# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_11ajj0001 _database_code_depnum_ccdc_archive 'CCDC 881025' #TrackingRef '- Te_all15_3.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2011-12-24 _audit_author_name 'Webster, M.' _chemical_name_systematic ; Tetrachloro-(1,2-bis(methylsulfanyl)benzene)tellurium(IV) ; # o-C6H4(SMe)2 = C8H10S2 # 1,2-bis(methylthio)benzene (iLab defaults) # 1,2-bis(methylsulfanyl)benzene (iLab selected options & chemspider) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H10 S2, Cl4 Te' _chemical_formula_sum 'C8 H10 Cl4 S2 Te' _chemical_formula_weight 439.68 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 orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _space_group_IT_number 33 _space_group_name_Hall 'P 2c -2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 10.038(2) _cell_length_b 14.622(2) _cell_length_c 9.5760(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1405.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 31232 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.078 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 840 _exptl_absorpt_coefficient_mu 3.140 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8122 # Expt'l Tmin & Tmax _exptl_absorpt_correction_T_max 1.0000 # scaled to Tmax=1.0 _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 APEX II 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 16155 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_sigmaI/netI 0.0298 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.25 _diffrn_reflns_theta_max 27.49 _reflns_number_total 3181 _reflns_number_gt 3067 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997)' _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^+1.0145P] 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' _chemical_absolute_configuration ad _refine_ls_abs_structure_Flack 0.075(16) _refine_ls_number_reflns 3181 _refine_ls_number_parameters 138 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0218 _refine_ls_R_factor_gt 0.0201 _refine_ls_wR_factor_ref 0.0391 _refine_ls_wR_factor_gt 0.0385 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _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 0.738431(14) 0.565913(9) 0.23210(4) 0.01609(5) Uani 1 1 d . . . Cl1 Cl 0.92341(7) 0.67373(5) 0.21929(11) 0.03304(18) Uani 1 1 d . . . Cl2 Cl 0.61822(9) 0.64980(6) 0.06463(9) 0.02835(19) Uani 1 1 d . . . Cl3 Cl 0.54587(7) 0.45643(5) 0.25720(9) 0.02807(18) Uani 1 1 d . . . Cl4 Cl 0.64390(7) 0.65307(6) 0.41199(8) 0.02368(18) Uani 1 1 d . . . S1 S 0.82787(7) 0.46033(5) -0.02713(8) 0.02030(15) Uani 1 1 d . . . S2 S 1.11608(7) 0.52372(5) -0.02577(8) 0.02057(15) Uani 1 1 d . . . C1 C 0.6944(3) 0.3800(2) -0.0548(3) 0.0258(7) Uani 1 1 d . . . H1A H 0.6535 0.3645 0.0351 0.039 Uiso 1 1 calc R . . H1B H 0.7297 0.3245 -0.0983 0.039 Uiso 1 1 calc R . . H1C H 0.6272 0.4075 -0.1161 0.039 Uiso 1 1 calc R . . C2 C 0.9417(3) 0.40025(19) 0.0810(3) 0.0183(6) Uani 1 1 d . . . C3 C 0.9040(3) 0.3258(2) 0.1636(3) 0.0240(6) Uani 1 1 d . . . H3 H 0.8165 0.3015 0.1557 0.029 Uiso 1 1 calc R . . C4 C 0.9930(3) 0.28735(18) 0.2565(3) 0.0230(7) Uani 1 1 d . . . H4 H 0.9668 0.2367 0.3122 0.028 Uiso 1 1 calc R . . C5 C 1.1207(3) 0.32283(19) 0.2683(3) 0.0247(7) Uani 1 1 d . . . H5 H 1.1811 0.2973 0.3340 0.030 Uiso 1 1 calc R . . C6 C 1.1608(3) 0.39510(19) 0.1852(3) 0.0202(6) Uani 1 1 d . . . H6 H 1.2488 0.4185 0.1933 0.024 Uiso 1 1 calc R . . C7 C 1.0727(3) 0.43373(18) 0.0896(3) 0.0180(6) Uani 1 1 d . . . C8 C 1.2487(3) 0.5825(2) 0.0634(4) 0.0299(8) Uani 1 1 d . . . H8A H 1.3256 0.5416 0.0724 0.045 Uiso 1 1 calc R . . H8B H 1.2183 0.6010 0.1565 0.045 Uiso 1 1 calc R . . H8C H 1.2743 0.6369 0.0100 0.045 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Te1 0.01544(8) 0.01626(8) 0.01658(9) -0.00055(10) 0.00055(11) -0.00015(6) Cl1 0.0229(3) 0.0300(3) 0.0463(5) -0.0048(4) 0.0107(4) -0.0086(3) Cl2 0.0303(4) 0.0317(4) 0.0231(4) 0.0045(3) -0.0023(3) 0.0106(4) Cl3 0.0241(3) 0.0248(3) 0.0353(5) -0.0021(3) 0.0035(3) -0.0071(3) Cl4 0.0222(4) 0.0255(4) 0.0234(4) -0.0059(3) 0.0022(3) 0.0014(3) S1 0.0177(3) 0.0234(4) 0.0198(4) 0.0032(3) 0.0001(3) 0.0033(3) S2 0.0194(3) 0.0214(3) 0.0209(4) 0.0034(3) 0.0017(3) 0.0004(3) C1 0.0204(15) 0.0280(16) 0.0291(19) -0.0025(13) -0.0051(13) -0.0029(13) C2 0.0201(14) 0.0197(14) 0.0151(14) -0.0019(11) 0.0018(11) 0.0030(12) C3 0.0265(16) 0.0231(15) 0.0223(15) -0.0021(12) 0.0055(13) 0.0003(12) C4 0.0352(15) 0.0180(12) 0.0159(18) 0.0029(12) 0.0033(13) 0.0035(11) C5 0.0304(16) 0.0259(15) 0.0178(18) 0.0012(11) -0.0020(11) 0.0141(13) C6 0.0162(13) 0.0246(15) 0.0199(15) -0.0027(11) -0.0019(11) 0.0063(12) C7 0.0203(14) 0.0189(14) 0.0149(15) -0.0009(11) 0.0014(11) 0.0017(11) C8 0.0301(18) 0.0286(17) 0.031(2) -0.0056(15) -0.0015(14) -0.0093(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Te1 Cl4 2.3435(9) . ? Te1 Cl2 2.3521(9) . ? Te1 Cl1 2.4389(7) . ? Te1 Cl3 2.5212(8) . ? Te1 S2 3.0375(8) 2_765 ? Te1 S1 3.0580(9) . ? S1 C2 1.775(3) . ? S1 C1 1.801(3) . ? S1 S2 3.0379(13) . ? S2 C7 1.773(3) . ? S2 C8 1.800(3) . ? S2 Te1 3.0375(8) 2_764 ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.398(4) . ? C2 C7 1.405(4) . ? C3 C4 1.380(4) . ? C3 H3 0.9500 . ? C4 C5 1.388(4) . ? C4 H4 0.9500 . ? C5 C6 1.383(4) . ? C5 H5 0.9500 . ? C6 C7 1.392(4) . ? C6 H6 0.9500 . ? 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 Cl4 Te1 Cl2 90.57(3) . . ? Cl4 Te1 Cl1 89.64(3) . . ? Cl2 Te1 Cl1 91.10(3) . . ? Cl4 Te1 Cl3 87.99(3) . . ? Cl2 Te1 Cl3 90.16(3) . . ? Cl1 Te1 Cl3 177.32(4) . . ? Cl4 Te1 S2 82.42(3) . 2_765 ? Cl2 Te1 S2 172.79(3) . 2_765 ? Cl1 Te1 S2 87.20(3) . 2_765 ? Cl3 Te1 S2 91.25(3) . 2_765 ? Cl4 Te1 S1 171.93(3) . . ? Cl2 Te1 S1 81.98(3) . . ? Cl1 Te1 S1 93.56(3) . . ? Cl3 Te1 S1 88.96(2) . . ? S2 Te1 S1 105.11(2) 2_765 . ? C2 S1 C1 104.02(14) . . ? C2 S1 S2 62.31(10) . . ? C1 S1 S2 155.23(11) . . ? C2 S1 Te1 88.01(9) . . ? C1 S1 Te1 103.29(11) . . ? S2 S1 Te1 97.01(3) . . ? C7 S2 C8 103.90(16) . . ? C7 S2 Te1 105.89(10) . 2_764 ? C8 S2 Te1 102.28(12) . 2_764 ? C7 S2 S1 62.76(10) . . ? C8 S2 S1 148.42(12) . . ? Te1 S2 S1 108.84(3) 2_764 . ? 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 C7 119.5(3) . . ? C3 C2 S1 122.7(2) . . ? C7 C2 S1 117.7(2) . . ? C4 C3 C2 120.4(3) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 119.9(3) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C6 C5 C4 120.5(3) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C5 C6 C7 120.2(3) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? C6 C7 C2 119.4(3) . . ? C6 C7 S2 123.7(2) . . ? C2 C7 S2 116.9(2) . . ? S2 C8 H8A 109.5 . . ? S2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? S2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Te1 S1 3.0580(9) . . ? Te1 S2 3.0375(8) . 2_765 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.385 _refine_diff_density_min -0.417 _refine_diff_density_rms 0.079 data_11aj21 _database_code_depnum_ccdc_archive 'CCDC 881026' #TrackingRef '- Te_all15_3.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2011-12-24 _audit_author_name 'Webster, M.' _chemical_name_systematic ; bis(trimethylselenonium) hexachlorotellurate(IV) ; # Me3Se+ = C3H9Se cation # trimethylselenonium (iLab name (defaults)) # SMILES: C[Se+](C)C _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C3 H9 Se 1+)2, Cl6 Te 2-' _chemical_formula_sum 'C6 H18 Cl6 Se2 Te' _chemical_formula_weight 588.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 '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 cubic _symmetry_space_group_name_H-M 'P a -3' _space_group_IT_number 205 _space_group_name_Hall '-P 2ac 2ab 3' # '-P 2ac 2ab' # There is something odd about the Hall group for this space group. # See S.R. Hall, Acta Cryst., 1981, A37, 517. Table 6, entry for 205 # has error (missing bar) and Hall symbol includes '3'. mw loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' '-z, -x, -y' '-z-1/2, x-1/2, y' 'z-1/2, x, -y-1/2' 'z, -x-1/2, y-1/2' '-y, -z, -x' 'y, -z-1/2, x-1/2' '-y-1/2, z-1/2, x' 'y-1/2, z, -x-1/2' _cell_length_a 12.513(3) _cell_length_b 12.513(3) _cell_length_c 12.513(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1959.2(8) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6001 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.995 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 6.029 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5009 # Expt'l Tmin & Tmax _exptl_absorpt_correction_T_max 1.0000 # scaled to Tmax=1.0 _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 APEX II 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 6437 _diffrn_reflns_av_R_equivalents 0.1359 _diffrn_reflns_av_sigmaI/netI 0.0704 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.26 _diffrn_reflns_theta_max 26.34 _reflns_number_total 662 _reflns_number_gt 460 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997)' _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^+24.2365P] 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 662 _refine_ls_number_parameters 25 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1077 _refine_ls_R_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.1125 _refine_ls_wR_factor_gt 0.0971 _refine_ls_goodness_of_fit_ref 1.159 _refine_ls_restrained_S_all 1.159 _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 0.5000 0.5000 0.0000 0.0245(4) Uani 1 6 d S . . Se1 Se 0.27562(7) 0.22438(7) 0.77562(7) 0.0268(4) Uani 1 3 d S . . Cl1 Cl 0.4608(2) 0.30648(19) -0.04604(19) 0.0332(6) Uani 1 1 d . . . C1 C 0.3405(8) 0.3368(8) 0.6912(7) 0.035(2) Uani 1 1 d . . . H1A H 0.3877 0.3051 0.6374 0.052 Uiso 1 1 calc R . . H1B H 0.3821 0.3839 0.7380 0.052 Uiso 1 1 calc R . . H1C H 0.2845 0.3783 0.6555 0.052 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 0.0245(4) 0.0245(4) 0.0245(4) 0.0008(4) -0.0008(4) -0.0008(4) Se1 0.0268(4) 0.0268(4) 0.0268(4) 0.0000(4) 0.0000(4) 0.0000(4) Cl1 0.0379(14) 0.0276(13) 0.0341(13) -0.0021(10) -0.0044(10) -0.0012(10) C1 0.038(6) 0.038(6) 0.029(5) 0.005(5) 0.000(5) -0.016(5) _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 2.537(2) 13_665 ? Te1 Cl1 2.537(2) 22_565 ? Te1 Cl1 2.537(2) . ? Te1 Cl1 2.537(2) 7_564 ? Te1 Cl1 2.537(2) 19_656 ? Te1 Cl1 2.537(2) 10_655 ? Se1 C1 1.938(9) 6_456 ? Se1 C1 1.938(9) 12_565 ? Se1 C1 1.938(9) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 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 Cl1 90.67(8) 13_665 22_565 ? Cl1 Te1 Cl1 180.00(11) 13_665 . ? Cl1 Te1 Cl1 89.33(8) 22_565 . ? Cl1 Te1 Cl1 89.33(8) 13_665 7_564 ? Cl1 Te1 Cl1 89.33(8) 22_565 7_564 ? Cl1 Te1 Cl1 90.67(8) . 7_564 ? Cl1 Te1 Cl1 90.67(8) 13_665 19_656 ? Cl1 Te1 Cl1 90.67(8) 22_565 19_656 ? Cl1 Te1 Cl1 89.33(8) . 19_656 ? Cl1 Te1 Cl1 180.0 7_564 19_656 ? Cl1 Te1 Cl1 89.33(8) 13_665 10_655 ? Cl1 Te1 Cl1 180.00(15) 22_565 10_655 ? Cl1 Te1 Cl1 90.67(8) . 10_655 ? Cl1 Te1 Cl1 90.67(8) 7_564 10_655 ? Cl1 Te1 Cl1 89.33(8) 19_656 10_655 ? C1 Se1 C1 97.9(4) 6_456 12_565 ? C1 Se1 C1 97.9(4) 6_456 . ? C1 Se1 C1 97.9(4) 12_565 . ? Se1 C1 H1A 109.5 . . ? Se1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Se1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 26.34 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.695 _refine_diff_density_min -0.706 _refine_diff_density_rms 0.174 data_11ajj18a _database_code_depnum_ccdc_archive 'CCDC 881027' #TrackingRef '- Te_all15_3.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2011-12-25 _audit_author_name 'Webster, M.' _chemical_name_systematic ; tetrachloro(1,2-bis(methylsulfanylmethyl)benzene-S,S')tellurium(IV) ; # o-C6H4(CH2SMe)2 = C10H14S2 # 1,2-bis(methylthiomethyl)benzene # 1,2-bis[(methylthio)methyl]benzene (iLab IUPAC name (defaults)) # 1,2-bis(methylsulfanylmethyl)benzene (chemspider) # 1,2-bis[(methylsulfanyl)methyl]benzene (iLab selected options) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H14 Cl4 S2 Te' _chemical_formula_sum 'C10 H14 Cl4 S2 Te' _chemical_formula_weight 467.73 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 orthorhombic _symmetry_space_group_name_H-M 'P n m a' _space_group_IT_number 62 _space_group_name_Hall '-P 2ac 2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 19.451(3) _cell_length_b 11.603(2) _cell_length_c 7.1757(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1619.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2119 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.918 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 2.732 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7971 # Expt'l Tmin & Tmax _exptl_absorpt_correction_T_max 1.0000 # scaled to Tmax=1.0 _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 APEX II 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 12485 _diffrn_reflns_av_R_equivalents 0.0287 _diffrn_reflns_av_sigmaI/netI 0.0232 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.47 _reflns_number_total 1937 _reflns_number_gt 1853 _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^+2.0277P] 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 1937 _refine_ls_number_parameters 83 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0215 _refine_ls_R_factor_gt 0.0196 _refine_ls_wR_factor_ref 0.0428 _refine_ls_wR_factor_gt 0.0419 _refine_ls_goodness_of_fit_ref 1.131 _refine_ls_restrained_S_all 1.131 _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 0.114018(9) 0.2500 0.33856(2) 0.01501(6) Uani 1 2 d S . . Cl1 Cl 0.22250(4) 0.2500 0.15035(10) 0.02694(17) Uani 1 2 d S . . Cl2 Cl 0.02146(4) 0.2500 0.58127(11) 0.02514(16) Uani 1 2 d S . . Cl3 Cl 0.05880(3) 0.10554(4) 0.14648(7) 0.02371(12) Uani 1 1 d . . . S1 S 0.16974(2) 0.04907(4) 0.51555(7) 0.01821(11) Uani 1 1 d . . . C1 C 0.26249(10) 0.18961(17) 0.6797(3) 0.0162(4) Uani 1 1 d . . . C2 C 0.32277(10) 0.13125(18) 0.6300(3) 0.0190(4) Uani 1 1 d . . . H2 H 0.3229 0.0494 0.6282 0.023 Uiso 1 1 calc R . . C3 C 0.38223(10) 0.19020(19) 0.5836(3) 0.0217(4) Uani 1 1 d . . . H3 H 0.4228 0.1490 0.5519 0.026 Uiso 1 1 calc R . . C4 C 0.20036(10) 0.11742(17) 0.7282(3) 0.0186(4) Uani 1 1 d . . . H4A H 0.1638 0.1667 0.7819 0.022 Uiso 1 1 calc R . . H4B H 0.2129 0.0581 0.8213 0.022 Uiso 1 1 calc R . . C5 C 0.09853(12) -0.0340(2) 0.6039(3) 0.0291(5) Uani 1 1 d . . . H5A H 0.1157 -0.0939 0.6881 0.044 Uiso 1 1 calc R . . H5B H 0.0741 -0.0701 0.4998 0.044 Uiso 1 1 calc R . . H5C H 0.0671 0.0169 0.6719 0.044 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 0.01375(10) 0.01653(10) 0.01475(10) 0.000 0.00008(6) 0.000 Cl1 0.0190(3) 0.0434(4) 0.0183(3) 0.000 0.0034(3) 0.000 Cl2 0.0199(3) 0.0271(4) 0.0284(4) 0.000 0.0079(3) 0.000 Cl3 0.0223(3) 0.0211(2) 0.0278(3) -0.0047(2) -0.0068(2) 0.00021(19) S1 0.0181(2) 0.0180(2) 0.0186(2) -0.00012(19) -0.00142(19) -0.00096(18) C1 0.0150(9) 0.0228(10) 0.0107(8) -0.0001(7) -0.0014(7) -0.0008(8) C2 0.0189(10) 0.0212(10) 0.0169(9) 0.0001(8) -0.0009(8) 0.0027(8) C3 0.0166(10) 0.0293(11) 0.0190(10) -0.0006(9) 0.0011(8) 0.0043(8) C4 0.0175(9) 0.0235(10) 0.0149(9) 0.0021(8) -0.0006(8) -0.0017(8) C5 0.0277(11) 0.0270(11) 0.0327(12) 0.0071(10) -0.0026(10) -0.0106(9) _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 Cl3 2.4213(6) . ? Te1 Cl3 2.4213(6) 8_565 ? Te1 Cl2 2.5049(8) . ? Te1 Cl1 2.5052(8) . ? Te1 S1 2.8675(6) 8_565 ? Te1 S1 2.8675(6) . ? S1 C5 1.803(2) . ? S1 C4 1.820(2) . ? C1 C2 1.400(3) . ? C1 C1 1.401(4) 8_565 ? C1 C4 1.511(3) . ? C2 C3 1.384(3) . ? C2 H2 0.9500 . ? C3 C3 1.388(4) 8_565 ? C3 H3 0.9500 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 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 Cl3 Te1 Cl3 87.62(3) . 8_565 ? Cl3 Te1 Cl2 94.41(2) . . ? Cl3 Te1 Cl2 94.41(2) 8_565 . ? Cl3 Te1 Cl1 93.83(2) . . ? Cl3 Te1 Cl1 93.83(2) 8_565 . ? Cl2 Te1 Cl1 168.57(3) . . ? Cl3 Te1 S1 169.289(17) . 8_565 ? Cl3 Te1 S1 81.776(19) 8_565 8_565 ? Cl2 Te1 S1 87.919(16) . 8_565 ? Cl1 Te1 S1 85.436(16) . 8_565 ? Cl3 Te1 S1 81.776(19) . . ? Cl3 Te1 S1 169.289(17) 8_565 . ? Cl2 Te1 S1 87.919(16) . . ? Cl1 Te1 S1 85.436(16) . . ? S1 Te1 S1 108.78(2) 8_565 . ? C5 S1 C4 100.92(10) . . ? C5 S1 Te1 107.46(8) . . ? C4 S1 Te1 98.09(7) . . ? C2 C1 C1 118.93(12) . 8_565 ? C2 C1 C4 117.40(17) . . ? C1 C1 C4 123.67(11) 8_565 . ? C3 C2 C1 121.46(19) . . ? C3 C2 H2 119.3 . . ? C1 C2 H2 119.3 . . ? C2 C3 C3 119.61(12) . 8_565 ? C2 C3 H3 120.2 . . ? C3 C3 H3 120.2 8_565 . ? C1 C4 S1 108.08(13) . . ? C1 C4 H4A 110.1 . . ? S1 C4 H4A 110.1 . . ? C1 C4 H4B 110.1 . . ? S1 C4 H4B 110.1 . . ? H4A C4 H4B 108.4 . . ? S1 C5 H5A 109.5 . . ? S1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? S1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 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 Cl3 Te1 S1 C5 -60.30(9) . . . . ? Cl3 Te1 S1 C5 -68.39(13) 8_565 . . . ? Cl2 Te1 S1 C5 34.46(9) . . . . ? Cl1 Te1 S1 C5 -154.85(9) . . . . ? S1 Te1 S1 C5 121.55(9) 8_565 . . . ? Cl3 Te1 S1 C4 -164.50(7) . . . . ? Cl3 Te1 S1 C4 -172.59(11) 8_565 . . . ? Cl2 Te1 S1 C4 -69.74(7) . . . . ? Cl1 Te1 S1 C4 100.95(7) . . . . ? S1 Te1 S1 C4 17.35(7) 8_565 . . . ? C1 C1 C2 C3 0.9(2) 8_565 . . . ? C4 C1 C2 C3 -179.96(18) . . . . ? C1 C2 C3 C3 -0.9(2) . . . 8_565 ? C2 C1 C4 S1 -69.68(19) . . . . ? C1 C1 C4 S1 109.47(10) 8_565 . . . ? C5 S1 C4 C1 178.57(14) . . . . ? Te1 S1 C4 C1 -71.80(13) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.904 _refine_diff_density_min -0.423 _refine_diff_density_rms 0.079 data_11aj002c _database_code_depnum_ccdc_archive 'CCDC 881028' #TrackingRef '- Te_all15_3.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2011-12-26 _audit_author_name 'Webster, M.' _chemical_name_systematic ; tetrafluoro(trimethylphosphine oxide-O)tellurium(IV) ; # Me3PO = C3H9OP # trimethylphosphane oxide (Chemspider) # trimethylphosphine oxide (iLab name (defaults)) # dimethylphosphorylmethane (chemspider) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C3 H9 F4 O P Te' _chemical_formula_sum 'C3 H9 F4 O P Te' _chemical_formula_weight 295.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 6.500(4) _cell_length_b 10.790(5) _cell_length_c 12.442(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 872.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2325 _cell_measurement_theta_min 3.3 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.251 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 552 _exptl_absorpt_coefficient_mu 3.598 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.824 # Expt'l Tmin & Tmax _exptl_absorpt_correction_T_max 1.000 # scaled to Tmax=1.0 _exptl_absorpt_process_details ;Jacobson, R.A. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator ? _diffrn_radiation_collimation 'Confocal mirrors, HF VariMax ' _diffrn_source 'Rotating anode X-ray tube' _diffrn_source_type 'Rigaku FR-E+ SuperBright' _diffrn_measurement_device 'Four-circle \k diffractometer' _diffrn_measurement_device_type 'Rigaku AFC12 ' _diffrn_measurement_method 'Profile data from \w-scans' _diffrn_detector 'CCD plate' _diffrn_detector_type 'Rigaku HG Saturn724+ (2x2 bin mode)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2336 _diffrn_reflns_av_R_equivalents 0.0192 _diffrn_reflns_av_sigmaI/netI 0.0306 _diffrn_reflns_limit_h_min -2 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.27 _diffrn_reflns_theta_max 27.37 _reflns_number_total 1815 _reflns_number_gt 1758 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _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^)+(0.0040P)^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 -0.029(18) _chemical_absolute_configuration ad _refine_ls_number_reflns 1815 _refine_ls_number_parameters 94 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0143 _refine_ls_R_factor_gt 0.0138 _refine_ls_wR_factor_ref 0.0336 _refine_ls_wR_factor_gt 0.0335 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _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 0.35430(2) 0.104368(14) 0.420574(13) 0.01380(5) Uani 1 1 d . . . F1 F 0.5960(2) 0.00591(14) 0.41669(14) 0.0259(4) Uani 1 1 d . . . F2 F 0.5577(3) 0.22154(15) 0.47949(14) 0.0294(4) Uani 1 1 d . . . F3 F 0.3318(3) 0.03282(14) 0.56163(12) 0.0262(4) Uani 1 1 d . . . F4 F 0.2327(3) -0.04946(15) 0.36545(14) 0.0292(4) Uani 1 1 d . . . P1 P 0.63950(10) 0.11070(6) 0.18902(5) 0.01437(12) Uani 1 1 d . . . O1 O 0.4566(3) 0.14780(16) 0.26307(15) 0.0177(4) Uani 1 1 d . . . C1 C 0.8800(4) 0.1706(3) 0.2387(2) 0.0257(7) Uani 1 1 d . . . H1A H 0.8763 0.2614 0.2377 0.039 Uiso 1 1 calc R . . H1B H 0.9927 0.1413 0.1930 0.039 Uiso 1 1 calc R . . H1C H 0.9018 0.1418 0.3125 0.039 Uiso 1 1 calc R . . C2 C 0.5906(4) 0.1747(2) 0.0599(2) 0.0194(6) Uani 1 1 d . . . H2A H 0.4586 0.1437 0.0330 0.029 Uiso 1 1 calc R . . H2B H 0.7007 0.1503 0.0104 0.029 Uiso 1 1 calc R . . H2C H 0.5856 0.2652 0.0652 0.029 Uiso 1 1 calc R . . C3 C 0.6619(5) -0.0535(2) 0.1760(2) 0.0237(6) Uani 1 1 d . . . H3A H 0.7007 -0.0894 0.2454 0.036 Uiso 1 1 calc R . . H3B H 0.7675 -0.0731 0.1224 0.036 Uiso 1 1 calc R . . H3C H 0.5296 -0.0881 0.1529 0.036 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 0.01523(7) 0.01209(8) 0.01409(8) -0.00022(7) -0.00150(7) 0.00061(7) F1 0.0241(8) 0.0287(8) 0.0248(9) 0.0068(8) -0.0005(8) 0.0137(6) F2 0.0346(9) 0.0271(10) 0.0266(10) -0.0005(8) -0.0108(8) -0.0109(8) F3 0.0313(9) 0.0308(9) 0.0167(8) 0.0084(7) -0.0001(8) 0.0012(8) F4 0.0403(10) 0.0174(8) 0.0298(10) -0.0003(8) -0.0065(9) -0.0081(7) P1 0.0144(2) 0.0120(3) 0.0167(3) 0.0004(3) 0.0008(3) 0.0008(3) O1 0.0209(9) 0.0165(9) 0.0157(10) 0.0013(8) 0.0010(9) 0.0047(8) C1 0.0180(13) 0.0268(15) 0.0323(17) 0.0036(13) -0.0065(13) -0.0019(11) C2 0.0223(13) 0.0166(13) 0.0192(15) -0.0002(11) 0.0008(10) -0.0014(10) C3 0.0304(14) 0.0152(12) 0.0255(15) 0.0000(11) 0.0070(14) 0.0042(12) _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 F1 1.8973(17) . ? Te1 F3 1.9229(18) . ? Te1 F4 1.9623(18) . ? Te1 F2 1.9707(18) . ? Te1 O1 2.122(2) . ? P1 O1 1.556(2) . ? P1 C2 1.777(3) . ? P1 C3 1.785(3) . ? P1 C1 1.801(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 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 F1 Te1 F3 82.04(7) . . ? F1 Te1 F4 81.43(9) . . ? F3 Te1 F4 87.06(8) . . ? F1 Te1 F2 79.23(8) . . ? F3 Te1 F2 88.23(8) . . ? F4 Te1 F2 160.56(8) . . ? F1 Te1 O1 80.83(7) . . ? F3 Te1 O1 162.84(7) . . ? F4 Te1 O1 89.44(8) . . ? F2 Te1 O1 89.52(8) . . ? O1 P1 C2 107.38(12) . . ? O1 P1 C3 111.80(12) . . ? C2 P1 C3 108.53(13) . . ? O1 P1 C1 111.55(12) . . ? C2 P1 C1 109.02(13) . . ? C3 P1 C1 108.48(15) . . ? P1 O1 Te1 136.83(11) . . ? P1 C1 H1A 109.5 . . ? P1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? P1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? P1 C2 H2A 109.5 . . ? P1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? P1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? P1 C3 H3A 109.5 . . ? P1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? P1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 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 C2 P1 O1 Te1 172.14(15) . . . . ? C3 P1 O1 Te1 53.2(2) . . . . ? C1 P1 O1 Te1 -68.46(19) . . . . ? F1 Te1 O1 P1 0.64(16) . . . . ? F3 Te1 O1 P1 -2.6(4) . . . . ? F4 Te1 O1 P1 -80.77(18) . . . . ? F2 Te1 O1 P1 79.81(17) . . . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Te1 F2 2.965(2) . 3_456 ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.37 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.278 _refine_diff_density_min -0.375 _refine_diff_density_rms 0.072 data_11aj003r _database_code_depnum_ccdc_archive 'CCDC 881029' #TrackingRef '- Te_all15_3.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 201-12-27 _audit_author_name 'Webster, M.' _chemical_name_systematic ; Tetrafluoro(triphenylphosphine oxide-O)tellurium(IV) ; # Ph3PO = C18H15OP # triphenylphosphine oxide # triphenylphosphine oxide (i-Lab IUPAC name (defaults)) # triphenylphosphane oxide (iLab name (selected options) # Chemspider gave diphenylphosphorylbenzene (+ several other names) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H15 F4 O P Te' _chemical_formula_sum 'C18 H15 F4 O P Te' _chemical_formula_structural '((C6 H5)3 O P) (F4 Te)' _chemical_formula_weight 481.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 9.933(3) _cell_length_b 18.151(5) _cell_length_c 10.604(7) _cell_angle_alpha 90.00 _cell_angle_beta 113.90(4) _cell_angle_gamma 90.00 _cell_volume 1747.9(14) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7159 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.831 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 1.836 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.870 # Expt'l Tmin & Tmax _exptl_absorpt_correction_T_max 1.000 # scaled to Tmax=1.0 _exptl_absorpt_process_details ;Jacobson, R.A. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator ? _diffrn_radiation_collimation 'Confocal mirrors, VHF VariMax ' _diffrn_source 'Rotating anode X-ray tube' _diffrn_source_type 'Rigaku FR-E+ Superbright' _diffrn_measurement_device 'Four-circle \k diffractometer' _diffrn_measurement_device_type 'Rigaku AFC12 ' _diffrn_measurement_method 'Profile data from \w-scans' _diffrn_detector 'CCD plate' _diffrn_detector_type 'Rigaku HG Saturn724+ (2x2 bin mode)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7751 _diffrn_reflns_av_R_equivalents 0.0181 _diffrn_reflns_av_sigmaI/netI 0.0238 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3965 _reflns_number_gt 3677 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _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^)+(0.0159P)^2^+1.4166P] 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 3965 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0204 _refine_ls_R_factor_gt 0.0182 _refine_ls_wR_factor_ref 0.0443 _refine_ls_wR_factor_gt 0.0434 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 0.718463(12) 0.027609(6) 0.647640(10) 0.01245(4) Uani 1 1 d . . . F1 F 0.73096(13) 0.11429(6) 0.74489(11) 0.0203(2) Uani 1 1 d . . . F2 F 0.54761(12) 0.07901(7) 0.51479(11) 0.0228(2) Uani 1 1 d . . . F3 F 0.60408(13) -0.00406(7) 0.74417(11) 0.0227(2) Uani 1 1 d . . . F4 F 0.89584(13) 0.00662(7) 0.81154(11) 0.0250(3) Uani 1 1 d . . . P1 P 0.86449(5) 0.15010(2) 0.47557(4) 0.01147(9) Uani 1 1 d . . . O1 O 0.86196(14) 0.09195(7) 0.57872(12) 0.0157(2) Uani 1 1 d . . . C1 C 0.77933(18) 0.23426(10) 0.49355(17) 0.0126(3) Uani 1 1 d . . . C2 C 0.7930(2) 0.25506(10) 0.62553(17) 0.0161(3) Uani 1 1 d . . . H2 H 0.8478 0.2253 0.7031 0.019 Uiso 1 1 calc R . . C3 C 0.7263(2) 0.31915(11) 0.64266(18) 0.0194(4) Uani 1 1 d . . . H3 H 0.7352 0.3330 0.7321 0.023 Uiso 1 1 calc R . . C4 C 0.6464(2) 0.36325(10) 0.52955(19) 0.0191(4) Uani 1 1 d . . . H4 H 0.5995 0.4067 0.5415 0.023 Uiso 1 1 calc R . . C5 C 0.6355(2) 0.34354(10) 0.39896(19) 0.0189(4) Uani 1 1 d . . . H5 H 0.5824 0.3740 0.3219 0.023 Uiso 1 1 calc R . . C6 C 0.7019(2) 0.27945(10) 0.38078(17) 0.0163(3) Uani 1 1 d . . . H6 H 0.6947 0.2664 0.2915 0.020 Uiso 1 1 calc R . . C7 C 1.05437(19) 0.16710(10) 0.51153(17) 0.0141(3) Uani 1 1 d . . . C8 C 1.0965(2) 0.23140(10) 0.46450(18) 0.0186(4) Uani 1 1 d . . . H8 H 1.0244 0.2667 0.4134 0.022 Uiso 1 1 calc R . . C9 C 1.2448(2) 0.24359(11) 0.4929(2) 0.0237(4) Uani 1 1 d . . . H9 H 1.2738 0.2870 0.4604 0.028 Uiso 1 1 calc R . . C10 C 1.3497(2) 0.19219(12) 0.5686(2) 0.0256(4) Uani 1 1 d . . . H10 H 1.4507 0.2009 0.5890 0.031 Uiso 1 1 calc R . . C11 C 1.3081(2) 0.12801(12) 0.6150(2) 0.0237(4) Uani 1 1 d . . . H11 H 1.3806 0.0929 0.6663 0.028 Uiso 1 1 calc R . . C12 C 1.1606(2) 0.11519(11) 0.58632(18) 0.0180(4) Uani 1 1 d . . . H12 H 1.1321 0.0712 0.6175 0.022 Uiso 1 1 calc R . . C13 C 0.77476(19) 0.11961(9) 0.30056(17) 0.0136(3) Uani 1 1 d . . . C14 C 0.8566(2) 0.09474(10) 0.22877(18) 0.0174(3) Uani 1 1 d . . . H14 H 0.9611 0.0952 0.2716 0.021 Uiso 1 1 calc R . . C15 C 0.7843(2) 0.06926(11) 0.09383(18) 0.0197(4) Uani 1 1 d . . . H15 H 0.8394 0.0513 0.0451 0.024 Uiso 1 1 calc R . . C16 C 0.6315(2) 0.07020(10) 0.03086(18) 0.0192(4) Uani 1 1 d . . . H16 H 0.5825 0.0541 -0.0619 0.023 Uiso 1 1 calc R . . C17 C 0.5497(2) 0.09448(10) 0.10241(17) 0.0169(3) Uani 1 1 d . . . H17 H 0.4452 0.0946 0.0587 0.020 Uiso 1 1 calc R . . C18 C 0.6206(2) 0.11855(10) 0.23795(17) 0.0155(3) Uani 1 1 d . . . H18 H 0.5649 0.1342 0.2878 0.019 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 0.01341(6) 0.01308(6) 0.01177(6) -0.00013(4) 0.00603(4) -0.00001(4) F1 0.0297(6) 0.0163(5) 0.0197(5) -0.0059(4) 0.0149(5) -0.0038(5) F2 0.0168(5) 0.0298(6) 0.0196(5) 0.0037(4) 0.0052(4) 0.0050(5) F3 0.0263(6) 0.0266(6) 0.0209(5) -0.0020(4) 0.0154(5) -0.0077(5) F4 0.0197(6) 0.0308(6) 0.0201(6) 0.0107(5) 0.0034(5) 0.0020(5) P1 0.01138(19) 0.0127(2) 0.01030(18) 0.00012(14) 0.00441(15) 0.00083(16) O1 0.0148(6) 0.0172(6) 0.0156(6) 0.0040(5) 0.0069(5) 0.0011(5) C1 0.0105(7) 0.0134(8) 0.0139(7) -0.0017(6) 0.0049(6) 0.0001(6) C2 0.0185(8) 0.0161(8) 0.0127(8) -0.0004(6) 0.0052(7) -0.0016(7) C3 0.0252(10) 0.0184(9) 0.0183(9) -0.0054(7) 0.0127(8) -0.0023(8) C4 0.0183(9) 0.0163(9) 0.0239(9) -0.0043(7) 0.0098(7) 0.0010(7) C5 0.0174(9) 0.0174(9) 0.0182(8) -0.0003(7) 0.0036(7) 0.0043(7) C6 0.0166(8) 0.0179(9) 0.0125(8) -0.0017(6) 0.0040(6) 0.0016(7) C7 0.0129(8) 0.0173(8) 0.0125(7) -0.0041(6) 0.0054(6) -0.0005(7) C8 0.0193(9) 0.0179(9) 0.0203(8) -0.0024(7) 0.0097(7) -0.0011(7) C9 0.0241(10) 0.0207(10) 0.0325(10) -0.0082(8) 0.0179(9) -0.0067(8) C10 0.0156(9) 0.0322(11) 0.0312(10) -0.0121(8) 0.0118(8) -0.0048(8) C11 0.0157(9) 0.0305(11) 0.0229(9) -0.0034(8) 0.0059(7) 0.0059(8) C12 0.0168(8) 0.0199(9) 0.0173(8) -0.0004(7) 0.0069(7) 0.0028(7) C13 0.0157(8) 0.0122(8) 0.0122(7) -0.0009(6) 0.0049(6) -0.0006(7) C14 0.0155(8) 0.0189(9) 0.0176(8) -0.0036(6) 0.0064(7) -0.0001(7) C15 0.0231(9) 0.0207(9) 0.0185(8) -0.0057(7) 0.0116(7) -0.0016(8) C16 0.0250(9) 0.0186(9) 0.0136(8) -0.0040(6) 0.0073(7) -0.0052(8) C17 0.0155(8) 0.0177(9) 0.0151(8) -0.0016(6) 0.0037(7) -0.0038(7) C18 0.0163(8) 0.0168(8) 0.0153(8) -0.0005(6) 0.0082(7) -0.0009(7) _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 F1 1.8575(12) . ? Te1 F3 1.9005(13) . ? Te1 F4 1.9464(16) . ? Te1 F2 1.9488(14) . ? Te1 O1 2.1849(14) . ? P1 O1 1.5275(14) . ? P1 C13 1.790(2) . ? P1 C7 1.7930(19) . ? P1 C1 1.7935(18) . ? C1 C6 1.396(2) . ? C1 C2 1.402(2) . ? C2 C3 1.387(3) . ? C2 H2 0.9500 . ? C3 C4 1.392(3) . ? C3 H3 0.9500 . ? C4 C5 1.391(3) . ? C4 H4 0.9500 . ? C5 C6 1.389(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.397(3) . ? C7 C8 1.398(3) . ? C8 C9 1.397(3) . ? C8 H8 0.9500 . ? C9 C10 1.386(3) . ? C9 H9 0.9500 . ? C10 C11 1.391(3) . ? C10 H10 0.9500 . ? C11 C12 1.390(3) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.395(2) . ? C13 C18 1.400(2) . ? C14 C15 1.394(3) . ? C14 H14 0.9500 . ? C15 C16 1.388(3) . ? C15 H15 0.9500 . ? C16 C17 1.389(3) . ? C16 H16 0.9500 . ? C17 C18 1.390(2) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F1 Te1 F3 82.95(6) . . ? F1 Te1 F4 80.64(6) . . ? F3 Te1 F4 88.98(6) . . ? F1 Te1 F2 80.71(6) . . ? F3 Te1 F2 89.92(6) . . ? F4 Te1 F2 161.31(5) . . ? F1 Te1 O1 80.04(6) . . ? F3 Te1 O1 162.80(5) . . ? F4 Te1 O1 85.76(6) . . ? F2 Te1 O1 89.85(6) . . ? O1 P1 C13 112.52(8) . . ? O1 P1 C7 106.72(8) . . ? C13 P1 C7 108.22(9) . . ? O1 P1 C1 111.54(8) . . ? C13 P1 C1 108.39(8) . . ? C7 P1 C1 109.36(8) . . ? P1 O1 Te1 144.20(8) . . ? C6 C1 C2 119.60(16) . . ? C6 C1 P1 121.95(13) . . ? C2 C1 P1 118.45(13) . . ? C3 C2 C1 119.90(16) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C2 C3 C4 120.36(16) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C5 C4 C3 119.81(18) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C6 C5 C4 120.24(17) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C5 C6 C1 120.06(16) . . ? C5 C6 H6 120.0 . . ? C1 C6 H6 120.0 . . ? C12 C7 C8 119.95(17) . . ? C12 C7 P1 119.47(14) . . ? C8 C7 P1 120.58(14) . . ? C9 C8 C7 119.81(18) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C10 C9 C8 119.84(19) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C9 C10 C11 120.50(19) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C12 C11 C10 120.03(19) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C7 119.86(18) . . ? C11 C12 H12 120.1 . . ? C7 C12 H12 120.1 . . ? C14 C13 C18 120.24(16) . . ? C14 C13 P1 120.70(14) . . ? C18 C13 P1 119.02(14) . . ? C15 C14 C13 119.72(17) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C16 C15 C14 119.84(18) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C17 120.54(16) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C16 C17 C18 120.07(17) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C17 C18 C13 119.54(17) . . ? C17 C18 H18 120.2 . . ? C13 C18 H18 120.2 . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Te1 F2 3.163(2) . 3_656 ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.978 _refine_diff_density_min -0.487 _refine_diff_density_rms 0.072 data_11aj0108c _database_code_depnum_ccdc_archive 'CCDC 881030' #TrackingRef '- Te_all15_3.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2011-12-27 _audit_author_name 'Webster, M.' _chemical_name_systematic ; tetrabromo(methylselanylmethane-Se)tellurium(IV) ; # Me2Se = C2H6Se # dimethylselenide (chemspider) # methylselanylmethane (chemspider IUPAC name) # dimethyl selenide (chemspider) # (methylseleno)methane (iLab (defaults)) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H12 Br4 Se2 Te' _chemical_formula_sum 'C4 H12 Br4 Se2 Te' _chemical_formula_weight 665.30 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' Se Se -0.0929 2.2259 '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 6.720(2) _cell_length_b 13.138(4) _cell_length_c 8.486(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.967(5) _cell_angle_gamma 90.00 _cell_volume 712.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2889 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 31.4 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.100 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 592 _exptl_absorpt_coefficient_mu 18.361 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.618 # Expt'l Tmin & Tmax _exptl_absorpt_correction_T_max 1.000 # scaled to Tmax=1.0 _exptl_absorpt_process_details ;Jacobson, R.A. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator ? _diffrn_radiation_collimation 'Confocal mirrors, HF VariMax ' _diffrn_source 'Rotating anode X-ray tube' _diffrn_source_type 'Rigaku FR-E+ SuperBright' _diffrn_measurement_device 'Four-circle \k diffractometer' _diffrn_measurement_device_type 'Rigaku AFC12 ' _diffrn_measurement_method 'Profile data from \w-scans' _diffrn_detector 'CCD plate' _diffrn_detector_type 'Rigaku HG Saturn724+ (2x2 bin mode)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2502 _diffrn_reflns_av_R_equivalents 0.0200 _diffrn_reflns_av_sigmaI/netI 0.0335 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 26.37 _reflns_number_total 1387 _reflns_number_gt 1261 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _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^)+(0.0140P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1387 _refine_ls_number_parameters 54 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0226 _refine_ls_R_factor_gt 0.0198 _refine_ls_wR_factor_ref 0.0362 _refine_ls_wR_factor_gt 0.0355 _refine_ls_goodness_of_fit_ref 0.951 _refine_ls_restrained_S_all 0.951 _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 0.0000 0.0000 0.0000 0.01112(8) Uani 1 2 d S . . Br1 Br -0.08456(6) 0.12865(3) 0.21484(4) 0.01865(10) Uani 1 1 d . . . Br2 Br 0.36849(6) -0.04247(3) 0.22399(5) 0.01952(10) Uani 1 1 d . . . Se1 Se -0.19299(6) -0.16568(3) 0.12068(4) 0.01417(9) Uani 1 1 d . . . C1 C -0.0925(6) -0.1348(3) 0.3563(4) 0.0200(9) Uani 1 1 d . . . H1A H -0.1083 -0.1950 0.4196 0.030 Uiso 1 1 calc R . . H1B H -0.1740 -0.0784 0.3804 0.030 Uiso 1 1 calc R . . H1C H 0.0554 -0.1155 0.3875 0.030 Uiso 1 1 calc R . . C2 C 0.0096(6) -0.2720(2) 0.1247(5) 0.0217(9) Uani 1 1 d . . . H2A H 0.1514 -0.2441 0.1671 0.033 Uiso 1 1 calc R . . H2B H -0.0137 -0.2981 0.0122 0.033 Uiso 1 1 calc R . . H2C H -0.0067 -0.3276 0.1968 0.033 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 0.01097(18) 0.01039(16) 0.01253(17) -0.00026(13) 0.00440(13) 0.00107(12) Br1 0.0234(2) 0.01685(19) 0.0181(2) -0.00334(16) 0.00992(17) 0.00263(15) Br2 0.0131(2) 0.01865(19) 0.0240(2) 0.00161(17) 0.00168(16) 0.00108(15) Se1 0.0141(2) 0.01382(18) 0.01485(19) 0.00044(15) 0.00489(16) -0.00094(14) C1 0.023(2) 0.022(2) 0.0141(19) -0.0009(17) 0.0047(17) -0.0032(16) C2 0.026(2) 0.0148(19) 0.028(2) 0.0037(17) 0.0134(19) 0.0025(16) _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 2.6726(7) 3 ? Te1 Br1 2.6726(7) . ? Te1 Br2 2.6745(8) . ? Te1 Br2 2.6745(8) 3 ? Te1 Se1 2.8789(7) . ? Te1 Se1 2.8789(7) 3 ? Se1 C2 1.944(3) . ? Se1 C1 1.946(3) . ? 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 Br1 180.000(19) 3 . ? Br1 Te1 Br2 90.45(2) 3 . ? Br1 Te1 Br2 89.55(2) . . ? Br1 Te1 Br2 89.55(2) 3 3 ? Br1 Te1 Br2 90.45(2) . 3 ? Br2 Te1 Br2 180.000(15) . 3 ? Br1 Te1 Se1 88.77(2) 3 . ? Br1 Te1 Se1 91.23(2) . . ? Br2 Te1 Se1 90.54(2) . . ? Br2 Te1 Se1 89.46(2) 3 . ? Br1 Te1 Se1 91.23(2) 3 3 ? Br1 Te1 Se1 88.77(2) . 3 ? Br2 Te1 Se1 89.46(2) . 3 ? Br2 Te1 Se1 90.54(2) 3 3 ? Se1 Te1 Se1 180.000(9) . 3 ? C2 Se1 C1 96.47(16) . . ? C2 Se1 Te1 99.19(11) . . ? C1 Se1 Te1 98.99(11) . . ? Se1 C1 H1A 109.5 . . ? Se1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Se1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Se1 C2 H2A 109.5 . . ? Se1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Se1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 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 # Se1 Te1 Se1 C2 -157.76(12) 3 . . . ? Br1 Te1 Se1 C2 41.92(12) 3 . . . ? Br1 Te1 Se1 C2 -138.08(12) . . . . ? Br2 Te1 Se1 C2 -48.51(12) . . . . ? Br2 Te1 Se1 C2 131.49(12) 3 . . . ? Br1 Te1 Se1 C1 140.04(12) 3 . . . ? Br1 Te1 Se1 C1 -39.96(12) . . . . ? Br2 Te1 Se1 C1 49.60(12) . . . . ? Br2 Te1 Se1 C1 -130.40(12) 3 . . . ? # Se1 Te1 Se1 C1 -59.64(12) 3 . . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Se1 Br1 3.574(1) . 2_445 ? Se1 Br2 3.697(1) . 1_455 ? _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.949 _refine_diff_density_max 0.466 _refine_diff_density_min -0.566 _refine_diff_density_rms 0.130 data_11aj0108 _database_code_depnum_ccdc_archive 'CCDC 881031' #TrackingRef '- Te_all15_3.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2011-12-30 _audit_author_name 'Webster, M.' _chemical_name_systematic ; tetrachloro(1,3-Bis(methylsulfanyl)propane-S,S')tellurium(IV) ; # MeS(CH2)3SMe = C5H12S2 # 2,6-dithiaheptane # 1,3-Bis(methylsulfanyl)propane (Chemspider IUPAC) # 1,3-Bis(methylthio)propane (Chemspider & iLab defaults) # 1,3-bis(methylsulfanyl)propane (iLab selected options) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C5 H12 Cl4 S2 Te' _chemical_formula_sum 'C5 H12 Cl4 S2 Te' _chemical_formula_weight 405.67 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' _space_group_crystal_system tetragonal _space_group_name_H-M_alt 'I 41/a' _space_group_IT_number 88 _space_group_name_Hall '-I 4ad' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x+1/2, -y, z+1/2' 3 '-y+3/4, x+1/4, z+1/4' 4 'y+3/4, -x+3/4, z+3/4' 5 'x+1/2, y+1/2, z+1/2' 6 '-x+1, -y+1/2, z+1' 7 '-y+5/4, x+3/4, z+3/4' 8 'y+5/4, -x+5/4, z+5/4' 9 '-x, -y, -z' 10 'x-1/2, y, -z-1/2' 11 'y-3/4, -x-1/4, -z-1/4' 12 '-y-3/4, x-3/4, -z-3/4' 13 '-x+1/2, -y+1/2, -z+1/2' 14 'x, y+1/2, -z' 15 'y-1/4, -x+1/4, -z+1/4' 16 '-y-1/4, x-1/4, -z-1/4' _cell_length_a 9.881(3) _cell_length_b 9.881(3) _cell_length_c 26.388(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2576.4(14) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3122 _cell_measurement_theta_min 2.9 _cell_measurement_theta_max 31.3 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.092 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 3.416 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.808 # Expt'l Tmin & Tmax _exptl_absorpt_correction_T_max 1.000 # scaled to Tmax=1.0 _exptl_absorpt_process_details ; Jacobson, R.A. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator ? _diffrn_radiation_collimation 'Confocal mirrors, HF VariMax' _diffrn_source 'Rotating anode X-ray tube' _diffrn_source_type 'Rigaku FR-E+ SuperBright' _diffrn_measurement_device 'Four-circle \k diffractometer' _diffrn_measurement_device_type 'Rigaku AFC12' _diffrn_measurement_method 'Profile data from \w-scans' _diffrn_detector 'CCD plate' _diffrn_detector_type 'Rigaku HG Saturn724+ (2x2 bin mode)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12362 _diffrn_reflns_av_R_equivalents 0.0544 _diffrn_reflns_av_sigmaI/netI 0.0333 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 28.27 _reflns_number_total 1596 _reflns_number_gt 1575 _reflns_threshold_expression I>\s(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _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^+19.5788P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 1596 _refine_ls_number_parameters 58 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0423 _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_ref 0.0670 _refine_ls_wR_factor_gt 0.0668 _refine_ls_goodness_of_fit_ref 1.211 _refine_ls_restrained_S_all 1.211 _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 0.5000 0.2500 0.622475(16) 0.01375(11) Uani 1 2 d S . . Cl1 Cl 0.57617(15) 0.08777(15) 0.55938(5) 0.0218(3) Uani 1 1 d . . . Cl2 Cl 0.72479(14) 0.36620(15) 0.62623(5) 0.0210(3) Uani 1 1 d . . . S1 S 0.59825(14) 0.08623(14) 0.70421(5) 0.0170(3) Uani 1 1 d . . . C1 C 0.5000 0.2500 0.7809(2) 0.0215(14) Uani 1 2 d S . . H1A H 0.5780 0.2293 0.8031 0.026 Uiso 0.50 1 calc PR . . H1B H 0.4220 0.2707 0.8031 0.026 Uiso 0.50 1 calc PR . . C2 C 0.4666(5) 0.1237(5) 0.7505(2) 0.0200(12) Uani 1 1 d . . . H2A H 0.3793 0.1369 0.7328 0.024 Uiso 1 1 calc R . . H2B H 0.4565 0.0460 0.7739 0.024 Uiso 1 1 calc R . . C3 C 0.5422(6) -0.0785(5) 0.6844(2) 0.0200(12) Uani 1 1 d . . . H3A H 0.5506 -0.1422 0.7126 0.030 Uiso 1 1 calc R . . H3B H 0.5981 -0.1096 0.6560 0.030 Uiso 1 1 calc R . . H3C H 0.4474 -0.0735 0.6736 0.030 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 0.0148(2) 0.0153(2) 0.01112(18) 0.000 0.000 0.0001(2) Cl1 0.0281(8) 0.0190(7) 0.0184(6) -0.0026(5) 0.0064(5) 0.0008(6) Cl2 0.0170(6) 0.0245(7) 0.0214(6) -0.0014(6) 0.0002(5) -0.0028(6) S1 0.0152(6) 0.0189(7) 0.0168(6) 0.0005(5) 0.0002(5) 0.0026(6) C1 0.026(4) 0.025(4) 0.013(3) 0.000 0.000 0.004(4) C2 0.023(3) 0.022(3) 0.015(2) 0.004(2) 0.005(2) 0.005(2) C3 0.023(3) 0.012(3) 0.025(3) 0.002(2) -0.002(2) 0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Te1 Cl1 2.4307(15) 6_554 ? Te1 Cl1 2.4307(15) . ? Te1 Cl2 2.5023(16) . ? Te1 Cl2 2.5023(16) 6_554 ? Te1 S1 2.8658(15) . ? Te1 S1 2.8658(15) 6_554 ? S1 C3 1.798(6) . ? S1 C2 1.824(5) . ? C1 C2 1.519(6) . ? C1 C2 1.519(6) 6_554 ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 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 Cl1 93.53(7) 6_554 . ? Cl1 Te1 Cl2 89.96(5) 6_554 . ? Cl1 Te1 Cl2 93.15(5) . . ? Cl1 Te1 Cl2 93.15(5) 6_554 6_554 ? Cl1 Te1 Cl2 89.96(5) . 6_554 ? Cl2 Te1 Cl2 175.46(6) . 6_554 ? Cl1 Te1 S1 173.12(5) 6_554 . ? Cl1 Te1 S1 92.19(5) . . ? Cl2 Te1 S1 85.90(4) . . ? Cl2 Te1 S1 90.68(4) 6_554 . ? Cl1 Te1 S1 92.19(5) 6_554 6_554 ? Cl1 Te1 S1 173.12(5) . 6_554 ? Cl2 Te1 S1 90.68(4) . 6_554 ? Cl2 Te1 S1 85.90(4) 6_554 6_554 ? S1 Te1 S1 82.37(6) . 6_554 ? C3 S1 C2 99.2(3) . . ? C3 S1 Te1 100.81(18) . . ? C2 S1 Te1 98.52(18) . . ? C2 C1 C2 116.3(6) . 6_554 ? C2 C1 H1A 108.2 . . ? C2 C1 H1A 108.2 6_554 . ? C2 C1 H1B 108.2 . . ? C2 C1 H1B 108.2 6_554 . ? H1A C1 H1B 107.4 . . ? C1 C2 S1 111.4(3) . . ? C1 C2 H2A 109.3 . . ? S1 C2 H2A 109.3 . . ? C1 C2 H2B 109.3 . . ? S1 C2 H2B 109.3 . . ? H2A C2 H2B 108.0 . . ? S1 C3 H3A 109.5 . . ? S1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? S1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 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 # Cl1 Te1 S1 C3 170.0(4) 6_554 . . . ? # Cl1 Te1 S1 C2 68.9(4) 6_554 . . . ? Cl1 Te1 S1 C3 -43.8(2) . . . . ? Cl2 Te1 S1 C3 -136.78(19) . . . . ? Cl2 Te1 S1 C3 46.2(2) 6_554 . . . ? S1 Te1 S1 C3 132.0(2) 6_554 . . . ? Cl1 Te1 S1 C2 -144.91(18) . . . . ? Cl2 Te1 S1 C2 122.09(18) . . . . ? Cl2 Te1 S1 C2 -54.92(18) 6_554 . . . ? S1 Te1 S1 C2 30.86(18) 6_554 . . . ? C2 C1 C2 S1 52.8(2) 6_554 . . . ? C3 S1 C2 C1 170.4(4) . . . . ? Te1 S1 C2 C1 -87.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.656 _refine_diff_density_min -0.800 _refine_diff_density_rms 0.132 data_12aj001ri _database_code_depnum_ccdc_archive 'CCDC 881032' #TrackingRef '- Te_all15_3.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2012-02-03 _audit_author_name 'Webster, M.' _chemical_name_systematic ; trans-tetrachlorobis(methylselanylmethane-Se)tellurium(IV) ; # Me2Se = C2H6Se # dimethylselenide (chemspider) # methylselanylmethane (chemspider IUPAC name) # dimethyl selenide (chemspider) # (methylseleno)methane (iLab (defaults)) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H12 Cl4 Se2 Te' _chemical_formula_sum 'C4 H12 Cl4 Se2 Te' _chemical_formula_weight 487.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 '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' _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'P 21/n' _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' loop_ _space_group_symop_operation_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 6.487(2) _cell_length_b 12.872(4) _cell_length_c 8.215(3) _cell_angle_alpha 90.00 _cell_angle_beta 108.245(8) _cell_angle_gamma 90.00 _cell_volume 651.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2866 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.485 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 448 _exptl_absorpt_coefficient_mu 8.641 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.786 # Expt'l Tmin & Tmax _exptl_absorpt_correction_T_max 1.000 # scaled to Tmax=1.0 _exptl_absorpt_process_details ; Jacobson, R.A. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator ? _diffrn_radiation_collimation 'Confocal mirrors, VHF VariMax ' _diffrn_source 'Rotating anode X-ray tube' _diffrn_source_type 'Rigaku FR-E+ Superbright' _diffrn_measurement_device 'Four-circle \k diffractometer' _diffrn_measurement_device_type 'Rigaku AFC12 ' _diffrn_measurement_method 'Profile data from \w-scans' _diffrn_detector 'CCD plate' _diffrn_detector_type 'Rigaku HG Saturn724+ (2x2 bin mode)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3103 _diffrn_reflns_av_R_equivalents 0.0191 _diffrn_reflns_av_sigmaI/netI 0.0237 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 27.47 _reflns_number_total 1475 _reflns_number_gt 1354 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0104P)^2^+0.5926P] 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 1475 _refine_ls_number_parameters 54 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0188 _refine_ls_R_factor_gt 0.0163 _refine_ls_wR_factor_ref 0.0342 _refine_ls_wR_factor_gt 0.0336 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _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 0.0000 0.0000 0.0000 0.00901(6) Uani 1 2 d S . . Cl1 Cl 0.35034(9) -0.04107(5) 0.22955(8) 0.01800(12) Uani 1 1 d . . . Cl2 Cl 0.09039(9) -0.12762(4) -0.19825(7) 0.01787(12) Uani 1 1 d . . . Se1 Se -0.21063(3) -0.164168(17) 0.12445(3) 0.01166(6) Uani 1 1 d . . . C1 C -0.1084(4) -0.12837(18) 0.3660(3) 0.0152(5) Uani 1 1 d . . . H1A H -0.1278 -0.1880 0.4340 0.023 Uiso 1 1 calc R . . H1B H -0.1917 -0.0691 0.3869 0.023 Uiso 1 1 calc R . . H1C H 0.0458 -0.1099 0.3990 0.023 Uiso 1 1 calc R . . C2 C -0.0008(4) -0.27298(17) 0.1316(3) 0.0171(5) Uani 1 1 d . . . H2A H 0.1463 -0.2445 0.1762 0.026 Uiso 1 1 calc R . . H2B H -0.0243 -0.3001 0.0158 0.026 Uiso 1 1 calc R . . H2C H -0.0185 -0.3292 0.2066 0.026 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 0.01008(10) 0.00745(10) 0.00971(10) -0.00014(7) 0.00341(7) 0.00058(8) Cl1 0.0127(3) 0.0173(3) 0.0208(3) 0.0023(2) 0.0007(2) 0.0002(2) Cl2 0.0250(3) 0.0147(3) 0.0164(3) -0.0023(2) 0.0099(2) 0.0034(2) Se1 0.01251(11) 0.01060(12) 0.01165(11) 0.00052(8) 0.00344(9) -0.00120(8) C1 0.0175(11) 0.0164(12) 0.0122(11) 0.0011(9) 0.0054(9) 0.0019(10) C2 0.0215(12) 0.0074(11) 0.0240(13) 0.0006(9) 0.0094(10) 0.0024(9) _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 Cl2 2.5086(8) . ? Te1 Cl2 2.5086(8) 3 ? Te1 Cl1 2.5133(8) 3 ? Te1 Cl1 2.5133(8) . ? Te1 Se1 2.8727(6) . ? Te1 Se1 2.8727(6) 3 ? Se1 C1 1.940(2) . ? Se1 C2 1.941(2) . ? 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 Cl2 Te1 Cl2 180.00(3) . 3 ? Cl2 Te1 Cl1 89.48(3) . 3 ? Cl2 Te1 Cl1 90.52(3) 3 3 ? Cl2 Te1 Cl1 90.52(3) . . ? Cl2 Te1 Cl1 89.48(3) 3 . ? Cl1 Te1 Cl1 180.00(3) 3 . ? Cl2 Te1 Se1 89.04(3) . . ? Cl2 Te1 Se1 90.96(3) 3 . ? Cl1 Te1 Se1 90.15(2) 3 . ? Cl1 Te1 Se1 89.85(2) . . ? Cl2 Te1 Se1 90.96(3) . 3 ? Cl2 Te1 Se1 89.04(3) 3 3 ? Cl1 Te1 Se1 89.85(2) 3 3 ? Cl1 Te1 Se1 90.15(2) . 3 ? Se1 Te1 Se1 180.000(6) . 3 ? C1 Se1 C2 97.38(10) . . ? C1 Se1 Te1 98.10(7) . . ? C2 Se1 Te1 97.73(7) . . ? Se1 C1 H1A 109.5 . . ? Se1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Se1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Se1 C2 H2A 109.5 . . ? Se1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Se1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 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 # Se1 Te1 Se1 C1 -1(100) 3 . . . ? Cl2 Te1 Se1 C1 139.02(7) . . . . ? Cl2 Te1 Se1 C1 -40.98(7) 3 . . . ? Cl1 Te1 Se1 C1 -131.50(7) 3 . . . ? Cl1 Te1 Se1 C1 48.50(7) . . . . ? Cl2 Te1 Se1 C2 40.38(8) . . . . ? Cl2 Te1 Se1 C2 -139.62(8) 3 . . . ? Cl1 Te1 Se1 C2 129.85(8) 3 . . . ? Cl1 Te1 Se1 C2 -50.15(8) . . . . ? # Se1 Te1 Se1 C2 -100(100) 3 . . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Se1 Cl1 3.592(1) . 1_455 ? Se1 Cl2 3.485(1) . 4_556 ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.493 _refine_diff_density_min -0.520 _refine_diff_density_rms 0.102 data_11aj004r _database_code_depnum_ccdc_archive 'CCDC 881033' #TrackingRef '- Te_all15_3.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2012-02-23 _audit_author_name 'Webster, M.' _chemical_name_systematic ; 1,3-dibromo-1,1,3,3-tetramethyl-1\l^4^,3\l^4^-ditelluroxane dichloromethane solvate ; # \m~2~-oxo-bis(bromodimethyltellurium) # (Me2BrTe)2O = C4H12Br2OTe2 # 1,3-dibromo-1,1,3,3-tetramethyl-1l4,3l4-ditelluroxane (iLab defaults) # 1,3-dibromo-1,1,3,3-tetramethyl-1l4,3l4-ditelluroxane (iLab selected options) # -1l4,3l4- The '4' is superscript and 'l' is Greek lc lambda ie -1\l^4^- _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H12 Br2 O Te2, 0.6(C H2 Cl2)' _chemical_formula_sum 'C4.60 H13.20 Br2 Cl1.20 O Te2' _chemical_formula_weight 542.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M 'I a -3 d' _space_group_IT_number 230 _space_group_name_Hall '-I 4bd 2c 3' loop_ _space_group_symop_id # insert this and add number _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x+1/2, -y, z+1/2' 3 '-x, y+1/2, -z+1/2' 4 'x+1/2, -y+1/2, -z' 5 'z, x, y' 6 'z+1/2, -x+1/2, -y' 7 '-z+1/2, -x, y+1/2' 8 '-z, x+1/2, -y+1/2' 9 'y, z, x' 10 '-y, z+1/2, -x+1/2' 11 'y+1/2, -z+1/2, -x' 12 '-y+1/2, -z, x+1/2' 13 'y+3/4, x+1/4, -z+1/4' 14 '-y+3/4, -x+3/4, -z+3/4' 15 'y+1/4, -x+1/4, z+3/4' 16 '-y+1/4, x+3/4, z+1/4' 17 'x+3/4, z+1/4, -y+1/4' 18 '-x+1/4, z+3/4, y+1/4' 19 '-x+3/4, -z+3/4, -y+3/4' 20 'x+1/4, -z+1/4, y+3/4' 21 'z+3/4, y+1/4, -x+1/4' 22 'z+1/4, -y+1/4, x+3/4' 23 '-z+1/4, y+3/4, x+1/4' 24 '-z+3/4, -y+3/4, -x+3/4' 25 'x+1/2, y+1/2, z+1/2' 26 '-x+1, -y+1/2, z+1' 27 '-x+1/2, y+1, -z+1' 28 'x+1, -y+1, -z+1/2' 29 'z+1/2, x+1/2, y+1/2' 30 'z+1, -x+1, -y+1/2' 31 '-z+1, -x+1/2, y+1' 32 '-z+1/2, x+1, -y+1' 33 'y+1/2, z+1/2, x+1/2' 34 '-y+1/2, z+1, -x+1' 35 'y+1, -z+1, -x+1/2' 36 '-y+1, -z+1/2, x+1' 37 'y+5/4, x+3/4, -z+3/4' 38 '-y+5/4, -x+5/4, -z+5/4' 39 'y+3/4, -x+3/4, z+5/4' 40 '-y+3/4, x+5/4, z+3/4' 41 'x+5/4, z+3/4, -y+3/4' 42 '-x+3/4, z+5/4, y+3/4' 43 '-x+5/4, -z+5/4, -y+5/4' 44 'x+3/4, -z+3/4, y+5/4' 45 'z+5/4, y+3/4, -x+3/4' 46 'z+3/4, -y+3/4, x+5/4' 47 '-z+3/4, y+5/4, x+3/4' 48 '-z+5/4, -y+5/4, -x+5/4' 49 '-x, -y, -z' 50 'x-1/2, y, -z-1/2' 51 'x, -y-1/2, z-1/2' 52 '-x-1/2, y-1/2, z' 53 '-z, -x, -y' 54 '-z-1/2, x-1/2, y' 55 'z-1/2, x, -y-1/2' 56 'z, -x-1/2, y-1/2' 57 '-y, -z, -x' 58 'y, -z-1/2, x-1/2' 59 '-y-1/2, z-1/2, x' 60 'y-1/2, z, -x-1/2' 61 '-y-3/4, -x-1/4, z-1/4' 62 'y-3/4, x-3/4, z-3/4' 63 '-y-1/4, x-1/4, -z-3/4' 64 'y-1/4, -x-3/4, -z-1/4' 65 '-x-3/4, -z-1/4, y-1/4' 66 'x-1/4, -z-3/4, -y-1/4' 67 'x-3/4, z-3/4, y-3/4' 68 '-x-1/4, z-1/4, -y-3/4' 69 '-z-3/4, -y-1/4, x-1/4' 70 '-z-1/4, y-1/4, -x-3/4' 71 'z-1/4, -y-3/4, -x-1/4' 72 'z-3/4, y-3/4, x-3/4' 73 '-x+1/2, -y+1/2, -z+1/2' 74 'x, y+1/2, -z' 75 'x+1/2, -y, z' 76 '-x, y, z+1/2' 77 '-z+1/2, -x+1/2, -y+1/2' 78 '-z, x, y+1/2' 79 'z, x+1/2, -y' 80 'z+1/2, -x, y' 81 '-y+1/2, -z+1/2, -x+1/2' 82 'y+1/2, -z, x' 83 '-y, z, x+1/2' 84 'y, z+1/2, -x' 85 '-y-1/4, -x+1/4, z+1/4' 86 'y-1/4, x-1/4, z-1/4' 87 '-y+1/4, x+1/4, -z-1/4' 88 'y+1/4, -x-1/4, -z+1/4' 89 '-x-1/4, -z+1/4, y+1/4' 90 'x+1/4, -z-1/4, -y+1/4' 91 'x-1/4, z-1/4, y-1/4' 92 '-x+1/4, z+1/4, -y-1/4' 93 '-z-1/4, -y+1/4, x+1/4' 94 '-z+1/4, y+1/4, -x-1/4' 95 'z+1/4, -y-1/4, -x+1/4' 96 'z-1/4, y-1/4, x-1/4' _cell_length_a 25.509(3) _cell_length_b 25.509(3) _cell_length_c 25.509(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 16599(4) _cell_formula_units_Z 48 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 27804 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.603 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 11674 _exptl_absorpt_coefficient_mu 10.187 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.731 # Expt'l Tmin & Tmax _exptl_absorpt_correction_T_max 1.000 # scaled to Tmax=1.0 _exptl_absorpt_process_details ;Jacobson, R.A. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator ? _diffrn_radiation_collimation 'Confocal mirrors, VHF VariMax ' _diffrn_source 'Rotating anode X-ray tube' _diffrn_source_type 'Rigaku FR-E+ Superbright' _diffrn_measurement_device 'Four-circle \k diffractometer' _diffrn_measurement_device_type 'Rigaku AFC12 ' _diffrn_measurement_method 'Profile data from \w-scans' _diffrn_detector 'CCD plate' _diffrn_detector_type 'Rigaku HG Saturn724+ (2x2 bin mode)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34117 _diffrn_reflns_av_R_equivalents 0.0258 _diffrn_reflns_av_sigmaI/netI 0.0110 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.19 _diffrn_reflns_theta_max 27.46 _reflns_number_total 1585 _reflns_number_gt 1470 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. No H atoms were included with the disordered CH2Cl2 solvate. The C atom associated with Cl2, Cl3 could not be identified in difference ed maps. All Cl atoms and C3 were treated as isotropic. ; _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^)+(0.0374P)^2^+285.4000P] 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 1585 _refine_ls_number_parameters 54 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0312 _refine_ls_R_factor_gt 0.0291 _refine_ls_wR_factor_ref 0.0778 _refine_ls_wR_factor_gt 0.0766 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.003 _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 0.568750(12) 0.359026(12) 0.088041(12) 0.02036(12) Uani 1 1 d . . . Br1 Br 0.46736(2) 0.33718(2) 0.04288(2) 0.02990(15) Uani 1 1 d . . . O1 O 0.64233(14) 0.3750 0.10767(14) 0.0301(12) Uani 1 2 d S . . C1 C 0.5730(2) 0.4166(2) 0.0285(2) 0.0299(11) Uani 1 1 d . . . H1A H 0.5437 0.4411 0.0323 0.045 Uiso 1 1 calc R . . H1B H 0.5710 0.3995 -0.0059 0.045 Uiso 1 1 calc R . . H1C H 0.6062 0.4356 0.0314 0.045 Uiso 1 1 calc R . . C2 C 0.5967(2) 0.2963(2) 0.0426(2) 0.0321(12) Uani 1 1 d . . . H2A H 0.5986 0.3071 0.0058 0.048 Uiso 1 1 calc R . . H2B H 0.5728 0.2664 0.0460 0.048 Uiso 1 1 calc R . . H2C H 0.6316 0.2862 0.0549 0.048 Uiso 1 1 calc R . . Cl1 Cl 0.1250 0.5415(3) 0.7915(3) 0.110(2) Uiso 0.60 2 d SP . 1 C3 C 0.0807(17) 0.5000 0.7500 0.067(10) Uiso 0.30 2 d SP . 1 Cl2 Cl 0.1250 0.4817(2) 0.7683(2) 0.0639(18) Uiso 0.40 2 d SP . 2 Cl3 Cl 0.1160(4) 0.5640(4) 0.8336(4) 0.020(2) Uiso 0.10 1 d P . 2 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 0.02104(18) 0.01997(17) 0.02006(17) 0.00085(11) -0.00329(11) -0.00007(11) Br1 0.0221(3) 0.0305(3) 0.0371(3) 0.0041(2) -0.0062(2) -0.0038(2) O1 0.0225(15) 0.045(3) 0.0225(15) -0.0034(16) -0.0048(19) -0.0034(16) C1 0.035(3) 0.026(3) 0.028(3) 0.008(2) -0.007(2) -0.008(2) C2 0.030(3) 0.029(3) 0.038(3) -0.007(2) -0.003(2) 0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Te1 O1 1.985(3) . ? Te1 C2 2.099(5) . ? Te1 C1 2.115(5) . ? Te1 Br1 2.8858(7) . ? O1 Te1 1.985(3) 24 ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? Cl1 C3 1.88(3) . ? Cl1 C3 1.88(3) 18_545 ? C3 Cl1 1.88(3) 28_456 ? # Cl2 Cl2 1.322(16) 28_456 ? # Cl3 Cl3 0.84(2) 18_545 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag # C3 Cl1 C3 74(2) . 18_545 ? O1 Te1 C2 88.56(18) . . ? O1 Te1 C1 89.45(17) . . ? C2 Te1 C1 96.6(2) . . ? O1 Te1 Br1 171.08(13) . . ? C2 Te1 Br1 86.37(16) . . ? C1 Te1 Br1 83.86(15) . . ? Te1 O1 Te1 121.3(3) . 24 ? Te1 C1 H1A 109.5 . . ? Te1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Te1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Te1 C2 H2A 109.5 . . ? Te1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Te1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Cl1 C3 Cl1 106(2) . 28_456 ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl2 Cl3 2.859(11) . 28_456 ? Te1 Br1 3.422(1) . 55_656 ? Te1 Br1 3.639(1) . 88_565 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.965 _refine_diff_density_min -2.781 _refine_diff_density_rms 0.166 data_12aj006r _database_code_depnum_ccdc_archive 'CCDC 881034' #TrackingRef '- Te_all15_3.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2012-03-21 _audit_author_name 'Webster, M.' _chemical_name_systematic ; trans-tetrabromobis(tetrahydrothiophene)tellurium(IV) ; # C4H8S = THF or thf # tetrahydrothiophene (Chemspider) # tetrahydrothiophene (ACD iLab defaults & selected options) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H16 Br4 S2 Te' _chemical_formula_sum 'C8 H16 Br4 S2 Te' _chemical_formula_weight 623.57 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 8.624(2) _cell_length_b 7.5542(12) _cell_length_c 12.754(2) _cell_angle_alpha 90.00 _cell_angle_beta 109.630(5) _cell_angle_gamma 90.00 _cell_volume 782.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5079 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.646 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 576 _exptl_absorpt_coefficient_mu 12.350 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.729 # Expt'l Tmin & Tmax _exptl_absorpt_correction_T_max 1.000 # scaled to Tmax=1.0 _exptl_absorpt_process_details ;Jacobson, R.A. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator ? _diffrn_radiation_collimation 'Confocal mirrors, VHF VariMax ' _diffrn_source 'Rotating anode X-ray tube' _diffrn_source_type 'Rigaku FR-E+ Superbright' _diffrn_measurement_device 'Four-circle \k diffractometer' _diffrn_measurement_device_type 'Rigaku AFC12 ' _diffrn_measurement_method 'Profile data from \w-scans' _diffrn_detector 'CCD plate' _diffrn_detector_type 'Rigaku HG Saturn724+ (2x2 bin mode)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5336 _diffrn_reflns_av_R_equivalents 0.0243 _diffrn_reflns_av_sigmaI/netI 0.0248 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.19 _diffrn_reflns_theta_max 27.45 _reflns_number_total 1774 _reflns_number_gt 1677 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _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^)+(0.0201P)^2^+0.3723P] 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 1774 _refine_ls_number_parameters 70 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0198 _refine_ls_R_factor_gt 0.0181 _refine_ls_wR_factor_ref 0.0420 _refine_ls_wR_factor_gt 0.0414 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _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 0.0000 0.5000 0.0000 0.01012(7) Uani 1 2 d S . . Br1 Br 0.30795(3) 0.60063(3) 0.022693(19) 0.01453(7) Uani 1 1 d . . . Br2 Br -0.10643(3) 0.65867(3) -0.199593(19) 0.01715(7) Uani 1 1 d . . . S1 S -0.03445(7) 0.83090(8) 0.08121(5) 0.01421(12) Uani 1 1 d . . . C1 C -0.2536(3) 0.8815(3) 0.01162(19) 0.0143(5) Uani 1 1 d . . . H1A H -0.2671 0.9861 -0.0373 0.017 Uiso 1 1 calc R . . H1B H -0.3113 0.7797 -0.0337 0.017 Uiso 1 1 calc R . . C2 C -0.3208(3) 0.9186(3) 0.1054(2) 0.0164(5) Uani 1 1 d . . . H2A H -0.2967 1.0423 0.1315 0.020 Uiso 1 1 calc R . . H2B H -0.4416 0.9012 0.0793 0.020 Uiso 1 1 calc R . . C3 C -0.2376(3) 0.7905(4) 0.1990(2) 0.0170(5) Uani 1 1 d . . . H3A H -0.2787 0.6688 0.1780 0.020 Uiso 1 1 calc R . . H3B H -0.2605 0.8242 0.2674 0.020 Uiso 1 1 calc R . . C4 C -0.0534(3) 0.8001(4) 0.21883(19) 0.0173(5) Uani 1 1 d . . . H4A H 0.0018 0.6894 0.2535 0.021 Uiso 1 1 calc R . . H4B H -0.0030 0.9006 0.2683 0.021 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 0.00887(11) 0.01297(12) 0.00806(10) 0.00093(7) 0.00221(8) 0.00072(7) Br1 0.01057(12) 0.01719(14) 0.01495(12) -0.00001(9) 0.00314(9) -0.00117(8) Br2 0.01516(13) 0.02426(15) 0.01111(12) 0.00548(9) 0.00318(10) 0.00284(9) S1 0.0119(3) 0.0162(3) 0.0142(3) -0.0002(2) 0.0039(2) 0.0000(2) C1 0.0128(11) 0.0163(12) 0.0127(11) 0.0015(9) 0.0028(9) 0.0021(9) C2 0.0132(11) 0.0190(13) 0.0173(12) -0.0002(10) 0.0052(10) 0.0012(9) C3 0.0183(12) 0.0195(13) 0.0136(11) 0.0011(9) 0.0059(10) 0.0020(10) C4 0.0162(12) 0.0231(14) 0.0099(11) -0.0009(10) 0.0007(9) 0.0046(10) _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 2.6814(5) 3_565 ? Te1 Br2 2.6814(5) . ? Te1 Br1 2.6830(7) 3_565 ? Te1 Br1 2.6830(7) . ? Te1 S1 2.7598(7) . ? Te1 S1 2.7598(7) 3_565 ? S1 C4 1.831(2) . ? S1 C1 1.838(2) . ? C1 C2 1.520(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.517(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.524(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? 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 Br2 180.000(10) 3_565 . ? Br2 Te1 Br1 89.225(11) 3_565 3_565 ? Br2 Te1 Br1 90.775(11) . 3_565 ? Br2 Te1 Br1 90.775(11) 3_565 . ? Br2 Te1 Br1 89.225(11) . . ? Br1 Te1 Br1 180.0 3_565 . ? Br2 Te1 S1 95.407(17) 3_565 . ? Br2 Te1 S1 84.593(17) . . ? Br1 Te1 S1 93.993(15) 3_565 . ? Br1 Te1 S1 86.007(15) . . ? Br2 Te1 S1 84.593(17) 3_565 3_565 ? Br2 Te1 S1 95.407(17) . 3_565 ? Br1 Te1 S1 86.007(15) 3_565 3_565 ? Br1 Te1 S1 93.993(15) . 3_565 ? S1 Te1 S1 180.0 . 3_565 ? C4 S1 C1 94.64(11) . . ? C4 S1 Te1 107.46(9) . . ? C1 S1 Te1 103.29(8) . . ? C2 C1 S1 105.09(16) . . ? C2 C1 H1A 110.7 . . ? S1 C1 H1A 110.7 . . ? C2 C1 H1B 110.7 . . ? S1 C1 H1B 110.7 . . ? H1A C1 H1B 108.8 . . ? C3 C2 C1 107.26(19) . . ? C3 C2 H2A 110.3 . . ? C1 C2 H2A 110.3 . . ? C3 C2 H2B 110.3 . . ? C1 C2 H2B 110.3 . . ? H2A C2 H2B 108.5 . . ? C2 C3 C4 107.0(2) . . ? C2 C3 H3A 110.3 . . ? C4 C3 H3A 110.3 . . ? C2 C3 H3B 110.3 . . ? C4 C3 H3B 110.3 . . ? H3A C3 H3B 108.6 . . ? C3 C4 S1 105.70(15) . . ? C3 C4 H4A 110.6 . . ? S1 C4 H4A 110.6 . . ? C3 C4 H4B 110.6 . . ? S1 C4 H4B 110.6 . . ? H4A C4 H4B 108.7 . . ? 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 Te1 S1 C4 -158(83) 3_565 . . . ? # S1 Te1 S1 C1 103(83) 3_565 . . . ? Br2 Te1 S1 C4 -21.65(8) 3_565 . . . ? Br2 Te1 S1 C4 158.35(8) . . . . ? Br1 Te1 S1 C4 67.95(8) 3_565 . . . ? Br1 Te1 S1 C4 -112.05(8) . . . . ? Br2 Te1 S1 C1 -120.94(8) 3_565 . . . ? Br2 Te1 S1 C1 59.06(8) . . . . ? Br1 Te1 S1 C1 -31.34(8) 3_565 . . . ? Br1 Te1 S1 C1 148.66(8) . . . . ? C4 S1 C1 C2 14.45(18) . . . . ? Te1 S1 C1 C2 123.63(15) . . . . ? S1 C1 C2 C3 -37.9(2) . . . . ? C1 C2 C3 C4 49.0(3) . . . . ? C2 C3 C4 S1 -36.2(2) . . . . ? C1 S1 C4 C3 12.29(19) . . . . ? Te1 S1 C4 C3 -93.21(17) . . . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag S1 S1 3.464(1) . 3_575 ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.643 _refine_diff_density_min -0.892 _refine_diff_density_rms 0.112 data_2 _database_code_depnum_ccdc_archive 'CCDC 881035' #TrackingRef 'UJANA.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H16 O' _chemical_formula_weight 296.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.9052(2) _cell_length_b 10.4099(3) _cell_length_c 15.6229(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.067(2) _cell_angle_gamma 90.00 _cell_volume 1586.11(7) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 4178 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 27.28 _exptl_crystal_description rectanguler _exptl_crystal_colour yellowish _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.38 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.241 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 624 _exptl_absorpt_coefficient_mu 0.075 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8721 _exptl_absorpt_correction_T_max 0.9139 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 12878 _diffrn_reflns_av_R_equivalents 0.0241 _diffrn_reflns_av_sigmaI/netI 0.0267 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3635 _reflns_number_gt 2640 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0754P)^2^+0.2796P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0046(14) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3635 _refine_ls_number_parameters 210 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0697 _refine_ls_R_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.1502 _refine_ls_wR_factor_gt 0.1362 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 O1 O 1.14541(11) 0.87162(12) 0.13860(9) 0.0661(4) Uani 1 1 d . . . C1 C 0.9614(2) 1.19533(19) 0.32099(12) 0.0690(5) Uani 1 1 d . . . H1 H 0.9482 1.2577 0.3613 0.083 Uiso 1 1 calc R . . C2 C 0.85857(18) 1.10969(17) 0.29139(10) 0.0557(4) Uani 1 1 d . . . H2 H 0.7759 1.1139 0.3117 0.067 Uiso 1 1 calc R . . C3 C 0.87804(14) 1.01752(15) 0.23152(9) 0.0442(4) Uani 1 1 d . . . H3 H 0.8076 0.9605 0.2109 0.053 Uiso 1 1 calc R . . C4 C 1.00150(13) 1.00878(14) 0.20153(9) 0.0404(3) Uani 1 1 d . . . C5 C 1.02847(14) 0.90491(14) 0.14150(10) 0.0440(3) Uani 1 1 d . . . C6 C 0.90896(14) 0.84389(14) 0.08352(9) 0.0420(3) Uani 1 1 d . . . C7 C 0.89604(15) 0.70592(14) 0.07491(9) 0.0423(3) Uani 1 1 d . . . C8 C 0.78427(16) 0.65389(15) 0.01611(9) 0.0446(4) Uani 1 1 d . . . C9 C 0.76921(19) 0.51902(16) 0.01260(11) 0.0549(4) Uani 1 1 d . . . H9 H 0.6962 0.4840 -0.0259 0.066 Uiso 1 1 calc R . . C10 C 0.8578(2) 0.43761(16) 0.06361(11) 0.0582(5) Uani 1 1 d . . . C11 C 0.8377(3) 0.29438(16) 0.05977(14) 0.0782(6) Uani 1 1 d . . . H11A H 0.7635 0.2735 0.0136 0.117 Uiso 1 1 calc R . . H11B H 0.8165 0.2645 0.1140 0.117 Uiso 1 1 calc R . . H11C H 0.9202 0.2537 0.0492 0.117 Uiso 1 1 calc R . . C12 C 0.98692(17) 0.62169(15) 0.12629(10) 0.0512(4) Uani 1 1 d . . . H12 H 1.0613 0.6547 0.1646 0.061 Uiso 1 1 calc R . . C13 C 0.96724(19) 0.49017(17) 0.12061(11) 0.0588(5) Uani 1 1 d . . . H13 H 1.0283 0.4361 0.1555 0.071 Uiso 1 1 calc R . . C14 C 0.68751(16) 0.73906(15) -0.03740(9) 0.0457(4) Uani 1 1 d . . . C15 C 0.57814(19) 0.69520(18) -0.09947(11) 0.0635(5) Uani 1 1 d . . . H15 H 0.5653 0.6074 -0.1082 0.076 Uiso 1 1 calc R . . C16 C 0.4896(2) 0.7795(2) -0.14757(13) 0.0722(6) Uani 1 1 d . . . H16 H 0.4177 0.7479 -0.1885 0.087 Uiso 1 1 calc R . . C17 C 0.50508(18) 0.9108(2) -0.13640(11) 0.0645(5) Uani 1 1 d . . . H17 H 0.4438 0.9670 -0.1692 0.077 Uiso 1 1 calc R . . C18 C 0.61186(17) 0.95724(17) -0.07641(10) 0.0552(4) Uani 1 1 d . . . H18 H 0.6230 1.0455 -0.0688 0.066 Uiso 1 1 calc R . . C19 C 0.70399(15) 0.87337(15) -0.02661(9) 0.0450(4) Uani 1 1 d . . . C20 C 0.81489(15) 0.92252(14) 0.03510(10) 0.0451(4) Uani 1 1 d . . . H20 H 0.8235 1.0109 0.0427 0.054 Uiso 1 1 calc R . . C21 C 1.10521(16) 1.09567(17) 0.23237(11) 0.0570(4) Uani 1 1 d . . . H21 H 1.1889 1.0907 0.2134 0.068 Uiso 1 1 calc R . . C22 C 1.0840(2) 1.18919(19) 0.29115(13) 0.0723(6) Uani 1 1 d . . . H22 H 1.1529 1.2484 0.3107 0.087 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 O1 0.0420(6) 0.0623(8) 0.0922(9) -0.0150(7) 0.0071(6) 0.0089(5) C1 0.0788(13) 0.0664(12) 0.0599(11) -0.0226(9) 0.0074(9) -0.0015(10) C2 0.0547(9) 0.0647(11) 0.0485(9) -0.0056(8) 0.0107(7) 0.0041(8) C3 0.0403(7) 0.0462(8) 0.0436(8) -0.0001(7) 0.0003(6) -0.0031(6) C4 0.0380(7) 0.0383(7) 0.0420(7) 0.0007(6) -0.0009(6) -0.0007(6) C5 0.0394(8) 0.0405(8) 0.0509(8) 0.0023(7) 0.0046(6) 0.0011(6) C6 0.0427(8) 0.0395(8) 0.0441(8) -0.0036(6) 0.0084(6) -0.0002(6) C7 0.0480(8) 0.0390(8) 0.0418(7) -0.0012(6) 0.0132(6) 0.0021(6) C8 0.0555(9) 0.0428(8) 0.0374(7) -0.0064(6) 0.0137(6) -0.0055(7) C9 0.0761(11) 0.0444(9) 0.0462(8) -0.0044(7) 0.0160(8) -0.0043(8) C10 0.0870(13) 0.0386(9) 0.0557(10) -0.0013(8) 0.0306(9) 0.0012(8) C11 0.1201(17) 0.0402(10) 0.0825(13) 0.0003(9) 0.0404(13) -0.0012(10) C12 0.0533(9) 0.0481(9) 0.0522(9) 0.0038(8) 0.0098(7) 0.0085(7) C13 0.0715(11) 0.0485(9) 0.0594(10) 0.0087(8) 0.0197(9) 0.0147(8) C14 0.0555(9) 0.0434(8) 0.0390(7) -0.0044(7) 0.0102(6) -0.0055(7) C15 0.0714(11) 0.0576(10) 0.0563(10) -0.0107(9) -0.0029(9) -0.0088(9) C16 0.0672(12) 0.0797(14) 0.0608(11) -0.0108(10) -0.0136(9) -0.0065(10) C17 0.0594(10) 0.0736(12) 0.0545(10) 0.0005(9) -0.0074(8) 0.0103(9) C18 0.0560(9) 0.0532(10) 0.0535(9) 0.0019(8) 0.0019(7) 0.0054(8) C19 0.0470(8) 0.0464(8) 0.0410(7) -0.0012(7) 0.0063(6) 0.0001(6) C20 0.0475(8) 0.0360(7) 0.0499(8) -0.0044(7) 0.0032(6) -0.0004(6) C21 0.0434(8) 0.0592(10) 0.0666(10) -0.0111(9) 0.0045(7) -0.0099(7) C22 0.0680(12) 0.0670(12) 0.0780(13) -0.0252(10) 0.0018(10) -0.0218(10) _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 O1 C5 1.2175(17) . ? C1 C2 1.372(2) . ? C1 C22 1.376(3) . ? C1 H1 0.9300 . ? C2 C3 1.377(2) . ? C2 H2 0.9300 . ? C3 C4 1.3870(19) . ? C3 H3 0.9300 . ? C4 C21 1.390(2) . ? C4 C5 1.486(2) . ? C5 C6 1.5001(19) . ? C6 C20 1.365(2) . ? C6 C7 1.446(2) . ? C7 C12 1.404(2) . ? C7 C8 1.417(2) . ? C8 C9 1.412(2) . ? C8 C14 1.457(2) . ? C9 C10 1.370(2) . ? C9 H9 0.9300 . ? C10 C13 1.390(3) . ? C10 C11 1.504(2) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C13 1.384(2) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C15 1.398(2) . ? C14 C19 1.414(2) . ? C15 C16 1.369(3) . ? C15 H15 0.9300 . ? C16 C17 1.383(3) . ? C16 H16 0.9300 . ? C17 C18 1.373(2) . ? C17 H17 0.9300 . ? C18 C19 1.397(2) . ? C18 H18 0.9300 . ? C19 C20 1.424(2) . ? C20 H20 0.9300 . ? C21 C22 1.379(2) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C22 120.19(17) . . ? C2 C1 H1 119.9 . . ? C22 C1 H1 119.9 . . ? C1 C2 C3 119.87(16) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C2 C3 C4 120.77(14) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C3 C4 C21 118.82(14) . . ? C3 C4 C5 121.83(13) . . ? C21 C4 C5 119.26(13) . . ? O1 C5 C4 120.52(13) . . ? O1 C5 C6 120.83(14) . . ? C4 C5 C6 118.64(12) . . ? C20 C6 C7 120.21(13) . . ? C20 C6 C5 118.08(13) . . ? C7 C6 C5 121.62(13) . . ? C12 C7 C8 118.84(14) . . ? C12 C7 C6 121.98(14) . . ? C8 C7 C6 119.10(13) . . ? C9 C8 C7 118.07(15) . . ? C9 C8 C14 121.89(14) . . ? C7 C8 C14 120.03(13) . . ? C10 C9 C8 122.67(16) . . ? C10 C9 H9 118.7 . . ? C8 C9 H9 118.7 . . ? C9 C10 C13 118.53(15) . . ? C9 C10 C11 121.54(19) . . ? C13 C10 C11 119.93(18) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C7 120.81(16) . . ? C13 C12 H12 119.6 . . ? C7 C12 H12 119.6 . . ? C12 C13 C10 121.08(16) . . ? C12 C13 H13 119.5 . . ? C10 C13 H13 119.5 . . ? C15 C14 C19 117.70(15) . . ? C15 C14 C8 123.46(15) . . ? C19 C14 C8 118.85(13) . . ? C16 C15 C14 121.04(17) . . ? C16 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C15 C16 C17 121.21(16) . . ? C15 C16 H16 119.4 . . ? C17 C16 H16 119.4 . . ? C18 C17 C16 119.31(17) . . ? C18 C17 H17 120.3 . . ? C16 C17 H17 120.3 . . ? C17 C18 C19 120.69(17) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C18 C19 C14 120.06(14) . . ? C18 C19 C20 120.26(14) . . ? C14 C19 C20 119.69(14) . . ? C6 C20 C19 122.05(14) . . ? C6 C20 H20 119.0 . . ? C19 C20 H20 119.0 . . ? C22 C21 C4 120.05(16) . . ? C22 C21 H21 120.0 . . ? C4 C21 H21 120.0 . . ? C1 C22 C21 120.28(17) . . ? C1 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.213 _refine_diff_density_min -0.166 _refine_diff_density_rms 0.038 data_12aj004r _database_code_depnum_ccdc_archive 'CCDC 881036' #TrackingRef '- Te_all15_3.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2012-03-22 _audit_author_name 'Webster, M.' _chemical_name_systematic ; di(\m~2~-bromo)bis(tetrahydrothiophene)-bis(tribromotellurium(IV)) ; # C4H8S = THF or thf # tetrahydrothiophene (Chemspider) # tetrahydrothiophene (ACD iLab defaults & selected options) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H16 Br8 S2 Te2' _chemical_formula_sum 'C8 H16 Br8 S2 Te2' _chemical_formula_weight 1070.81 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 8.502(3) _cell_length_b 8.623(3) _cell_length_c 8.734(3) _cell_angle_alpha 71.099(5) _cell_angle_beta 87.043(6) _cell_angle_gamma 72.783(5) _cell_volume 577.9(3) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4959 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.077 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 480 _exptl_absorpt_coefficient_mu 16.523 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.726 # Expt'l Tmin & Tmax _exptl_absorpt_correction_T_max 1.000 # scaled to Tmax=1.0 _exptl_absorpt_process_details ; Jacobson, R.A. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator ? _diffrn_radiation_collimation 'Confocal mirrors, VHF VariMax ' _diffrn_source 'Rotating anode X-ray tube' _diffrn_source_type 'Rigaku FR-E+ Superbright' _diffrn_measurement_device 'Four-circle \k diffractometer' _diffrn_measurement_device_type 'Rigaku AFC12 ' _diffrn_measurement_method 'Profile data from \w-scans' _diffrn_detector 'CCD plate' _diffrn_detector_type 'Rigaku HG Saturn724+ (2x2 bin mode)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5419 _diffrn_reflns_av_R_equivalents 0.0230 _diffrn_reflns_av_sigmaI/netI 0.0292 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2630 _reflns_number_gt 2410 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _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 'calc w=1/[\s^2^(Fo^2^)+(0.0096P)^2^+0.4665P] 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 2630 _refine_ls_number_parameters 91 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0218 _refine_ls_R_factor_gt 0.0187 _refine_ls_wR_factor_ref 0.0382 _refine_ls_wR_factor_gt 0.0373 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _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 0.85667(2) 0.40042(2) 0.18758(2) 0.01012(5) Uani 1 1 d . . . Br1 Br 0.58926(3) 0.32515(3) 0.19295(3) 0.01512(7) Uani 1 1 d . . . Br2 Br 1.04022(4) 0.09101(4) 0.23158(4) 0.02298(8) Uani 1 1 d . . . Br3 Br 0.85278(3) 0.36557(4) 0.48734(3) 0.01586(7) Uani 1 1 d . . . Br4 Br 0.85048(3) 0.48064(4) -0.16402(3) 0.01592(7) Uani 1 1 d . . . S1 S 0.64755(8) 0.74827(9) 0.11135(9) 0.01424(14) Uani 1 1 d . . . C1 C 0.7552(4) 0.8519(4) 0.2056(4) 0.0204(6) Uani 1 1 d . . . H1A H 0.8740 0.7879 0.2242 0.025 Uiso 1 1 calc R . . H1B H 0.7434 0.9711 0.1351 0.025 Uiso 1 1 calc R . . C2 C 0.6754(4) 0.8509(4) 0.3661(4) 0.0224(7) Uani 1 1 d . . . H2A H 0.7248 0.7399 0.4515 0.027 Uiso 1 1 calc R . . H2B H 0.6910 0.9441 0.4007 0.027 Uiso 1 1 calc R . . C3 C 0.4938(4) 0.8777(4) 0.3368(4) 0.0219(6) Uani 1 1 d . . . H3A H 0.4402 0.9966 0.2666 0.026 Uiso 1 1 calc R . . H3B H 0.4382 0.8572 0.4408 0.026 Uiso 1 1 calc R . . C4 C 0.4827(3) 0.7502(4) 0.2546(4) 0.0204(6) Uani 1 1 d . . . H4A H 0.3738 0.7871 0.1971 0.025 Uiso 1 1 calc R . . H4B H 0.4991 0.6347 0.3351 0.025 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 0.00929(9) 0.01119(9) 0.01050(9) -0.00416(7) 0.00026(6) -0.00317(6) Br1 0.01186(13) 0.01590(13) 0.01787(15) -0.00347(11) -0.00148(10) -0.00630(11) Br2 0.01661(15) 0.01399(14) 0.03616(19) -0.00891(13) -0.00215(12) 0.00009(11) Br3 0.01773(14) 0.01975(14) 0.00984(14) -0.00344(11) -0.00062(10) -0.00645(11) Br4 0.01273(13) 0.02625(15) 0.01284(14) -0.00958(12) 0.00182(10) -0.00826(11) S1 0.0148(3) 0.0142(3) 0.0141(3) -0.0057(3) 0.0012(3) -0.0037(3) C1 0.0148(14) 0.0190(14) 0.0337(19) -0.0158(13) 0.0023(12) -0.0062(12) C2 0.0280(17) 0.0177(14) 0.0211(16) -0.0103(13) -0.0048(13) -0.0007(12) C3 0.0267(16) 0.0200(15) 0.0191(16) -0.0070(12) 0.0073(12) -0.0073(13) C4 0.0122(14) 0.0236(15) 0.0278(18) -0.0113(13) 0.0090(12) -0.0066(12) _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 Br3 2.5364(9) . ? Te1 Br1 2.5367(7) . ? Te1 Br2 2.5757(7) . ? Te1 S1 2.8761(10) . ? Te1 Br4 2.9208(11) . ? Te1 Br4 2.9350(8) 2_765 ? Br4 Te1 2.9350(8) 2_765 ? S1 C4 1.830(3) . ? S1 C1 1.831(3) . ? C1 C2 1.524(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.514(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.521(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? 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 Br3 Te1 Br1 92.321(12) . . ? Br3 Te1 Br2 93.918(13) . . ? Br1 Te1 Br2 94.08(2) . . ? Br3 Te1 S1 90.686(18) . . ? Br1 Te1 S1 84.92(3) . . ? Br2 Te1 S1 175.326(18) . . ? Br3 Te1 Br4 173.786(11) . . ? Br1 Te1 Br4 89.324(12) . . ? Br2 Te1 Br4 91.940(13) . . ? S1 Te1 Br4 83.488(17) . . ? Br3 Te1 Br4 89.494(11) . 2_765 ? Br1 Te1 Br4 174.815(11) . 2_765 ? Br2 Te1 Br4 90.64(2) . 2_765 ? S1 Te1 Br4 90.21(3) . 2_765 ? Br4 Te1 Br4 88.370(11) . 2_765 ? Te1 Br4 Te1 91.630(11) . 2_765 ? C4 S1 C1 94.07(14) . . ? C4 S1 Te1 107.71(10) . . ? C1 S1 Te1 104.83(10) . . ? C2 C1 S1 106.3(2) . . ? C2 C1 H1A 110.5 . . ? S1 C1 H1A 110.5 . . ? C2 C1 H1B 110.5 . . ? S1 C1 H1B 110.5 . . ? H1A C1 H1B 108.7 . . ? C3 C2 C1 106.3(2) . . ? C3 C2 H2A 110.5 . . ? C1 C2 H2A 110.5 . . ? C3 C2 H2B 110.5 . . ? C1 C2 H2B 110.5 . . ? H2A C2 H2B 108.7 . . ? C2 C3 C4 106.8(2) . . ? C2 C3 H3A 110.4 . . ? C4 C3 H3A 110.4 . . ? C2 C3 H3B 110.4 . . ? C4 C3 H3B 110.4 . . ? H3A C3 H3B 108.6 . . ? C3 C4 S1 105.3(2) . . ? C3 C4 H4A 110.7 . . ? S1 C4 H4A 110.7 . . ? C3 C4 H4B 110.7 . . ? S1 C4 H4B 110.7 . . ? H4A C4 H4B 108.8 . . ? 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 S1 C4 125.7(2) . . . . ? # Br2 Te1 S1 C1 -135.0(2) . . . . ? Br3 Te1 S1 C4 -44.39(11) . . . . ? Br1 Te1 S1 C4 47.88(11) . . . . ? Br4 Te1 S1 C4 137.78(11) . . . . ? Br4 Te1 S1 C4 -133.89(11) 2_765 . . . ? Br3 Te1 S1 C1 54.91(11) . . . . ? Br1 Te1 S1 C1 147.18(11) . . . . ? Br4 Te1 S1 C1 -122.92(11) . . . . ? Br4 Te1 S1 C1 -34.59(11) 2_765 . . . ? C4 S1 C1 C2 11.2(2) . . . . ? Te1 S1 C1 C2 -98.36(19) . . . . ? S1 C1 C2 C3 -35.8(3) . . . . ? C1 C2 C3 C4 49.6(3) . . . . ? C2 C3 C4 S1 -39.8(3) . . . . ? C1 S1 C4 C3 16.2(2) . . . . ? Te1 S1 C4 C3 123.15(18) . . . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Br4 Br1 3.600(1) . 2_665 ? Br4 Br3 3.492(1) . 1_554 ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.553 _refine_diff_density_min -0.593 _refine_diff_density_rms 0.134 data_12aj007r _database_code_depnum_ccdc_archive 'CCDC 881037' #TrackingRef '- Te_all15_3.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2012-03-23 _audit_author_name 'Webster, M.' _chemical_name_systematic ; Tetrachloro(1,4,8,11-tetrathiacyclotetradecane-S,S')tellurium(IV) ; # [14]aneS4 = C10H20S4 # 1,4,8,11-tetrathiacyclotetradecane # 1,4,8,11-tetrathiacyclotetradecane iLab name (defaults & selected options) # 1,4,8,11-tetrathiacyclotetradecane Chemspider name (input SMILES string) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H20 Cl4 S4 Te' _chemical_formula_sum 'C10 H20 Cl4 S4 Te' _chemical_formula_weight 537.90 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 9.080(2) _cell_length_b 20.950(5) _cell_length_c 9.990(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.068(7) _cell_angle_gamma 90.00 _cell_volume 1889.8(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 11021 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.891 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 2.567 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.722 # Expt'l Tmin & Tmax _exptl_absorpt_correction_T_max 1.000 # scaled to Tmax=1.0 _exptl_absorpt_process_details ;Jacobson, R.A. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator ? _diffrn_radiation_collimation 'Confocal mirrors, VHF VariMax ' _diffrn_source 'Rotating anode X-ray tube' _diffrn_source_type 'Rigaku FR-E+ Superbright' _diffrn_measurement_device 'Four-circle \k diffractometer' _diffrn_measurement_device_type 'Rigaku AFC12' _diffrn_measurement_method 'Profile data from \w-scans' _diffrn_detector 'CCD plate' _diffrn_detector_type 'Rigaku HG Saturn724+ (2x2 bin mode)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13343 _diffrn_reflns_av_R_equivalents 0.0441 _diffrn_reflns_av_sigmaI/netI 0.0481 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 27.47 _reflns_number_total 4293 _reflns_number_gt 3436 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _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^)+(0.0201P)^2^+1.5197P] 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 4293 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0466 _refine_ls_R_factor_gt 0.0319 _refine_ls_wR_factor_ref 0.0646 _refine_ls_wR_factor_gt 0.0603 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _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 0.77972(2) 0.745845(10) 0.01577(2) 0.01263(7) Uani 1 1 d . . . Cl1 Cl 0.99106(9) 0.67869(4) 0.01530(8) 0.01858(18) Uani 1 1 d . . . Cl2 Cl 0.93230(9) 0.83835(4) 0.01081(9) 0.01925(18) Uani 1 1 d . . . Cl3 Cl 0.79831(10) 0.74890(4) 0.26708(8) 0.02115(18) Uani 1 1 d . . . Cl4 Cl 0.74170(9) 0.73812(4) -0.23443(8) 0.01898(18) Uani 1 1 d . . . S1 S 0.63602(9) 0.62509(4) 0.05073(8) 0.01373(17) Uani 1 1 d . . . S2 S 0.37744(9) 0.47896(4) 0.33256(9) 0.01598(18) Uani 1 1 d . . . S3 S 0.50881(9) 0.82903(4) 0.01469(8) 0.01530(18) Uani 1 1 d . . . S4 S 0.33605(9) 1.03228(4) -0.33880(8) 0.01525(18) Uani 1 1 d . . . C1 C 0.6844(4) 0.56462(16) -0.1797(3) 0.0157(7) Uani 1 1 d . . . H1A H 0.7384 0.5350 -0.1147 0.019 Uiso 1 1 calc R . . H1B H 0.7545 0.5983 -0.2014 0.019 Uiso 1 1 calc R . . C2 C 0.5590(4) 0.59518(16) -0.1140(3) 0.0161(7) Uani 1 1 d . . . H2A H 0.4804 0.5634 -0.1033 0.019 Uiso 1 1 calc R . . H2B H 0.5153 0.6307 -0.1702 0.019 Uiso 1 1 calc R . . C3 C 0.4717(4) 0.64758(15) 0.1283(3) 0.0152(7) Uani 1 1 d . . . H3A H 0.5013 0.6746 0.2078 0.018 Uiso 1 1 calc R . . H3B H 0.4064 0.6734 0.0635 0.018 Uiso 1 1 calc R . . C4 C 0.3842(3) 0.58998(16) 0.1724(3) 0.0159(7) Uani 1 1 d . . . H4A H 0.2993 0.6055 0.2180 0.019 Uiso 1 1 calc R . . H4B H 0.3439 0.5658 0.0916 0.019 Uiso 1 1 calc R . . C5 C 0.4777(4) 0.54505(15) 0.2675(3) 0.0143(7) Uani 1 1 d . . . H5A H 0.5241 0.5703 0.3445 0.017 Uiso 1 1 calc R . . H5B H 0.5585 0.5275 0.2192 0.017 Uiso 1 1 calc R . . C6 C 0.6669(3) 0.91611(15) 0.1938(3) 0.0149(7) Uani 1 1 d . . . H6A H 0.6903 0.9418 0.1156 0.018 Uiso 1 1 calc R . . H6B H 0.7461 0.8838 0.2124 0.018 Uiso 1 1 calc R . . C7 C 0.5195(4) 0.88236(16) 0.1591(3) 0.0161(7) Uani 1 1 d . . . H7A H 0.4414 0.9152 0.1422 0.019 Uiso 1 1 calc R . . H7B H 0.4971 0.8574 0.2386 0.019 Uiso 1 1 calc R . . C8 C 0.5433(3) 0.88162(15) -0.1228(3) 0.0146(7) Uani 1 1 d . . . H8A H 0.6374 0.9047 -0.0979 0.017 Uiso 1 1 calc R . . H8B H 0.5563 0.8553 -0.2031 0.017 Uiso 1 1 calc R . . C9 C 0.4211(3) 0.93049(16) -0.1604(3) 0.0145(7) Uani 1 1 d . . . H9A H 0.4087 0.9584 -0.0825 0.017 Uiso 1 1 calc R . . H9B H 0.3260 0.9084 -0.1867 0.017 Uiso 1 1 calc R . . C10 C 0.4653(3) 0.97040(15) -0.2782(3) 0.0139(7) Uani 1 1 d . . . H10A H 0.4789 0.9413 -0.3540 0.017 Uiso 1 1 calc R . . H10B H 0.5623 0.9906 -0.2503 0.017 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 0.01701(11) 0.00911(11) 0.01160(11) 0.00079(8) 0.00069(8) 0.00040(9) Cl1 0.0206(4) 0.0171(4) 0.0176(4) 0.0008(3) -0.0004(3) 0.0031(3) Cl2 0.0236(4) 0.0145(4) 0.0195(4) 0.0009(3) 0.0016(3) -0.0048(3) Cl3 0.0293(4) 0.0202(4) 0.0137(4) 0.0025(3) 0.0012(3) 0.0025(4) Cl4 0.0253(4) 0.0175(4) 0.0138(4) 0.0010(3) -0.0001(3) 0.0008(3) S1 0.0148(4) 0.0128(4) 0.0139(4) -0.0009(3) 0.0029(3) -0.0010(3) S2 0.0200(4) 0.0151(4) 0.0135(4) -0.0002(3) 0.0049(3) 0.0001(3) S3 0.0207(4) 0.0131(4) 0.0114(4) 0.0003(3) -0.0018(3) -0.0017(3) S4 0.0192(4) 0.0122(4) 0.0131(4) -0.0005(3) -0.0040(3) 0.0007(3) C1 0.0167(16) 0.0158(17) 0.0154(18) -0.0037(14) 0.0050(14) -0.0028(14) C2 0.0154(16) 0.0188(17) 0.0144(18) -0.0049(14) 0.0031(14) -0.0001(14) C3 0.0198(17) 0.0116(16) 0.0151(18) -0.0007(13) 0.0065(14) 0.0014(14) C4 0.0135(15) 0.0177(17) 0.0170(18) -0.0004(14) 0.0041(14) 0.0000(14) C5 0.0179(16) 0.0090(16) 0.0165(18) -0.0016(13) 0.0044(14) -0.0015(13) C6 0.0186(16) 0.0119(16) 0.0134(17) -0.0023(13) -0.0021(14) 0.0027(14) C7 0.0179(16) 0.0170(18) 0.0139(17) -0.0009(14) 0.0037(14) -0.0023(14) C8 0.0141(15) 0.0149(16) 0.0141(17) 0.0010(13) -0.0015(13) -0.0002(14) C9 0.0138(15) 0.0159(17) 0.0139(17) 0.0006(13) 0.0021(13) 0.0032(14) C10 0.0160(15) 0.0118(15) 0.0138(17) -0.0018(13) 0.0019(13) 0.0008(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Te1 Cl1 2.3799(9) . ? Te1 Cl2 2.3859(9) . ? Te1 Cl4 2.4921(12) . ? Te1 Cl3 2.4992(12) . ? Te1 S1 2.8846(10) . ? Te1 S3 3.0137(10) . ? S1 C3 1.815(3) . ? S1 C2 1.829(3) . ? S2 C5 1.815(3) . ? S2 C1 1.816(3) 3_665 ? S3 C8 1.814(3) . ? S3 C7 1.819(3) . ? S4 C10 1.810(3) . ? S4 C6 1.810(3) 3_675 ? C1 C2 1.515(4) . ? C1 S2 1.816(3) 3_665 ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.535(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.530(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.521(4) . ? C6 S4 1.810(3) 3_675 ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.527(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.531(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? 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 90.58(4) . . ? Cl1 Te1 Cl4 89.19(3) . . ? Cl2 Te1 Cl4 92.93(3) . . ? Cl1 Te1 Cl3 92.76(3) . . ? Cl2 Te1 Cl3 91.28(3) . . ? Cl4 Te1 Cl3 175.34(3) . . ? Cl1 Te1 S1 81.77(3) . . ? Cl2 Te1 S1 170.40(3) . . ? Cl4 Te1 S1 92.75(3) . . ? Cl3 Te1 S1 83.35(3) . . ? Cl1 Te1 S3 179.03(3) . . ? Cl2 Te1 S3 90.33(3) . . ? Cl4 Te1 S3 90.43(3) . . ? Cl3 Te1 S3 87.55(3) . . ? S1 Te1 S3 97.36(3) . . ? C3 S1 C2 102.65(15) . . ? C3 S1 Te1 103.12(11) . . ? C2 S1 Te1 109.06(12) . . ? C5 S2 C1 101.81(16) . 3_665 ? C8 S3 C7 103.21(16) . . ? C8 S3 Te1 98.49(11) . . ? C7 S3 Te1 112.15(11) . . ? C10 S4 C6 102.96(15) . 3_675 ? C2 C1 S2 113.4(2) . 3_665 ? C2 C1 H1A 108.9 . . ? S2 C1 H1A 108.9 3_665 . ? C2 C1 H1B 108.9 . . ? S2 C1 H1B 108.9 3_665 . ? H1A C1 H1B 107.7 . . ? C1 C2 S1 107.5(2) . . ? C1 C2 H2A 110.2 . . ? S1 C2 H2A 110.2 . . ? C1 C2 H2B 110.2 . . ? S1 C2 H2B 110.2 . . ? H2A C2 H2B 108.5 . . ? C4 C3 S1 113.1(2) . . ? C4 C3 H3A 109.0 . . ? S1 C3 H3A 109.0 . . ? C4 C3 H3B 109.0 . . ? S1 C3 H3B 109.0 . . ? H3A C3 H3B 107.8 . . ? C5 C4 C3 113.1(3) . . ? C5 C4 H4A 109.0 . . ? C3 C4 H4A 109.0 . . ? C5 C4 H4B 109.0 . . ? C3 C4 H4B 109.0 . . ? H4A C4 H4B 107.8 . . ? C4 C5 S2 115.2(2) . . ? C4 C5 H5A 108.5 . . ? S2 C5 H5A 108.5 . . ? C4 C5 H5B 108.5 . . ? S2 C5 H5B 108.5 . . ? H5A C5 H5B 107.5 . . ? C7 C6 S4 111.9(2) . 3_675 ? C7 C6 H6A 109.2 . . ? S4 C6 H6A 109.2 3_675 . ? C7 C6 H6B 109.2 . . ? S4 C6 H6B 109.2 3_675 . ? H6A C6 H6B 107.9 . . ? C6 C7 S3 116.0(2) . . ? C6 C7 H7A 108.3 . . ? S3 C7 H7A 108.3 . . ? C6 C7 H7B 108.3 . . ? S3 C7 H7B 108.3 . . ? H7A C7 H7B 107.4 . . ? C9 C8 S3 114.5(2) . . ? C9 C8 H8A 108.6 . . ? S3 C8 H8A 108.6 . . ? C9 C8 H8B 108.6 . . ? S3 C8 H8B 108.6 . . ? H8A C8 H8B 107.6 . . ? C8 C9 C10 108.2(3) . . ? C8 C9 H9A 110.1 . . ? C10 C9 H9A 110.1 . . ? C8 C9 H9B 110.1 . . ? C10 C9 H9B 110.1 . . ? H9A C9 H9B 108.4 . . ? C9 C10 S4 115.8(2) . . ? C9 C10 H10A 108.3 . . ? S4 C10 H10A 108.3 . . ? C9 C10 H10B 108.3 . . ? S4 C10 H10B 108.3 . . ? H10A C10 H10B 107.4 . . ? 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 S3 Te1 S1 C3 -23.56(12) . . . . ? S3 Te1 S1 C2 85.01(11) . . . . ? S1 Te1 S3 C8 -137.40(11) . . . . ? S1 Te1 S3 C7 114.52(12) . . . . ? S2 C1 C2 S1 170.69(18) 3_665 . . . ? C3 S1 C2 C1 -170.7(2) . . . . ? Te1 S1 C2 C1 80.4(2) . . . . ? C2 S1 C3 C4 73.3(3) . . . . ? Te1 S1 C3 C4 -173.3(2) . . . . ? S1 C3 C4 C5 55.7(3) . . . . ? C3 C4 C5 S2 175.9(2) . . . . ? C1 S2 C5 C4 63.0(3) 3_665 . . . ? S4 C6 C7 S3 179.97(17) 3_675 . . . ? C8 S3 C7 C6 -60.7(3) . . . . ? Te1 S3 C7 C6 44.3(3) . . . . ? C7 S3 C8 C9 -67.8(3) . . . . ? Te1 S3 C8 C9 176.9(2) . . . . ? S3 C8 C9 C10 -179.3(2) . . . . ? C8 C9 C10 S4 -179.5(2) . . . . ? C6 S4 C10 C9 61.9(3) 3_675 . . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl3 S3 3.382(1) . 4_676 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.521 _refine_diff_density_min -0.492 _refine_diff_density_rms 0.124 data_11aj007k _database_code_depnum_ccdc_archive 'CCDC 881038' #TrackingRef '- Te_all15_3.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2012-04-29 _audit_author_name 'Webster, M.' _chemical_name_systematic ; trimethyldiselanium pentafluorotellurate(IV) ; # [C3H9Se2]+ = [Me2SeSeMe]+ # trimethyldiselanium (ACD iLab defaults & selected options) # SMILES: C[Se+](C)[Se]C _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C3 H9 Se2 1+, F5 Te 1-' _chemical_formula_sum 'C3 H9 F5 Se2 Te' _chemical_formula_weight 425.62 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 7.864(3) _cell_length_b 7.253(2) _cell_length_c 17.044(6) _cell_angle_alpha 90.00 _cell_angle_beta 92.737(7) _cell_angle_gamma 90.00 _cell_volume 971.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4722 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.911 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 10.577 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.743 # Expt'l Tmin & Tmax _exptl_absorpt_correction_T_max 1.000 # scaled to Tmax=1.0 _exptl_absorpt_process_details ;Jacobson, R.A. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator ? _diffrn_radiation_collimation 'Confocal mirrors, HF VariMax ' _diffrn_source 'Rotating anode X-ray tube' _diffrn_source_type 'Rigaku FR-E+ SuperBright' _diffrn_measurement_device 'Four-circle \k diffractometer' _diffrn_measurement_device_type 'Rigaku AFC12 ' _diffrn_measurement_method 'Profile data from \w-scans' _diffrn_detector 'CCD plate' _diffrn_detector_type 'Rigaku HG Saturn724+ (2x2 bin mode)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5338 _diffrn_reflns_av_R_equivalents 0.0414 _diffrn_reflns_av_sigmaI/netI 0.0542 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.82 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2205 _reflns_number_gt 1829 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _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^)+(0.0161P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2205 _refine_ls_number_parameters 103 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0367 _refine_ls_R_factor_gt 0.0265 _refine_ls_wR_factor_ref 0.0583 _refine_ls_wR_factor_gt 0.0562 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 0.70100(3) 0.84160(4) 0.839463(16) 0.01077(8) Uani 1 1 d . . . F1 F 0.5794(3) 0.9875(3) 0.90778(15) 0.0210(6) Uani 1 1 d . . . F2 F 0.4894(3) 0.8738(4) 0.77582(16) 0.0270(7) Uani 1 1 d . . . F3 F 0.7718(3) 1.0858(4) 0.80510(16) 0.0300(7) Uani 1 1 d . . . F4 F 0.8718(3) 0.8567(3) 0.92700(15) 0.0213(6) Uani 1 1 d . . . F5 F 0.5888(3) 0.6453(3) 0.89729(16) 0.0243(6) Uani 1 1 d . . . Se1 Se 0.12901(5) 0.56241(6) 0.90467(3) 0.01688(12) Uani 1 1 d . . . Se2 Se 0.33466(5) 0.32877(5) 0.90135(3) 0.01245(11) Uani 1 1 d . . . C1 C 0.2331(6) 0.6937(6) 0.9950(3) 0.0199(10) Uani 1 1 d . . . H1A H 0.2567 0.6066 1.0381 0.030 Uiso 1 1 calc R . . H1B H 0.1549 0.7893 1.0120 0.030 Uiso 1 1 calc R . . H1C H 0.3397 0.7509 0.9801 0.030 Uiso 1 1 calc R . . C2 C 0.3988(5) 0.3431(6) 0.7935(3) 0.0161(10) Uani 1 1 d . . . H2A H 0.4806 0.2451 0.7833 0.024 Uiso 1 1 calc R . . H2B H 0.4508 0.4633 0.7841 0.024 Uiso 1 1 calc R . . H2C H 0.2973 0.3281 0.7584 0.024 Uiso 1 1 calc R . . C3 C 0.1818(5) 0.1192(6) 0.8878(3) 0.0180(10) Uani 1 1 d . . . H3A H 0.0956 0.1460 0.8460 0.027 Uiso 1 1 calc R . . H3B H 0.1259 0.0960 0.9370 0.027 Uiso 1 1 calc R . . H3C H 0.2470 0.0100 0.8737 0.027 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 0.00789(13) 0.01326(14) 0.01112(17) -0.00077(11) 0.00014(10) 0.00051(10) F1 0.0194(14) 0.0218(13) 0.0220(15) -0.0079(11) 0.0030(11) 0.0065(11) F2 0.0174(14) 0.0344(16) 0.0281(17) -0.0045(13) -0.0106(11) 0.0036(12) F3 0.0282(16) 0.0272(15) 0.0346(18) 0.0173(14) 0.0006(13) -0.0048(13) F4 0.0173(14) 0.0275(15) 0.0184(15) -0.0021(11) -0.0073(11) 0.0019(11) F5 0.0211(14) 0.0180(14) 0.0341(18) 0.0048(12) 0.0041(12) -0.0097(11) Se1 0.0133(2) 0.0172(2) 0.0198(3) -0.00161(19) -0.00173(17) 0.00160(17) Se2 0.0106(2) 0.0132(2) 0.0135(3) -0.00107(17) -0.00047(16) 0.00019(16) C1 0.022(2) 0.021(2) 0.017(3) -0.0088(19) -0.0027(19) 0.0000(18) C2 0.015(2) 0.018(2) 0.016(3) 0.0029(19) 0.0056(17) -0.0054(17) C3 0.014(2) 0.012(2) 0.027(3) -0.003(2) 0.0009(18) -0.0031(17) _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 F1 1.870(2) . ? Te1 F3 1.955(3) . ? Te1 F2 1.956(3) . ? Te1 F4 1.962(2) . ? Te1 F5 1.965(3) . ? Se1 C1 1.956(4) . ? Se1 Se2 2.3450(8) . ? Se2 C2 1.932(4) . ? Se2 C3 1.945(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 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 F1 Te1 F3 80.50(12) . . ? F1 Te1 F2 80.27(11) . . ? F3 Te1 F2 88.41(11) . . ? F1 Te1 F4 81.17(11) . . ? F3 Te1 F4 89.02(11) . . ? F2 Te1 F4 161.44(11) . . ? F1 Te1 F5 80.95(12) . . ? F3 Te1 F5 161.45(11) . . ? F2 Te1 F5 88.53(12) . . ? F4 Te1 F5 88.08(11) . . ? C1 Se1 Se2 96.19(13) . . ? C2 Se2 C3 96.73(19) . . ? C2 Se2 Se1 101.29(13) . . ? C3 Se2 Se1 98.33(13) . . ? Se1 C1 H1A 109.5 . . ? Se1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Se1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Se2 C2 H2A 109.5 . . ? Se2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Se2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Se2 C3 H3A 109.5 . . ? Se2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Se2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Te1 F3 3.100(3) . 2_646 ? Se1 F4 2.978(3) . 1_455 ? Se2 F1 3.134(3) . 1_545 ? Se2 F5 3.047(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.722 _refine_diff_density_min -1.186 _refine_diff_density_rms 0.173 data_12aj008r _database_code_depnum_ccdc_archive 'CCDC 881039' #TrackingRef '- Te_all15_3.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2012-05-01 _audit_author_name 'Webster, M.' _chemical_name_systematic ; tetrachloro(1,2-bis(methylseleno)benzene-Se,Se')tellurium(IV) ; # o-C6H4(SeMe)2 = C8H10Se2 # 1,2-bis(methylseleno)benzene (iLab defaults) # 1,2-bis(methylselanyl)benzene (iLab selected options) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H10 Cl4 Se2 Te' _chemical_formula_sum 'C8 H10 Cl4 Se2 Te' _chemical_formula_weight 533.48 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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/m' _space_group_IT_number 11 _space_group_name_Hall '-P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 6.804(3) _cell_length_b 10.725(5) _cell_length_c 9.969(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.156(7) _cell_angle_gamma 90.00 _cell_volume 718.3(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3128 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description needle _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.467 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 492 _exptl_absorpt_coefficient_mu 7.850 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.737 # Expt'l Tmin & Tmax _exptl_absorpt_correction_T_max 1.000 # scaled to Tmax=1.0 _exptl_absorpt_process_details ;Jacobson, R.A. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator ? _diffrn_radiation_collimation 'Confocal mirrors, VHF VariMax ' _diffrn_source 'Rotating anode X-ray tube' _diffrn_source_type 'Rigaku FR-E+ Superbright' _diffrn_measurement_device 'Four-circle \k diffractometer' _diffrn_measurement_device_type 'Rigaku AFC12 ' _diffrn_measurement_method 'Profile data from \w-scans' _diffrn_detector 'CCD plate' _diffrn_detector_type 'Rigaku HG Saturn724+ (2x2 bin mode)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3583 _diffrn_reflns_av_R_equivalents 0.0279 _diffrn_reflns_av_sigmaI/netI 0.0433 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.48 _reflns_number_total 1717 _reflns_number_gt 1426 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0430P)^2^+0.7117P] 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 1717 _refine_ls_number_parameters 74 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0452 _refine_ls_R_factor_gt 0.0337 _refine_ls_wR_factor_ref 0.0841 _refine_ls_wR_factor_gt 0.0799 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _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 0.05867(6) 0.2500 0.35982(4) 0.01163(14) Uani 1 2 d S . . Se1 Se -0.27773(7) 0.40600(5) 0.22780(4) 0.01349(15) Uani 1 1 d . . . Cl1 Cl -0.1257(3) 0.2500 0.55128(16) 0.0178(4) Uani 1 2 d S . . Cl2 Cl 0.2188(3) 0.2500 0.14209(17) 0.0204(4) Uani 1 2 d S . . Cl3 Cl 0.27901(19) 0.41879(12) 0.46132(12) 0.0177(3) Uani 1 1 d . . . C1 C -0.3131(6) 0.3150(4) 0.0584(5) 0.0119(10) Uani 1 1 d . . . C2 C -0.3468(7) 0.3804(5) -0.0646(5) 0.0154(10) Uani 1 1 d . . . H2 H -0.3459 0.4690 -0.0647 0.018 Uiso 1 1 calc R . . C3 C -0.3816(7) 0.3146(5) -0.1871(5) 0.0162(11) Uani 1 1 d . . . H3 H -0.4054 0.3587 -0.2708 0.019 Uiso 1 1 calc R . . C4 C -0.1154(8) 0.5441(5) 0.1773(5) 0.0216(11) Uani 1 1 d . . . H4A H -0.0099 0.5110 0.1309 0.032 Uiso 1 1 calc R . . H4B H -0.0556 0.5890 0.2594 0.032 Uiso 1 1 calc R . . H4C H -0.1995 0.6012 0.1165 0.032 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 0.0124(2) 0.0133(2) 0.0091(2) 0.000 0.00137(15) 0.000 Se1 0.0172(3) 0.0130(3) 0.0105(2) -0.00049(19) 0.00274(18) 0.0005(2) Cl1 0.0247(8) 0.0180(8) 0.0124(7) 0.000 0.0075(7) 0.000 Cl2 0.0195(8) 0.0274(10) 0.0151(8) 0.000 0.0058(6) 0.000 Cl3 0.0246(6) 0.0140(6) 0.0150(5) -0.0038(5) 0.0045(5) -0.0055(5) C1 0.0088(19) 0.014(3) 0.013(2) 0.0006(19) 0.0009(16) -0.0003(19) C2 0.017(2) 0.017(2) 0.012(2) 0.003(2) 0.0035(18) 0.002(2) C3 0.013(2) 0.024(3) 0.012(2) 0.005(2) 0.0016(17) 0.001(2) C4 0.031(3) 0.015(3) 0.018(2) -0.001(2) 0.000(2) -0.008(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 Cl1 2.445(2) . ? Te1 Cl3 2.4630(14) . ? Te1 Cl3 2.4630(14) 4_565 ? Te1 Cl2 2.579(2) . ? Te1 Se1 2.9686(10) 4_565 ? Te1 Se1 2.9686(10) . ? Se1 C1 1.932(5) . ? Se1 C4 1.960(5) . ? C1 C1 1.393(9) 4_565 ? C1 C2 1.400(6) . ? C2 C3 1.398(7) . ? C2 H2 0.9500 . ? C3 C3 1.386(10) 4_565 ? C3 H3 0.9500 . ? 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 91.93(5) . . ? Cl1 Te1 Cl3 91.93(5) . 4_565 ? Cl3 Te1 Cl3 94.62(7) . 4_565 ? Cl1 Te1 Cl2 174.21(6) . . ? Cl3 Te1 Cl2 91.99(5) . . ? Cl3 Te1 Cl2 91.99(5) 4_565 . ? Cl1 Te1 Se1 83.74(5) . 4_565 ? Cl3 Te1 Se1 166.52(3) . 4_565 ? Cl3 Te1 Se1 98.28(5) 4_565 4_565 ? Cl2 Te1 Se1 91.49(4) . 4_565 ? Cl1 Te1 Se1 83.74(5) . . ? Cl3 Te1 Se1 98.28(5) . . ? Cl3 Te1 Se1 166.52(3) 4_565 . ? Cl2 Te1 Se1 91.49(4) . . ? Se1 Te1 Se1 68.61(4) 4_565 . ? C1 Se1 C4 98.9(2) . . ? C1 Se1 Te1 94.74(13) . . ? C4 Se1 Te1 96.50(17) . . ? C1 C1 C2 120.1(3) 4_565 . ? C1 C1 Se1 120.36(14) 4_565 . ? C2 C1 Se1 119.5(4) . . ? C3 C2 C1 119.6(5) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C3 C3 C2 120.3(3) 4_565 . ? C3 C3 H3 119.8 4_565 . ? C2 C3 H3 119.8 . . ? Se1 C4 H4A 109.5 . . ? Se1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Se1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Se1 Cl3 3.626(2) . 3_566 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.295 _refine_diff_density_min -1.183 _refine_diff_density_rms 0.191