C1 C 0.4750(11) 0.3852(6) 0.7298(5) 0.0364(19) Uani 1 1 d . . . H1A H 0.5860 0.3581 0.7138 0.055 Uiso 1 1 calc R . . H1B H 0.4306 0.3533 0.7795 0.055 Uiso 1 1 calc R . . H1C H 0.4974 0.4467 0.7465 0.055 Uiso 1 1 calc R . . C2 C 0.3969(14) 0.4308(5) 0.5728(5) 0.042(2) Uani 1 1 d . . . H2A H 0.4287 0.4911 0.5903 0.063 Uiso 1 1 calc R . . H2B H 0.3002 0.4319 0.5259 0.063 Uiso 1 1 calc R . . H2C H 0.5009 0.4014 0.5514 0.063 Uiso 1 1 calc R . . C3 C 0.3368(11) 0.3814(5) 0.6513(5) 0.0268(16) Uani 1 1 d . . . H3 H 0.2221 0.4069 0.6684 0.032 Uiso 1 1 calc R . . C4 C 0.1244(10) 0.2697(5) 0.5339(5) 0.0311(18) Uani 1 1 d . . . H4A H 0.1603 0.3102 0.4876 0.037 Uiso 1 1 calc R . . H4B H 0.1106 0.2105 0.5073 0.037 Uiso 1 1 calc R . . C5 C -0.0559(10) 0.2991(5) 0.5617(5) 0.0310(17) Uani 1 1 d . . . H5A H -0.1332 0.3135 0.5081 0.037 Uiso 1 1 calc R . . H5B H -0.0390 0.3538 0.5966 0.037 Uiso 1 1 calc R . . C6 C -0.2219(10) 0.1298(5) 0.5479(5) 0.0278(16) Uani 1 1 d . . . H6 H -0.1094 0.1089 0.5239 0.033 Uiso 1 1 calc R . . C7 C -0.3506(10) 0.1617(5) 0.4721(5) 0.0327(18) Uani 1 1 d . . . H7A H -0.3827 0.1124 0.4325 0.049 Uiso 1 1 calc R . . H7B H -0.2934 0.2079 0.4393 0.049 Uiso 1 1 calc R . . H7C H -0.4582 0.1853 0.4957 0.049 Uiso 1 1 calc R . . C8 C -0.2995(10) 0.0565(5) 0.6010(5) 0.0337(18) Uani 1 1 d . . . H8A H -0.4072 0.0776 0.6264 0.051 Uiso 1 1 calc R . . H8B H -0.2118 0.0383 0.6484 0.051 Uiso 1 1 calc R . . H8C H -0.3296 0.0062 0.5623 0.051 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 0.0253(2) 0.0214(2) 0.0170(2) -0.00009(18) -0.00091(17) -0.00032(19) Br1 0.0636(6) 0.0377(5) 0.0287(4) -0.0033(3) 0.0121(4) -0.0218(4) Br2 0.0364(4) 0.0310(4) 0.0355(4) 0.0018(3) -0.0141(3) 0.0002(3) Br3 0.0397(4) 0.0263(4) 0.0226(3) -0.0028(3) 0.0059(3) 0.0027(3) Br4 0.0276(4) 0.0250(4) 0.0322(4) -0.0059(3) -0.0014(3) 0.0029(3) S1 0.0245(9) 0.0239(9) 0.0212(8) -0.0025(7) 0.0032(7) -0.0008(7) S2 0.0246(9) 0.0303(10) 0.0228(8) -0.0020(7) -0.0005(7) 0.0009(8) C1 0.041(5) 0.034(4) 0.033(4) -0.012(4) -0.001(4) -0.003(4) C2 0.071(6) 0.028(4) 0.029(4) -0.001(3) 0.013(4) -0.014(4) C3 0.036(4) 0.021(4) 0.025(3) -0.003(3) 0.009(3) -0.003(3) C4 0.037(4) 0.035(4) 0.022(4) -0.002(3) 0.000(3) -0.017(4) C5 0.028(4) 0.031(4) 0.033(4) 0.013(3) -0.005(3) -0.002(3) C6 0.028(4) 0.033(4) 0.022(3) 0.001(3) 0.004(3) 0.000(3) C7 0.029(4) 0.041(5) 0.026(4) -0.009(3) -0.006(3) 0.008(4) C8 0.026(4) 0.036(4) 0.039(4) -0.002(4) 0.000(3) -0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Te1 Br2 2.5914(11) . ? Te1 Br1 2.6517(10) . ? Te1 Br4 2.6724(9) . ? Te1 Br3 2.6725(10) . ? Te1 S1 2.7532(18) . ? Te1 S2 2.8459(19) . ? S1 C4 1.819(8) . ? S1 C3 1.834(7) . ? S2 C5 1.807(7) . ? S2 C6 1.836(8) . ? C1 C3 1.524(11) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.510(10) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3 1.0000 . ? C4 C5 1.521(11) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C8 1.522(11) . ? C6 C7 1.527(10) . ? C6 H6 1.0000 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 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 Br2 Te1 Br1 95.13(4) . . ? Br2 Te1 Br4 93.23(3) . . ? Br1 Te1 Br4 94.91(3) . . ? Br2 Te1 Br3 96.08(3) . . ? Br1 Te1 Br3 94.47(3) . . ? Br4 Te1 Br3 166.13(3) . . ? Br2 Te1 S1 86.80(5) . . ? Br1 Te1 S1 174.84(4) . . ? Br4 Te1 S1 80.19(4) . . ? Br3 Te1 S1 90.07(4) . . ? Br2 Te1 S2 167.29(5) . . ? Br1 Te1 S2 97.24(5) . . ? Br4 Te1 S2 88.64(4) . . ? Br3 Te1 S2 80.06(4) . . ? S1 Te1 S2 81.13(6) . . ? C4 S1 C3 103.2(4) . . ? C4 S1 Te1 98.2(2) . . ? C3 S1 Te1 112.3(2) . . ? C5 S2 C6 103.6(4) . . ? C5 S2 Te1 96.8(2) . . ? C6 S2 Te1 109.9(3) . . ? C3 C1 H1A 109.5 . . ? C3 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C3 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 H2A 109.5 . . ? C3 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C3 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C2 C3 C1 111.8(7) . . ? C2 C3 S1 109.0(5) . . ? C1 C3 S1 107.7(5) . . ? C2 C3 H3 109.4 . . ? C1 C3 H3 109.4 . . ? S1 C3 H3 109.4 . . ? C5 C4 S1 115.7(5) . . ? C5 C4 H4A 108.3 . . ? S1 C4 H4A 108.3 . . ? C5 C4 H4B 108.3 . . ? S1 C4 H4B 108.3 . . ? H4A C4 H4B 107.4 . . ? C4 C5 S2 115.4(5) . . ? C4 C5 H5A 108.4 . . ? S2 C5 H5A 108.4 . . ? C4 C5 H5B 108.4 . . ? S2 C5 H5B 108.4 . . ? H5A C5 H5B 107.5 . . ? C8 C6 C7 112.7(7) . . ? C8 C6 S2 106.1(5) . . ? C7 C6 S2 109.8(5) . . ? C8 C6 H6 109.4 . . ? C7 C6 H6 109.4 . . ? S2 C6 H6 109.4 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 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 # Br1 Te1 S1 C4 58.1(6) . . . . ? # Br1 Te1 S1 C3 166.0(5) . . . . ? Br2 Te1 S1 C4 170.2(3) . . . . ? Br4 Te1 S1 C4 76.4(3) . . . . ? Br3 Te1 S1 C4 -93.7(3) . . . . ? S2 Te1 S1 C4 -13.8(3) . . . . ? Br2 Te1 S1 C3 -81.8(3) . . . . ? Br4 Te1 S1 C3 -175.7(3) . . . . ? Br3 Te1 S1 C3 14.2(3) . . . . ? S2 Te1 S1 C3 94.2(3) . . . . ? Br2 Te1 S2 C5 6.2(4) . . . . ? Br1 Te1 S2 C5 172.7(3) . . . . ? Br4 Te1 S2 C5 -92.5(3) . . . . ? Br3 Te1 S2 C5 79.4(3) . . . . ? S1 Te1 S2 C5 -12.2(3) . . . . ? Br2 Te1 S2 C6 113.3(3) . . . . ? Br1 Te1 S2 C6 -80.1(3) . . . . ? Br4 Te1 S2 C6 14.7(3) . . . . ? Br3 Te1 S2 C6 -173.4(3) . . . . ? S1 Te1 S2 C6 95.0(3) . . . . ? C4 S1 C3 C2 -63.0(7) . . . . ? Te1 S1 C3 C2 -167.7(5) . . . . ? C4 S1 C3 C1 175.5(5) . . . . ? Te1 S1 C3 C1 70.8(5) . . . . ? C3 S1 C4 C5 -67.0(6) . . . . ? Te1 S1 C4 C5 48.3(6) . . . . ? S1 C4 C5 S2 -72.5(7) . . . . ? C6 S2 C5 C4 -66.3(6) . . . . ? Te1 S2 C5 C4 46.1(6) . . . . ? C5 S2 C6 C8 173.6(5) . . . . ? Te1 S2 C6 C8 71.0(5) . . . . ? C5 S2 C6 C7 -64.4(6) . . . . ? Te1 S2 C6 C7 -166.9(5) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.57 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.946 _refine_diff_density_min -1.074 _refine_diff_density_rms 0.219 #===END OF CIF ============================================================== # 08mj67 data_08mj67 _database_code_depnum_ccdc_archive 'CCDC 721179' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2009-01-13 _audit_author_name 'Webster, M.' _chemical_name_systematic ; bis(trichloro(\m~2~-chloro)(dimethylsulfide-S)tellurium(IV)) ; # hexachloro-di(\m~2~-chloro)bis(dimethylsulfide-S)ditellurium(IV) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H12 Cl8 S2 Te2' _chemical_formula_sum 'C4 H12 Cl8 S2 Te2' _chemical_formula_weight 663.06 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' Cl Cl 0.1484 0.1585 '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' _space_group_IT_number 14 _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 7.338(3) _cell_length_b 12.998(5) _cell_length_c 9.945(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.89(3) _cell_angle_gamma 90.00 _cell_volume 920.8(6) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 52591 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.392 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 616 _exptl_absorpt_coefficient_mu 4.531 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7001 # 0.7132 _exptl_absorpt_correction_T_max 1.0000 # 0.9148 _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15850 _diffrn_reflns_av_R_equivalents 0.0799 _diffrn_reflns_av_sigmaI/netI 0.0468 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 27.65 _reflns_number_total 2143 _reflns_number_gt 1584 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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 'w=1/[\s^2^(Fo^2^)+(0.0075P)^2^+7.7774P] 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 2143 _refine_ls_number_parameters 75 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0730 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.0923 _refine_ls_wR_factor_gt 0.0798 _refine_ls_goodness_of_fit_ref 1.130 _refine_ls_restrained_S_all 1.130 _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 0.16783(5) 0.00095(4) 0.20145(4) 0.02328(13) Uani 1 1 d . . . Cl1 Cl 0.2134(2) 0.12580(14) 0.37738(18) 0.0335(4) Uani 1 1 d . . . Cl2 Cl 0.3893(2) -0.11542(14) 0.33130(19) 0.0335(4) Uani 1 1 d . . . Cl3 Cl -0.0780(2) -0.07648(14) 0.29171(19) 0.0329(4) Uani 1 1 d . . . Cl4 Cl 0.0804(2) -0.13736(13) -0.02627(19) 0.0311(4) Uani 1 1 d . . . S1 S 0.4990(2) 0.07487(13) 0.14018(18) 0.0269(4) Uani 1 1 d . . . C1 C 0.4176(10) 0.1812(5) 0.0268(8) 0.0329(16) Uani 1 1 d . . . H1A H 0.3420 0.2271 0.0698 0.049 Uiso 1 1 calc R . . H1B H 0.3407 0.1555 -0.0614 0.049 Uiso 1 1 calc R . . H1C H 0.5254 0.2190 0.0100 0.049 Uiso 1 1 calc R . . C2 C 0.6291(10) 0.1405(6) 0.2920(7) 0.0332(16) Uani 1 1 d . . . H2A H 0.7415 0.1718 0.2724 0.050 Uiso 1 1 calc R . . H2B H 0.6664 0.0912 0.3682 0.050 Uiso 1 1 calc R . . H2C H 0.5505 0.1942 0.3181 0.050 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 0.0229(2) 0.0215(2) 0.0245(2) 0.00042(19) 0.00390(15) 0.00045(19) Cl1 0.0338(9) 0.0337(10) 0.0334(9) -0.0085(7) 0.0086(8) -0.0010(7) Cl2 0.0293(8) 0.0337(10) 0.0357(9) 0.0096(7) 0.0044(7) 0.0040(7) Cl3 0.0305(8) 0.0326(9) 0.0375(9) 0.0038(8) 0.0120(7) 0.0004(7) Cl4 0.0327(9) 0.0247(8) 0.0369(9) 0.0007(7) 0.0101(7) 0.0032(7) S1 0.0282(8) 0.0251(8) 0.0280(9) -0.0024(7) 0.0076(7) 0.0007(7) C1 0.027(3) 0.032(4) 0.038(4) -0.001(3) 0.005(3) 0.000(3) C2 0.029(4) 0.038(4) 0.030(4) -0.005(3) 0.004(3) 0.000(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Te1 Cl1 2.3507(19) . ? Te1 Cl2 2.3641(19) . ? Te1 Cl3 2.4183(19) . ? Te1 S1 2.813(2) . ? Te1 Cl4 2.8239(19) 3 ? Te1 Cl4 2.842(2) . ? Cl4 Te1 2.8239(19) 3 ? S1 C1 1.793(7) . ? S1 C2 1.796(7) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 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 Cl1 Te1 Cl2 94.53(7) . . ? Cl1 Te1 Cl3 89.80(7) . . ? Cl2 Te1 Cl3 90.41(7) . . ? Cl1 Te1 S1 87.11(6) . . ? Cl2 Te1 S1 79.66(6) . . ? Cl3 Te1 S1 169.32(6) . . ? Cl1 Te1 Cl4 88.91(7) . 3 ? Cl2 Te1 Cl4 174.76(6) . 3 ? Cl3 Te1 Cl4 93.56(6) . 3 ? S1 Te1 Cl4 96.59(6) . 3 ? Cl1 Te1 Cl4 173.99(6) . . ? Cl2 Te1 Cl4 91.41(7) . . ? Cl3 Te1 Cl4 89.24(6) . . ? S1 Te1 Cl4 94.87(5) . . ? Cl4 Te1 Cl4 85.23(6) 3 . ? Te1 Cl4 Te1 94.77(6) 3 . ? C1 S1 C2 101.1(4) . . ? C1 S1 Te1 103.0(2) . . ? C2 S1 Te1 107.0(2) . . ? S1 C1 H1A 109.5 . . ? S1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? S1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? S1 C2 H2A 109.5 . . ? S1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? S1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.65 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.278 _refine_diff_density_min -1.033 _refine_diff_density_rms 0.200 #===END OF CIF ============================================================== # 09mj03 data_09mj03 _database_code_depnum_ccdc_archive 'CCDC 721180' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2009-01-28 _audit_author_name 'Webster, M.' _chemical_name_systematic ; bis(tribromo(\m~2~-bromo)(dimethylsulfide-S)tellurium(IV)) ; # hexabromo-di(\m~2~-bromo)bis(dimethylsulfide-S)ditellurium(IV) # S ligand: methylsulfanylmethane (chemspider) # (methylthio)methane (ACD iLab) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H12 Br8 S2 Te2' _chemical_formula_sum 'C4 H12 Br8 S2 Te2' _chemical_formula_weight 1018.74 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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' _space_group_IT_number 14 _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 7.5223(10) _cell_length_b 13.462(2) _cell_length_c 10.4791(15) _cell_angle_alpha 90.00 _cell_angle_beta 104.490(10) _cell_angle_gamma 90.00 _cell_volume 1027.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 13110 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.293 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 18.578 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4624 # 0.3180 _exptl_absorpt_correction_T_max 1.0000 # 0.5236 _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11501 _diffrn_reflns_av_R_equivalents 0.0692 _diffrn_reflns_av_sigmaI/netI 0.0461 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.53 _reflns_number_total 2353 _reflns_number_gt 2068 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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 'w=1/[\s^2^(Fo^2^)+(0.0228P)^2^+15.5098P] 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 2353 _refine_ls_number_parameters 75 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0491 _refine_ls_R_factor_gt 0.0407 _refine_ls_wR_factor_ref 0.0960 _refine_ls_wR_factor_gt 0.0900 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _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 0.66032(6) 0.00529(3) 0.20625(4) 0.01511(14) Uani 1 1 d . . . Br1 Br 0.69605(11) 0.14530(5) 0.37044(7) 0.02277(19) Uani 1 1 d . . . Br2 Br 0.90356(10) -0.10594(6) 0.34752(8) 0.02309(19) Uani 1 1 d . . . Br3 Br 0.40666(11) -0.07680(6) 0.29890(8) 0.02445(19) Uani 1 1 d . . . Br4 Br 0.59945(10) -0.13454(5) -0.02000(7) 0.01997(18) Uani 1 1 d . . . S1 S 0.9766(3) 0.07608(13) 0.13688(18) 0.0200(4) Uani 1 1 d . . . C1 C 0.8960(11) 0.1783(6) 0.0285(8) 0.0265(17) Uani 1 1 d . . . H1A H 0.8261 0.2240 0.0703 0.040 Uiso 1 1 calc R . . H1B H 0.8167 0.1535 -0.0542 0.040 Uiso 1 1 calc R . . H1C H 1.0010 0.2135 0.0102 0.040 Uiso 1 1 calc R . . C2 C 1.1096(12) 0.1415(6) 0.2790(8) 0.0275(17) Uani 1 1 d . . . H2A H 1.2165 0.1722 0.2574 0.041 Uiso 1 1 calc R . . H2B H 1.1509 0.0947 0.3520 0.041 Uiso 1 1 calc R . . H2C H 1.0336 0.1932 0.3048 0.041 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 0.0169(2) 0.0126(2) 0.0155(2) 0.00045(16) 0.00344(17) 0.00069(16) Br1 0.0261(4) 0.0206(4) 0.0214(4) -0.0068(3) 0.0056(3) 0.0010(3) Br2 0.0219(4) 0.0214(4) 0.0240(4) 0.0060(3) 0.0020(3) 0.0039(3) Br3 0.0247(4) 0.0223(4) 0.0287(4) 0.0036(3) 0.0113(3) -0.0007(3) Br4 0.0232(4) 0.0159(3) 0.0201(4) 0.0005(3) 0.0041(3) 0.0041(3) S1 0.0223(9) 0.0182(8) 0.0203(9) -0.0015(7) 0.0070(7) -0.0005(7) C1 0.020(4) 0.023(4) 0.033(4) 0.010(3) 0.001(3) -0.003(3) C2 0.028(4) 0.031(4) 0.025(4) -0.005(3) 0.008(3) -0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Te1 Br1 2.5206(9) . ? Te1 Br2 2.5349(9) . ? Te1 Br3 2.5945(9) . ? Te1 S1 2.8216(19) . ? Te1 Br4 2.9575(9) 3_655 ? Te1 Br4 2.9717(9) . ? Br4 Te1 2.9575(9) 3_655 ? S1 C1 1.791(8) . ? S1 C2 1.802(8) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 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 Br1 Te1 Br2 96.03(3) . . ? Br1 Te1 Br3 91.48(3) . . ? Br2 Te1 Br3 91.19(3) . . ? Br1 Te1 S1 88.31(4) . . ? Br2 Te1 S1 79.52(4) . . ? Br3 Te1 S1 170.63(5) . . ? Br1 Te1 Br4 87.16(3) . 3_655 ? Br2 Te1 Br4 173.77(3) . 3_655 ? Br3 Te1 Br4 94.08(3) . 3_655 ? S1 Te1 Br4 95.26(4) . 3_655 ? Br1 Te1 Br4 170.77(3) . . ? Br2 Te1 Br4 92.08(3) . . ? Br3 Te1 Br4 92.74(3) . . ? S1 Te1 Br4 88.85(4) . . ? Br4 Te1 Br4 84.36(3) 3_655 . ? Te1 Br4 Te1 95.64(3) 3_655 . ? C1 S1 C2 100.3(4) . . ? C1 S1 Te1 104.4(3) . . ? C2 S1 Te1 106.4(3) . . ? S1 C1 H1A 109.5 . . ? S1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? S1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? S1 C2 H2A 109.5 . . ? S1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? S1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.152 _refine_diff_density_min -1.383 _refine_diff_density_rms 0.282 #===END OF CIF ============================================================== # 09mj04 data_09mj04 _database_code_depnum_ccdc_archive 'CCDC 721181' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2009-01-29 _audit_author_name 'Webster, M.' _chemical_name_systematic ; bis(tribromo(\m~2~-bromo)(dimethylsulfide-S)tellurium(IV)) ; # hexabromo-di(\m~2~-bromo)bis(dimethylsulfide-S)ditellurium(IV) # S ligand: methylsulfanylmethane (chemspider) # (methylthio)methane (ACD iLab) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H12 Br8 S2 Te2' _chemical_formula_sum 'C4 H12 Br8 S2 Te2' _chemical_formula_weight 1018.74 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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' _space_group_IT_number 2 _space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.5448(15) _cell_length_b 8.6401(15) _cell_length_c 8.9222(15) _cell_angle_alpha 73.688(10) _cell_angle_beta 84.565(15) _cell_angle_gamma 66.683(10) _cell_volume 512.53(16) _cell_formula_units_Z 1 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6120 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.301 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 452 _exptl_absorpt_coefficient_mu 18.621 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3459 # _exptl_absorpt_correction_T_max 1.0000 # _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7711 _diffrn_reflns_av_R_equivalents 0.0727 _diffrn_reflns_av_sigmaI/netI 0.0775 _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 -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 27.78 _reflns_number_total 2343 _reflns_number_gt 1827 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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 'w=1/[\s^2^(Fo^2^)+(0.0923P)^2^+23.9982P] 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 2343 _refine_ls_number_parameters 75 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1041 _refine_ls_R_factor_gt 0.0716 _refine_ls_wR_factor_ref 0.2011 _refine_ls_wR_factor_gt 0.1749 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _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 0.16462(13) 0.27947(13) 0.68996(11) 0.0168(3) Uani 1 1 d . . . Br1 Br 0.1252(2) 0.2341(2) 0.98317(19) 0.0279(4) Uani 1 1 d . . . Br2 Br 0.4749(2) 0.0137(2) 0.70958(19) 0.0229(4) Uani 1 1 d . . . Br3 Br -0.0357(2) 0.0997(2) 0.6789(2) 0.0261(4) Uani 1 1 d . . . Br4 Br 0.1802(2) 0.3836(2) 0.34658(18) 0.0218(4) Uani 1 1 d . . . S1 S 0.4394(5) 0.4221(5) 0.7023(4) 0.0201(8) Uani 1 1 d . . . C1 C 0.296(3) 0.642(2) 0.720(2) 0.034(4) Uani 1 1 d . . . H1A H 0.1970 0.6384 0.7987 0.051 Uiso 1 1 calc R . . H1B H 0.2344 0.7172 0.6192 0.051 Uiso 1 1 calc R . . H1C H 0.3804 0.6899 0.7522 0.051 Uiso 1 1 calc R . . C2 C 0.549(3) 0.321(2) 0.894(2) 0.033(4) Uani 1 1 d . . . H2A H 0.6437 0.3684 0.9053 0.049 Uiso 1 1 calc R . . H2B H 0.6138 0.1942 0.9083 0.049 Uiso 1 1 calc R . . H2C H 0.4493 0.3442 0.9727 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 Te1 0.0161(5) 0.0146(5) 0.0185(5) -0.0033(4) -0.0009(3) -0.0053(4) Br1 0.0256(8) 0.0345(10) 0.0213(8) -0.0060(7) 0.0009(6) -0.0103(7) Br2 0.0188(7) 0.0169(8) 0.0286(8) -0.0055(6) -0.0027(6) -0.0022(6) Br3 0.0250(8) 0.0240(9) 0.0332(9) -0.0063(7) -0.0003(6) -0.0140(7) Br4 0.0190(7) 0.0213(8) 0.0235(8) -0.0067(6) 0.0022(6) -0.0059(6) S1 0.0198(17) 0.020(2) 0.0214(18) -0.0052(15) -0.0015(14) -0.0079(15) C1 0.038(10) 0.021(9) 0.043(11) 0.000(8) 0.002(8) -0.018(8) C2 0.029(9) 0.027(10) 0.033(10) -0.007(8) -0.004(7) -0.001(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 Br2 2.5259(18) . ? Te1 Br1 2.5406(19) . ? Te1 Br3 2.5845(18) . ? Te1 S1 2.823(4) . ? Te1 Br4 2.9457(19) . ? Te1 Br4 2.9968(19) 2_566 ? Br4 Te1 2.9968(19) 2_566 ? S1 C2 1.797(18) . ? S1 C1 1.823(19) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 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 Br2 Te1 Br1 95.02(6) . . ? Br2 Te1 Br3 90.99(6) . . ? Br1 Te1 Br3 92.48(6) . . ? Br2 Te1 S1 79.11(9) . . ? Br1 Te1 S1 89.00(9) . . ? Br3 Te1 S1 170.08(10) . . ? Br2 Te1 Br4 91.98(6) . . ? Br1 Te1 Br4 172.11(6) . . ? Br3 Te1 Br4 91.01(6) . . ? S1 Te1 Br4 88.77(9) . . ? Br2 Te1 Br4 174.29(6) . 2_566 ? Br1 Te1 Br4 87.14(6) . 2_566 ? Br3 Te1 Br4 94.19(6) . 2_566 ? S1 Te1 Br4 95.68(9) . 2_566 ? Br4 Te1 Br4 85.55(5) . 2_566 ? Te1 Br4 Te1 94.45(5) . 2_566 ? C2 S1 C1 100.2(9) . . ? C2 S1 Te1 106.2(7) . . ? C1 S1 Te1 104.6(6) . . ? S1 C1 H1A 109.5 . . ? S1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? S1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? S1 C2 H2A 109.5 . . ? S1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? S1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 27.78 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 1.991 _refine_diff_density_min -2.307 _refine_diff_density_rms 0.500 #===END OF CIF ============================================================== # # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set. # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # #===END OF FILE =============================================================