# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_fcnte _database_code_depnum_ccdc_archive 'CCDC 259969' _audit_creation_method SHELXL-97 _chemical_name_systematic ; tellurtetrafluoride tetrahydrofuran solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H16 F4 O2 Te' _chemical_formula_weight 347.81 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' 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' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.8161(15) _cell_length_b 9.390(2) _cell_length_c 10.465(2) _cell_angle_alpha 109.140(4) _cell_angle_beta 101.744(6) _cell_angle_gamma 100.421(5) _cell_volume 596.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 882 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 30.4 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.935 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 336 _exptl_absorpt_coefficient_mu 2.524 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.74 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details 'SADABS (BRUKER-AXS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART CCD (Bruker-AXS)' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7429 _diffrn_reflns_av_R_equivalents 0.0134 _diffrn_reflns_av_sigmaI/netI 0.0195 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 30.53 _reflns_number_total 3579 _reflns_number_gt 3388 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker-AXS)' _computing_cell_refinement 'SAINT (BRUKER-AXS)' _computing_data_reduction 'SAINT (BRUKER-AXS)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP for Windows (Farrugia, 1997)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0216P)^2^+0.3340P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0233(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3579 _refine_ls_number_parameters 137 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0207 _refine_ls_R_factor_gt 0.0191 _refine_ls_wR_factor_ref 0.0475 _refine_ls_wR_factor_gt 0.0467 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _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 0.542435(16) 0.612388(13) 0.855906(12) 0.02668(5) Uani 1 1 d . . . C11 C 0.5606(3) 0.9050(3) 1.1704(2) 0.0435(5) Uani 1 1 d . . . H11A H 0.6240 1.0144 1.1839 0.052 Uiso 1 1 calc R . . H11B H 0.6726 0.8581 1.1989 0.052 Uiso 1 1 calc R . . C12 C 0.4076(4) 0.8993(4) 1.2550(3) 0.0549(6) Uani 1 1 d . . . H12A H 0.4471 0.9959 1.3407 0.066 Uiso 1 1 calc R . . H12B H 0.3988 0.8080 1.2831 0.066 Uiso 1 1 calc R . . C13 C 0.2040(4) 0.8851(3) 1.1552(3) 0.0499(6) Uani 1 1 d . . . H13A H 0.0846 0.8299 1.1767 0.060 Uiso 1 1 calc R . . H13B H 0.1877 0.9895 1.1608 0.060 Uiso 1 1 calc R . . C14 C 0.2202(4) 0.7921(3) 1.0127(3) 0.0520(6) Uani 1 1 d . . . H14A H 0.1512 0.6798 0.9847 0.062 Uiso 1 1 calc R . . H14B H 0.1531 0.8291 0.9411 0.062 Uiso 1 1 calc R . . C21 C 0.2747(5) 0.2986(5) 0.5119(3) 0.0685(9) Uani 1 1 d . . . H21A H 0.3641 0.2259 0.4983 0.082 Uiso 1 1 calc R . . H21B H 0.3333 0.3879 0.4881 0.082 Uiso 1 1 calc R . . C22 C 0.0578(4) 0.2166(4) 0.4196(3) 0.0574(7) Uani 1 1 d . . . H22A H 0.0437 0.1039 0.3703 0.069 Uiso 1 1 calc R . . H22B H 0.0203 0.2624 0.3483 0.069 Uiso 1 1 calc R . . C23 C -0.0803(4) 0.2393(3) 0.5170(3) 0.0519(6) Uani 1 1 d . . . H23A H -0.2031 0.2701 0.4775 0.062 Uiso 1 1 calc R . . H23B H -0.1280 0.1424 0.5333 0.062 Uiso 1 1 calc R . . C24 C 0.0580(3) 0.3685(3) 0.6511(2) 0.0437(5) Uani 1 1 d . . . H24A H 0.0473 0.4719 0.6501 0.052 Uiso 1 1 calc R . . H24B H 0.0193 0.3568 0.7340 0.052 Uiso 1 1 calc R . . F1 F 0.7153(2) 0.5654(2) 1.00360(16) 0.0521(4) Uani 1 1 d . . . F2 F 0.4598(2) 0.69813(18) 0.71429(15) 0.0484(3) Uani 1 1 d . . . F3 F 0.76557(19) 0.79050(15) 0.92717(15) 0.0437(3) Uani 1 1 d . . . F4 F 0.6957(2) 0.51410(17) 0.74258(15) 0.0445(3) Uani 1 1 d . . . O1 O 0.4408(2) 0.8152(2) 1.02457(18) 0.0502(4) Uani 1 1 d . . . O2 O 0.2658(2) 0.35313(19) 0.65513(15) 0.0378(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Te1 0.02360(7) 0.03322(7) 0.02830(7) 0.01483(5) 0.01026(4) 0.01034(4) C11 0.0338(10) 0.0427(11) 0.0393(11) 0.0022(9) 0.0048(8) 0.0065(9) C12 0.0516(14) 0.0668(17) 0.0400(12) 0.0134(12) 0.0117(11) 0.0153(13) C13 0.0440(12) 0.0577(15) 0.0544(14) 0.0219(12) 0.0235(11) 0.0162(11) C14 0.0300(10) 0.0668(16) 0.0479(13) 0.0051(12) 0.0084(9) 0.0202(10) C21 0.0466(14) 0.106(3) 0.0303(11) 0.0000(13) 0.0136(10) 0.0133(15) C22 0.0553(15) 0.0694(18) 0.0334(11) 0.0066(11) 0.0061(10) 0.0146(13) C23 0.0387(11) 0.0602(15) 0.0446(12) 0.0137(11) 0.0024(10) 0.0070(11) C24 0.0327(10) 0.0565(13) 0.0406(11) 0.0147(10) 0.0129(9) 0.0126(9) F1 0.0355(6) 0.0775(10) 0.0577(8) 0.0473(8) 0.0078(6) 0.0148(7) F2 0.0555(8) 0.0607(9) 0.0455(7) 0.0351(7) 0.0153(6) 0.0257(7) F3 0.0306(6) 0.0400(7) 0.0599(8) 0.0205(6) 0.0135(6) 0.0041(5) F4 0.0383(7) 0.0541(8) 0.0493(8) 0.0174(6) 0.0247(6) 0.0220(6) O1 0.0308(7) 0.0594(10) 0.0426(9) -0.0031(8) 0.0077(6) 0.0150(7) O2 0.0329(7) 0.0493(8) 0.0277(6) 0.0090(6) 0.0081(5) 0.0138(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Te1 F3 1.8619(13) . y Te1 F4 1.8667(12) . y Te1 F2 1.9413(13) . y Te1 F1 1.9664(13) . y Te1 O1 2.4482(17) . y C11 O1 1.451(3) . ? C11 C12 1.504(4) . ? C12 C13 1.512(4) . ? C13 C14 1.499(4) . ? C14 O1 1.453(3) . ? C21 O2 1.435(3) . ? C21 C22 1.493(4) . ? C22 C23 1.513(4) . ? C23 C24 1.504(3) . ? C24 O2 1.443(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F3 Te1 F4 86.98(6) . . y F3 Te1 F2 82.15(7) . . y F4 Te1 F2 86.45(6) . . y F3 Te1 F1 80.97(6) . . y F4 Te1 F1 84.74(7) . . y F2 Te1 F1 161.33(7) . . y F3 Te1 O1 73.97(6) . . y F4 Te1 O1 160.88(7) . . y F2 Te1 O1 89.33(7) . . y F1 Te1 O1 93.63(7) . . y O1 C11 C12 105.41(19) . . ? C11 C12 C13 103.8(2) . . ? C14 C13 C12 103.8(2) . . ? O1 C14 C13 106.5(2) . . ? O2 C21 C22 107.5(2) . . ? C21 C22 C23 105.8(2) . . ? C24 C23 C22 103.8(2) . . ? O2 C24 C23 105.22(19) . . ? C11 O1 C14 109.62(17) . . ? C11 O1 Te1 125.02(13) . . ? C14 O1 Te1 117.20(14) . . ? C21 O2 C24 106.74(18) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 30.53 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.984 _refine_diff_density_min -0.501 _refine_diff_density_rms 0.073 data_tef4tla _database_code_depnum_ccdc_archive 'CCDC 260727' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Telluriumtetrafluoride toluolene solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C7 H8 F4 Te' _chemical_formula_weight 295.73 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.5829(15) _cell_length_b 10.446(2) _cell_length_c 13.131(3) _cell_angle_alpha 107.632(4) _cell_angle_beta 96.929(4) _cell_angle_gamma 108.243(4) _cell_volume 914.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1007 _cell_measurement_theta_min 2.9 _cell_measurement_theta_max 30.4 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.148 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 552 _exptl_absorpt_coefficient_mu 3.260 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.802 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'SADABS (Bruker-AXS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART CCD (Bruker-AXS)' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11412 _diffrn_reflns_av_R_equivalents 0.0239 _diffrn_reflns_av_sigmaI/netI 0.0405 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 30.55 _reflns_number_total 5418 _reflns_number_gt 4218 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BRUKER-AXS)' _computing_cell_refinement 'SAINT (BRUKER-AXS)' _computing_data_reduction 'SAINT (BRUKER-AXS)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP for Windows (Farrugia, 1997)' _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^)+(0.0000P)^2^+5.0917P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5418 _refine_ls_number_parameters 222 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0540 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.0772 _refine_ls_wR_factor_gt 0.0735 _refine_ls_goodness_of_fit_ref 1.166 _refine_ls_restrained_S_all 1.166 _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 0.49441(4) 1.12111(3) 0.16806(3) 0.01839(8) Uani 1 1 d . . . Te2 Te 0.34167(4) 0.83261(3) 0.33985(3) 0.01771(8) Uani 1 1 d . . . F1 F 0.2413(4) 0.9994(3) 0.1116(3) 0.0288(7) Uani 1 1 d . . . F2 F 0.4323(5) 1.2415(3) 0.1014(3) 0.0337(7) Uani 1 1 d . . . F3 F 0.4162(4) 1.2157(3) 0.2900(3) 0.0300(7) Uani 1 1 d . . . F4 F 0.5000 1.0000 0.0000 0.0377(11) Uani 1 2 d S . . F5 F 0.4752(4) 0.9556(3) 0.2444(3) 0.0319(7) Uani 1 1 d . . . F6 F 0.2155(4) 0.9598(3) 0.3513(2) 0.0276(6) Uani 1 1 d . . . F7 F 0.1520(5) 0.7145(3) 0.2098(3) 0.0343(7) Uani 1 1 d . . . F8 F 0.1716(5) 0.7488(4) 0.4158(3) 0.0378(8) Uani 1 1 d . . . F9 F 0.5000 1.0000 0.5000 0.0463(13) Uani 1 2 d S . . C1 C 0.9119(7) 0.3207(6) 0.1597(4) 0.0266(11) Uani 1 1 d . . . C2 C 0.8680(7) 0.4020(6) 0.2522(5) 0.0310(12) Uani 1 1 d . . . H2 H 0.8353 0.4824 0.2513 0.037 Uiso 1 1 calc R . . C3 C 0.8721(8) 0.3649(8) 0.3458(5) 0.0428(16) Uani 1 1 d . . . H3 H 0.8409 0.4196 0.4083 0.051 Uiso 1 1 calc R . . C4 C 0.9213(8) 0.2488(8) 0.3479(5) 0.0422(16) Uani 1 1 d . . . H4 H 0.9245 0.2240 0.4118 0.051 Uiso 1 1 calc R . . C5 C 0.9656(8) 0.1695(7) 0.2575(5) 0.0387(14) Uani 1 1 d . . . H5 H 0.9984 0.0892 0.2586 0.046 Uiso 1 1 calc R . . C6 C 0.9626(7) 0.2062(6) 0.1641(5) 0.0282(11) Uani 1 1 d . . . H6 H 0.9959 0.1518 0.1025 0.034 Uiso 1 1 calc R . . C7 C 0.9071(10) 0.3601(7) 0.0594(5) 0.0447(16) Uani 1 1 d . . . H7A H 0.9720 0.3100 0.0107 0.067 Uiso 1 1 calc R . . H7B H 0.9722 0.4648 0.0810 0.067 Uiso 1 1 calc R . . H7C H 0.7740 0.3313 0.0208 0.067 Uiso 1 1 calc R . . C11 C 0.6290(10) 0.6773(8) 0.2336(5) 0.0409(15) Uani 1 1 d . . . C12 C 0.7490(8) 0.7702(7) 0.3338(7) 0.0446(17) Uani 1 1 d . . . H12 H 0.8596 0.8473 0.3369 0.054 Uiso 1 1 calc R . . C13 C 0.7104(11) 0.7526(8) 0.4306(6) 0.053(2) Uani 1 1 d . . . H13 H 0.7941 0.8167 0.4998 0.063 Uiso 1 1 calc R . . C14 C 0.5491(13) 0.6408(9) 0.4245(6) 0.056(2) Uani 1 1 d . . . H14 H 0.5194 0.6278 0.4899 0.067 Uiso 1 1 calc R . . C15 C 0.4311(10) 0.5481(7) 0.3240(8) 0.054(2) Uani 1 1 d . . . H15 H 0.3206 0.4702 0.3197 0.065 Uiso 1 1 calc R . . C16 C 0.4716(10) 0.5674(7) 0.2309(6) 0.0479(18) Uani 1 1 d . . . H16 H 0.3881 0.5025 0.1619 0.058 Uiso 1 1 calc R . . C17 C 0.6734(17) 0.6999(14) 0.1299(8) 0.106(4) Uani 1 1 d . . . H17A H 0.6336 0.6059 0.0702 0.159 Uiso 1 1 calc R . . H17B H 0.8111 0.7514 0.1425 0.159 Uiso 1 1 calc R . . H17C H 0.6042 0.7570 0.1096 0.159 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 0.01783(15) 0.01683(16) 0.02096(17) 0.00665(13) 0.00551(13) 0.00684(12) Te2 0.01683(15) 0.01683(16) 0.01759(16) 0.00543(13) 0.00306(12) 0.00492(12) F1 0.0176(14) 0.0266(16) 0.0309(17) 0.0027(13) 0.0036(12) 0.0017(12) F2 0.0392(18) 0.0292(17) 0.0373(19) 0.0165(15) 0.0031(15) 0.0166(15) F3 0.0312(16) 0.0282(16) 0.0318(17) 0.0073(14) 0.0142(14) 0.0135(14) F4 0.041(3) 0.040(3) 0.026(2) 0.004(2) 0.011(2) 0.014(2) F5 0.0308(16) 0.0328(17) 0.045(2) 0.0238(16) 0.0183(15) 0.0161(14) F6 0.0243(15) 0.0297(16) 0.0322(17) 0.0108(14) 0.0077(13) 0.0146(13) F7 0.0353(18) 0.0273(17) 0.0245(17) 0.0024(14) -0.0081(14) 0.0032(14) F8 0.0363(18) 0.048(2) 0.045(2) 0.0309(18) 0.0214(16) 0.0178(16) F9 0.047(3) 0.039(3) 0.038(3) -0.009(2) -0.009(2) 0.025(3) C1 0.023(2) 0.026(3) 0.025(3) 0.011(2) 0.001(2) 0.003(2) C2 0.020(2) 0.023(3) 0.034(3) 0.000(2) -0.004(2) 0.001(2) C3 0.022(3) 0.066(5) 0.019(3) -0.002(3) 0.000(2) 0.007(3) C4 0.024(3) 0.074(5) 0.032(3) 0.030(3) 0.002(2) 0.013(3) C5 0.026(3) 0.050(4) 0.055(4) 0.034(3) 0.014(3) 0.017(3) C6 0.020(2) 0.032(3) 0.034(3) 0.015(2) 0.010(2) 0.007(2) C7 0.046(4) 0.048(4) 0.038(4) 0.030(3) 0.005(3) 0.003(3) C11 0.053(4) 0.058(4) 0.036(3) 0.022(3) 0.021(3) 0.045(4) C12 0.022(3) 0.035(3) 0.083(6) 0.024(4) 0.013(3) 0.016(3) C13 0.055(4) 0.046(4) 0.045(4) -0.009(3) -0.023(3) 0.040(4) C14 0.090(6) 0.074(5) 0.056(5) 0.047(4) 0.041(5) 0.066(5) C15 0.044(4) 0.026(3) 0.103(7) 0.029(4) 0.024(4) 0.020(3) C16 0.044(4) 0.030(3) 0.054(4) -0.010(3) -0.007(3) 0.024(3) C17 0.168(11) 0.189(12) 0.078(6) 0.094(8) 0.094(7) 0.151(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 F1 1.846(3) . ? Te1 F2 1.873(3) . ? Te1 F3 1.879(3) . ? Te1 F4 2.1994(5) . ? Te1 F5 2.223(3) . ? Te2 F6 1.847(3) . ? Te2 F7 1.878(3) . ? Te2 F8 1.886(3) . ? Te2 F5 2.171(3) . ? Te2 F9 2.1841(5) . ? F4 Te1 2.1994(5) 2_675 ? F9 Te2 2.1841(5) 2_676 ? C1 C6 1.381(7) . ? C1 C2 1.398(8) . ? C1 C7 1.493(7) . ? C2 C3 1.396(8) . ? C3 C4 1.383(10) . ? C4 C5 1.372(9) . ? C5 C6 1.391(8) . ? C11 C16 1.360(10) . ? C11 C12 1.373(10) . ? C11 C17 1.510(9) . ? C12 C13 1.391(10) . ? C13 C14 1.376(11) . ? C14 C15 1.371(11) . ? C15 C16 1.353(10) . ? 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 F2 86.33(14) . . ? F1 Te1 F3 86.55(13) . . ? F2 Te1 F3 87.06(14) . . ? F1 Te1 F4 78.95(9) . . ? F2 Te1 F4 83.00(10) . . ? F3 Te1 F4 162.87(10) . . ? F1 Te1 F5 77.96(13) . . ? F2 Te1 F5 162.88(13) . . ? F3 Te1 F5 85.26(12) . . ? F4 Te1 F5 100.39(9) . . ? F6 Te2 F7 85.33(14) . . ? F6 Te2 F8 85.54(14) . . ? F7 Te2 F8 87.29(15) . . ? F6 Te2 F5 78.52(12) . . ? F7 Te2 F5 86.40(14) . . ? F8 Te2 F5 163.27(13) . . ? F6 Te2 F9 78.42(10) . . ? F7 Te2 F9 162.94(10) . . ? F8 Te2 F9 86.32(11) . . ? F5 Te2 F9 95.32(9) . . ? Te1 F4 Te1 180.000(10) . 2_675 ? Te2 F5 Te1 150.73(15) . . ? Te2 F9 Te2 180.0 2_676 . ? C6 C1 C2 118.8(5) . . ? C6 C1 C7 121.2(5) . . ? C2 C1 C7 120.1(5) . . ? C3 C2 C1 120.0(6) . . ? C4 C3 C2 120.2(6) . . ? C5 C4 C3 119.9(5) . . ? C4 C5 C6 120.2(6) . . ? C1 C6 C5 120.9(5) . . ? C16 C11 C12 118.7(6) . . ? C16 C11 C17 121.7(8) . . ? C12 C11 C17 119.6(8) . . ? C11 C12 C13 120.7(6) . . ? C14 C13 C12 118.9(6) . . ? C15 C14 C13 119.9(6) . . ? C16 C15 C14 120.2(7) . . ? C15 C16 C11 121.6(7) . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 30.55 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 1.437 _refine_diff_density_min -0.903 _refine_diff_density_rms 0.168 # Attachment 'TeCl4acetonitrile.cif' data_tecl4ac _database_code_depnum_ccdc_archive 'CCDC 750373' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'Tellurium Tetrachloride Acetonitrile Solvate' ; _chemical_name_common "'Tellurium Tetrachloride Acetonitrile Solvate'" _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H6 Cl4 N2 Te' _chemical_formula_weight 351.51 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.9326(11) _cell_length_b 7.4523(14) _cell_length_c 12.619(2) _cell_angle_alpha 88.750(4) _cell_angle_beta 88.661(4) _cell_angle_gamma 84.977(4) _cell_volume 555.50(18) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 970 _cell_measurement_theta_min 4.2 _cell_measurement_theta_max 30.5 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.102 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 328 _exptl_absorpt_coefficient_mu 3.586 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.692 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'SADABS 2.10 (Bruker-AXS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART CCD (Bruker-AXS)' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6407 _diffrn_reflns_av_R_equivalents 0.0152 _diffrn_reflns_av_sigmaI/netI 0.0226 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 30.57 _reflns_number_total 3295 _reflns_number_gt 3076 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker-AXS)' _computing_cell_refinement 'SAINT (Bruker-AXS)' _computing_data_reduction 'SAINT (Bruker-AXS)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep3 ( Farrugia, 1997)' _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^)+(0.0278P)^2^+0.2150P] 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 3295 _refine_ls_number_parameters 102 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0218 _refine_ls_R_factor_gt 0.0195 _refine_ls_wR_factor_ref 0.0508 _refine_ls_wR_factor_gt 0.0497 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 0.07529(2) 0.247147(15) 0.749817(9) 0.01751(4) Uani 1 1 d . . . Cl1 Cl -0.14807(10) 0.01602(7) 0.67320(4) 0.02856(11) Uani 1 1 d . . . Cl2 Cl 0.27119(10) 0.48896(7) 0.82870(5) 0.03083(11) Uani 1 1 d . . . Cl3 Cl -0.15641(9) 0.24799(7) 0.90006(4) 0.02556(10) Uani 1 1 d . . . Cl4 Cl -0.14974(9) 0.46827(7) 0.66037(4) 0.02811(11) Uani 1 1 d . . . N1L N 0.3327(3) -0.0144(3) 0.86139(16) 0.0294(4) Uani 1 1 d . . . N2L N 0.3228(4) 0.2651(3) 0.56432(17) 0.0341(4) Uani 1 1 d . . . C1L C 0.4888(4) -0.1099(3) 0.88019(16) 0.0227(4) Uani 1 1 d . . . C2L C 0.6869(4) -0.2322(3) 0.90467(18) 0.0275(4) Uani 1 1 d . . . H2A H 0.6531 -0.3076 0.9666 0.041 Uiso 1 1 calc R . . H2B H 0.8142 -0.1622 0.9201 0.041 Uiso 1 1 calc R . . H2C H 0.7268 -0.3090 0.8438 0.041 Uiso 1 1 calc R . . C3L C 0.4646(4) 0.2510(3) 0.50210(17) 0.0247(4) Uani 1 1 d . . . C4L C 0.6445(4) 0.2341(3) 0.42238(19) 0.0321(5) Uani 1 1 d . . . H4A H 0.5953 0.1676 0.3622 0.048 Uiso 1 1 calc R . . H4B H 0.7792 0.1690 0.4529 0.048 Uiso 1 1 calc R . . H4C H 0.6807 0.3543 0.3982 0.048 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 0.01666(7) 0.01843(6) 0.01707(7) 0.00178(4) -0.00013(4) -0.00008(4) Cl1 0.0317(3) 0.0265(2) 0.0284(3) -0.00367(19) -0.0027(2) -0.00593(19) Cl2 0.0333(3) 0.0302(2) 0.0309(3) 0.0024(2) -0.0059(2) -0.0128(2) Cl3 0.0238(2) 0.0301(2) 0.0226(2) -0.00108(18) 0.00593(18) -0.00299(18) Cl4 0.0282(2) 0.0256(2) 0.0294(3) 0.00416(19) -0.00689(19) 0.00470(18) N1L 0.0300(10) 0.0284(9) 0.0289(10) 0.0026(7) 0.0013(8) 0.0013(7) N2L 0.0314(10) 0.0417(11) 0.0277(10) 0.0045(8) 0.0028(8) 0.0023(8) C1L 0.0294(10) 0.0208(8) 0.0181(9) 0.0003(7) -0.0002(7) -0.0041(7) C2L 0.0303(11) 0.0239(9) 0.0278(11) 0.0007(8) -0.0046(8) 0.0019(8) C3L 0.0284(10) 0.0236(9) 0.0217(10) 0.0032(7) -0.0022(8) 0.0003(7) C4L 0.0347(12) 0.0330(11) 0.0272(12) 0.0006(9) 0.0099(9) 0.0020(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 2.3154(6) . ? Te1 Cl4 2.3186(6) . ? Te1 Cl2 2.4674(6) . ? Te1 Cl1 2.4879(6) . ? Te1 N2L 2.741(2) . ? Te1 N1L 2.752(2) . ? N1L C1L 1.144(3) . ? N2L C3L 1.137(3) . ? C1L C2L 1.458(3) . ? C3L C4L 1.449(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl3 Te1 Cl4 94.79(2) . . ? Cl3 Te1 Cl2 88.21(2) . . ? Cl4 Te1 Cl2 88.18(2) . . ? Cl3 Te1 Cl1 89.15(2) . . ? Cl4 Te1 Cl1 88.96(2) . . ? Cl2 Te1 Cl1 175.936(19) . . ? Cl3 Te1 N2L 175.30(5) . . ? Cl4 Te1 N2L 80.53(5) . . ? Cl2 Te1 N2L 92.17(5) . . ? Cl1 Te1 N2L 90.21(5) . . ? Cl3 Te1 N1L 83.37(5) . . ? Cl4 Te1 N1L 178.16(4) . . ? Cl2 Te1 N1L 91.74(5) . . ? Cl1 Te1 N1L 91.02(5) . . ? N2L Te1 N1L 101.30(6) . . ? C1L N1L Te1 156.64(18) . . ? C3L N2L Te1 163.35(19) . . ? N1L C1L C2L 179.7(3) . . ? N2L C3L C4L 179.6(3) . . ? 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 N1L C1L -167.5(4) . . . . ? Cl4 Te1 N1L C1L -167.3(11) . . . . ? Cl2 Te1 N1L C1L -79.5(4) . . . . ? Cl1 Te1 N1L C1L 103.5(4) . . . . ? N2L Te1 N1L C1L 13.0(4) . . . . ? Cl3 Te1 N2L C3L 170.3(4) . . . . ? Cl4 Te1 N2L C3L 163.6(7) . . . . ? Cl2 Te1 N2L C3L 75.8(7) . . . . ? Cl1 Te1 N2L C3L -107.5(7) . . . . ? N1L Te1 N2L C3L -16.4(7) . . . . ? Te1 N1L C1L C2L -175(100) . . . . ? Te1 N2L C3L C4L -162(100) . . . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 30.57 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 1.234 _refine_diff_density_min -0.530 _refine_diff_density_rms 0.097 # Attachment 'TeCl4dme.cif' data_teclm _database_code_depnum_ccdc_archive 'CCDC 750374' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'Tellurium Tetrachloride 1,2-Dimethoxyethane Solvate' ; _chemical_name_common "'Tellurium Tetrachloride 1,2-Dimethoxyethane Solvate'" _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H20 Cl4 O4 Te' _chemical_formula_weight 449.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.790(2) _cell_length_b 8.967(2) _cell_length_c 13.763(4) _cell_angle_alpha 72.544(6) _cell_angle_beta 83.443(6) _cell_angle_gamma 66.126(5) _cell_volume 838.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 947 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 30.4 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.781 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 440 _exptl_absorpt_coefficient_mu 2.410 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.885 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'SADABS 2.10 (Bruker-AXS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART CCD (Bruker-AXS)' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10420 _diffrn_reflns_av_R_equivalents 0.0114 _diffrn_reflns_av_sigmaI/netI 0.0149 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 30.54 _reflns_number_total 4963 _reflns_number_gt 4668 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker-AXS)' _computing_cell_refinement 'SAINT (Bruker-AXS)' _computing_data_reduction 'SAINT (Bruker-AXS)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep3( Farrugia, 1997)' _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^)+(0.0239P)^2^+0.1136P] 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 4963 _refine_ls_number_parameters 158 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0171 _refine_ls_R_factor_gt 0.0154 _refine_ls_wR_factor_ref 0.0407 _refine_ls_wR_factor_gt 0.0396 _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 0.577405(10) 0.304988(9) 0.290379(6) 0.02277(3) Uani 1 1 d . . . Cl1 Cl 0.36930(6) 0.60835(4) 0.21984(3) 0.04621(9) Uani 1 1 d . . . Cl2 Cl 0.77081(5) -0.00491(4) 0.34816(3) 0.03685(7) Uani 1 1 d . . . Cl3 Cl 0.32955(5) 0.26884(5) 0.39476(3) 0.03654(7) Uani 1 1 d . . . Cl4 Cl 0.46471(5) 0.24847(5) 0.16138(3) 0.03483(7) Uani 1 1 d . . . O1L O 0.68060(14) 0.28650(12) 0.48255(7) 0.03196(19) Uani 1 1 d . . . O2L O 0.80989(16) 0.48989(13) 0.31383(8) 0.0378(2) Uani 1 1 d . . . O3L O 1.14968(19) 0.14105(14) 0.03419(9) 0.0465(3) Uani 1 1 d . . . O4L O 0.81726(13) 0.32007(13) 0.15051(7) 0.0337(2) Uani 1 1 d . . . C1L C 0.6984(2) 0.13805(19) 0.56466(11) 0.0414(3) Uani 1 1 d . . . H1L1 H 0.8189 0.0494 0.5616 0.062 Uiso 1 1 calc R . . H1L2 H 0.6012 0.1010 0.5591 0.062 Uiso 1 1 calc R . . H1L3 H 0.6872 0.1643 0.6284 0.062 Uiso 1 1 calc R . . C2L C 0.8223(2) 0.34565(19) 0.48995(12) 0.0371(3) Uani 1 1 d . . . H2L1 H 0.9447 0.2635 0.4788 0.044 Uiso 1 1 calc R . . H2L2 H 0.8217 0.3580 0.5576 0.044 Uiso 1 1 calc R . . C3L C 0.7866(2) 0.51270(18) 0.41237(11) 0.0353(3) Uani 1 1 d . . . H3L1 H 0.6599 0.5921 0.4195 0.042 Uiso 1 1 calc R . . H3L2 H 0.8736 0.5592 0.4228 0.042 Uiso 1 1 calc R . . C4L C 0.8053(3) 0.6409(2) 0.23847(14) 0.0515(4) Uani 1 1 d . . . H4L1 H 0.6924 0.7347 0.2456 0.077 Uiso 1 1 calc R . . H4L2 H 0.8081 0.6263 0.1719 0.077 Uiso 1 1 calc R . . H4L3 H 0.9124 0.6631 0.2473 0.077 Uiso 1 1 calc R . . C5L C 1.2488(3) -0.0008(2) -0.00523(15) 0.0566(5) Uani 1 1 d . . . H5L1 H 1.3705 -0.0639 0.0264 0.085 Uiso 1 1 calc R . . H5L2 H 1.2627 0.0386 -0.0775 0.085 Uiso 1 1 calc R . . H5L3 H 1.1799 -0.0726 0.0088 0.085 Uiso 1 1 calc R . . C6L C 1.1210(2) 0.09025(18) 0.14021(11) 0.0364(3) Uani 1 1 d . . . H6L1 H 1.2411 0.0264 0.1753 0.044 Uiso 1 1 calc R . . H6L2 H 1.0516 0.0174 0.1549 0.044 Uiso 1 1 calc R . . C7L C 1.01308(18) 0.24430(18) 0.17721(11) 0.0321(3) Uani 1 1 d . . . H7L1 H 1.0255 0.2123 0.2507 0.039 Uiso 1 1 calc R . . H7L2 H 1.0677 0.3279 0.1485 0.039 Uiso 1 1 calc R . . C8L C 0.7715(2) 0.4304(2) 0.04869(11) 0.0376(3) Uani 1 1 d . . . H8L1 H 0.8288 0.5112 0.0357 0.056 Uiso 1 1 calc R . . H8L2 H 0.6377 0.4895 0.0415 0.056 Uiso 1 1 calc R . . H8L3 H 0.8174 0.3642 0.0009 0.056 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Te1 0.02153(4) 0.02138(4) 0.02546(4) -0.00562(3) 0.00008(3) -0.00908(3) Cl1 0.0441(2) 0.02538(14) 0.0561(2) -0.00379(14) -0.00727(17) -0.00397(13) Cl2 0.03890(17) 0.02356(13) 0.03964(17) -0.00541(12) 0.00007(13) -0.00620(12) Cl3 0.03114(15) 0.04282(17) 0.04142(17) -0.01589(14) 0.01186(13) -0.02025(13) Cl4 0.02997(15) 0.04562(17) 0.03611(16) -0.01646(13) -0.00191(12) -0.01778(13) O1L 0.0353(5) 0.0293(4) 0.0310(5) -0.0048(4) -0.0037(4) -0.0138(4) O2L 0.0525(6) 0.0325(5) 0.0362(5) -0.0128(4) 0.0047(4) -0.0232(5) O3L 0.0619(7) 0.0336(5) 0.0374(6) -0.0107(4) 0.0155(5) -0.0153(5) O4L 0.0250(4) 0.0465(5) 0.0259(4) -0.0014(4) -0.0012(3) -0.0161(4) C1L 0.0512(9) 0.0345(7) 0.0322(7) -0.0016(5) -0.0024(6) -0.0153(6) C2L 0.0349(7) 0.0409(7) 0.0371(7) -0.0099(6) -0.0067(6) -0.0153(6) C3L 0.0389(7) 0.0353(6) 0.0399(7) -0.0161(6) -0.0009(6) -0.0182(6) C4L 0.0801(13) 0.0435(8) 0.0439(9) -0.0113(7) 0.0072(8) -0.0392(9) C5L 0.0714(13) 0.0411(8) 0.0504(10) -0.0194(7) 0.0169(9) -0.0147(8) C6L 0.0376(7) 0.0346(6) 0.0361(7) -0.0076(5) 0.0046(6) -0.0162(6) C7L 0.0242(6) 0.0405(7) 0.0337(6) -0.0112(5) -0.0006(5) -0.0138(5) C8L 0.0373(7) 0.0452(7) 0.0270(6) -0.0011(5) -0.0018(5) -0.0187(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Te1 Cl4 2.3313(6) . ? Te1 Cl3 2.3431(6) . ? Te1 Cl1 2.4851(7) . ? Te1 Cl2 2.4866(7) . ? Te1 O4L 2.5380(11) . ? Te1 O1L 2.7899(12) . ? Te1 O2L 3.0030(12) . ? Te1 O3L 5.3554(15) . ? O1L C2L 1.4288(18) . ? O1L C1L 1.4325(16) . ? O2L C3L 1.4121(18) . ? O2L C4L 1.4272(19) . ? O3L C6L 1.4128(18) . ? O3L C5L 1.425(2) . ? O4L C7L 1.4362(16) . ? O4L C8L 1.4376(16) . ? C2L C3L 1.494(2) . ? C6L C7L 1.503(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl4 Te1 Cl3 89.78(2) . . ? Cl4 Te1 Cl1 87.44(2) . . ? Cl3 Te1 Cl1 88.47(2) . . ? Cl4 Te1 Cl2 86.78(2) . . ? Cl3 Te1 Cl2 90.932(19) . . ? Cl1 Te1 Cl2 174.187(14) . . ? Cl4 Te1 O4L 77.18(3) . . ? Cl3 Te1 O4L 166.85(3) . . ? Cl1 Te1 O4L 92.59(3) . . ? Cl2 Te1 O4L 86.69(3) . . ? Cl4 Te1 O1L 161.42(2) . . ? Cl3 Te1 O1L 76.32(3) . . ? Cl1 Te1 O1L 104.20(3) . . ? Cl2 Te1 O1L 81.26(2) . . ? O4L Te1 O1L 115.99(4) . . ? Cl4 Te1 O2L 139.14(2) . . ? Cl3 Te1 O2L 126.59(3) . . ? Cl1 Te1 O2L 76.93(3) . . ? Cl2 Te1 O2L 107.95(3) . . ? O4L Te1 O2L 66.28(4) . . ? O1L Te1 O2L 58.89(3) . . ? Cl4 Te1 O3L 73.87(3) . . ? Cl3 Te1 O3L 155.447(18) . . ? Cl1 Te1 O3L 108.49(2) . . ? Cl2 Te1 O3L 70.372(18) . . ? O4L Te1 O3L 16.63(3) . . ? O1L Te1 O3L 114.70(3) . . ? O2L Te1 O3L 75.78(3) . . ? C2L O1L C1L 110.57(11) . . ? C2L O1L Te1 118.89(8) . . ? C1L O1L Te1 118.59(9) . . ? C3L O2L C4L 111.01(12) . . ? C3L O2L Te1 109.92(8) . . ? C4L O2L Te1 121.09(10) . . ? C6L O3L C5L 111.94(12) . . ? C6L O3L Te1 43.48(7) . . ? C5L O3L Te1 135.75(10) . . ? C7L O4L C8L 115.43(10) . . ? C7L O4L Te1 119.07(8) . . ? C8L O4L Te1 124.09(8) . . ? O1L C2L C3L 109.90(12) . . ? O2L C3L C2L 109.42(12) . . ? O3L C6L C7L 109.64(12) . . ? O4L C7L C6L 113.13(12) . . ? 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 Cl4 Te1 O1L C2L 154.64(8) . . . . ? Cl3 Te1 O1L C2L -162.78(9) . . . . ? Cl1 Te1 O1L C2L -77.94(9) . . . . ? Cl2 Te1 O1L C2L 104.11(9) . . . . ? O4L Te1 O1L C2L 22.15(10) . . . . ? O2L Te1 O1L C2L -13.09(9) . . . . ? O3L Te1 O1L C2L 40.52(10) . . . . ? Cl4 Te1 O1L C1L 15.38(14) . . . . ? Cl3 Te1 O1L C1L 57.96(10) . . . . ? Cl1 Te1 O1L C1L 142.81(10) . . . . ? Cl2 Te1 O1L C1L -35.15(10) . . . . ? O4L Te1 O1L C1L -117.11(10) . . . . ? O2L Te1 O1L C1L -152.34(11) . . . . ? O3L Te1 O1L C1L -98.74(10) . . . . ? Cl4 Te1 O2L C3L 164.75(7) . . . . ? Cl3 Te1 O2L C3L 16.45(10) . . . . ? Cl1 Te1 O2L C3L 94.54(9) . . . . ? Cl2 Te1 O2L C3L -88.73(9) . . . . ? O4L Te1 O2L C3L -166.69(9) . . . . ? O1L Te1 O2L C3L -21.19(8) . . . . ? O3L Te1 O2L C3L -152.22(9) . . . . ? Cl4 Te1 O2L C4L 33.15(13) . . . . ? Cl3 Te1 O2L C4L -115.15(11) . . . . ? Cl1 Te1 O2L C4L -37.06(11) . . . . ? Cl2 Te1 O2L C4L 139.67(11) . . . . ? O4L Te1 O2L C4L 61.72(12) . . . . ? O1L Te1 O2L C4L -152.79(12) . . . . ? O3L Te1 O2L C4L 76.18(12) . . . . ? Cl4 Te1 O3L C6L -129.07(11) . . . . ? Cl3 Te1 O3L C6L -79.06(12) . . . . ? Cl1 Te1 O3L C6L 149.31(11) . . . . ? Cl2 Te1 O3L C6L -36.72(11) . . . . ? O4L Te1 O3L C6L 131.65(16) . . . . ? O1L Te1 O3L C6L 33.31(12) . . . . ? O2L Te1 O3L C6L 78.62(11) . . . . ? Cl4 Te1 O3L C5L -56.79(16) . . . . ? Cl3 Te1 O3L C5L -6.78(18) . . . . ? Cl1 Te1 O3L C5L -138.41(16) . . . . ? Cl2 Te1 O3L C5L 35.56(16) . . . . ? O4L Te1 O3L C5L -156.1(2) . . . . ? O1L Te1 O3L C5L 105.59(16) . . . . ? O2L Te1 O3L C5L 150.90(17) . . . . ? Cl4 Te1 O4L C7L -137.96(10) . . . . ? Cl3 Te1 O4L C7L -130.37(10) . . . . ? Cl1 Te1 O4L C7L 135.26(9) . . . . ? Cl2 Te1 O4L C7L -50.51(9) . . . . ? O1L Te1 O4L C7L 28.10(10) . . . . ? O2L Te1 O4L C7L 60.75(9) . . . . ? O3L Te1 O4L C7L -61.48(11) . . . . ? Cl4 Te1 O4L C8L 56.26(11) . . . . ? Cl3 Te1 O4L C8L 63.84(17) . . . . ? Cl1 Te1 O4L C8L -30.53(11) . . . . ? Cl2 Te1 O4L C8L 143.70(11) . . . . ? O1L Te1 O4L C8L -137.69(11) . . . . ? O2L Te1 O4L C8L -105.04(12) . . . . ? O3L Te1 O4L C8L 132.73(17) . . . . ? C1L O1L C2L C3L -172.48(12) . . . . ? Te1 O1L C2L C3L 45.26(15) . . . . ? C4L O2L C3L C2L -171.11(14) . . . . ? Te1 O2L C3L C2L 52.20(13) . . . . ? O1L C2L C3L O2L -66.34(16) . . . . ? C5L O3L C6L C7L -178.96(15) . . . . ? Te1 O3L C6L C7L -44.73(8) . . . . ? C8L O4L C7L C6L -81.56(15) . . . . ? Te1 O4L C7L C6L 111.45(11) . . . . ? O3L C6L C7L O4L 75.16(15) . . . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 30.54 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 0.508 _refine_diff_density_min -0.714 _refine_diff_density_rms 0.057 # Attachment 'TECLT.CIF' data_teclt _database_code_depnum_ccdc_archive 'CCDC 750375' _audit_creation_method SHELXL-97 _chemical_name_systematic ; tellurium tetrachloride ; _chemical_name_common 'tellurium tetrachloride' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Cl8 Te2' _chemical_formula_weight 538.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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 C2/c 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' '-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 16.917(3) _cell_length_b 10.3731(18) _cell_length_c 15.123(3) _cell_angle_alpha 90.00 _cell_angle_beta 116.866(3) _cell_angle_gamma 90.00 _cell_volume 2367.4(7) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1014 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 30.5 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.023 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1920 _exptl_absorpt_coefficient_mu 6.672 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2395 _exptl_absorpt_correction_T_max 0.3797 _exptl_absorpt_process_details 'SADABS Bruker-AXS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART CCD Bruker-AXS' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14235 _diffrn_reflns_av_R_equivalents 0.0176 _diffrn_reflns_av_sigmaI/netI 0.0160 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 30.53 _reflns_number_total 3616 _reflns_number_gt 3372 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BRUKER-AXS)' _computing_cell_refinement 'SAINT (BRUKER-AXS)' _computing_data_reduction 'SAINT (BRUKER-AXS)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP for Windows (Farrugia, 1997)' _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^)+(0.0142P)^2^+0.3791P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000489(19) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3616 _refine_ls_number_parameters 92 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0167 _refine_ls_R_factor_gt 0.0144 _refine_ls_wR_factor_ref 0.0300 _refine_ls_wR_factor_gt 0.0293 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.005 _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 0.857296(6) 1.025492(10) 0.179982(7) 0.01840(3) Uani 1 1 d . . . Te2 Te 0.997915(6) 0.732083(10) 0.108309(6) 0.01722(3) Uani 1 1 d . . . Cl2 Cl 0.75553(3) 1.01234(5) 0.24324(3) 0.03214(10) Uani 1 1 d . . . Cl1B Cl 0.99953(3) 1.01264(4) 0.12031(3) 0.02376(8) Uani 1 1 d . . . Cl2B Cl 0.86531(3) 0.74529(4) 0.18273(3) 0.02473(8) Uani 1 1 d . . . Cl3 Cl 0.75323(3) 1.02196(5) 0.01397(3) 0.03233(10) Uani 1 1 d . . . Cl6 Cl 0.88290(3) 0.73790(4) -0.05089(3) 0.02880(9) Uani 1 1 d . . . Cl4 Cl 1.10881(3) 0.74027(4) 0.05866(3) 0.02756(9) Uani 1 1 d . . . Cl5 Cl 0.99947(3) 0.50890(4) 0.12306(3) 0.02949(9) Uani 1 1 d . . . Cl1 Cl 0.86624(3) 1.24974(4) 0.18814(4) 0.03550(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Te1 0.01683(5) 0.01867(6) 0.02001(5) 0.00208(3) 0.00859(4) 0.00312(3) Te2 0.01792(5) 0.01607(6) 0.01835(4) -0.00111(3) 0.00879(4) 0.00030(3) Cl2 0.0264(2) 0.0420(3) 0.0355(2) 0.00497(18) 0.02051(17) 0.00630(18) Cl1B 0.02619(19) 0.0228(2) 0.02376(15) 0.00350(13) 0.01254(14) 0.00034(15) Cl2B 0.02190(18) 0.0256(2) 0.02672(17) -0.00083(14) 0.01105(14) -0.00358(14) Cl3 0.0251(2) 0.0438(3) 0.02208(16) 0.00331(16) 0.00544(14) 0.00300(17) Cl6 0.02460(19) 0.0343(2) 0.02145(16) 0.00103(15) 0.00505(14) -0.00294(16) Cl4 0.02394(19) 0.0320(2) 0.03221(18) 0.00443(16) 0.01750(16) 0.00464(16) Cl5 0.0421(2) 0.0167(2) 0.03232(18) -0.00032(15) 0.01918(18) 0.00012(17) Cl1 0.0458(3) 0.0193(2) 0.0416(2) 0.00263(16) 0.0200(2) 0.00383(18) _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 2.3208(5) . ? Te1 Cl3 2.3257(5) . ? Te1 Cl1 2.3307(6) . ? Te2 Cl6 2.3134(5) . ? Te2 Cl4 2.3159(5) . ? Te2 Cl5 2.3249(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl2 Te1 Cl3 95.93(2) . . ? Cl2 Te1 Cl1 94.553(18) . . ? Cl3 Te1 Cl1 94.142(18) . . ? Cl6 Te2 Cl4 94.89(2) . . ? Cl6 Te2 Cl5 95.366(16) . . ? Cl4 Te2 Cl5 95.274(15) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.53 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.414 _refine_diff_density_min -0.543 _refine_diff_density_rms 0.132 # Attachment 'tef4diethylether.cif' data_tef4eto _database_code_depnum_ccdc_archive 'CCDC 750376' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'Tellurium Tetrafluoride Diethyl Ether Solvate' ; _chemical_name_common "'Tellurium Tetrafluoride Diethyl Ether Solvate'" _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H20 F8 O2 Te2' _chemical_formula_weight 555.44 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' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.815(7) _cell_length_b 9.743(12) _cell_length_c 10.422(6) _cell_angle_alpha 92.39(7) _cell_angle_beta 105.18(6) _cell_angle_gamma 105.26(8) _cell_volume 827.5(13) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 906 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 30.5 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.229 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 520 _exptl_absorpt_coefficient_mu 3.602 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.757 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'SADABS 2.10 (Bruker-AXS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART CCD (Bruker-AXS)' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10116 _diffrn_reflns_av_R_equivalents 0.0284 _diffrn_reflns_av_sigmaI/netI 0.0426 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 30.67 _reflns_number_total 4885 _reflns_number_gt 4037 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker-AXS)' _computing_cell_refinement 'SAINT (Bruker-AXS)' _computing_data_reduction 'SAINT (Bruker-AXS)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond (Brandenburg, 2000)' _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^)+(0.1149P)^2^+42.1777P] 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 4885 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1132 _refine_ls_R_factor_gt 0.1001 _refine_ls_wR_factor_ref 0.2712 _refine_ls_wR_factor_gt 0.2623 _refine_ls_goodness_of_fit_ref 1.156 _refine_ls_restrained_S_all 1.156 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Te1 Te 1.29289(9) 0.90078(9) 0.81933(8) 0.0184(2) Uani 1 1 d . . . Te2 Te 0.78990(8) 0.82103(8) 0.87964(8) 0.0161(2) Uani 1 1 d . . . F1 F 1.3767(13) 0.8508(17) 0.6807(12) 0.059(4) Uani 1 1 d . . . F2 F 1.337(3) 1.0850(15) 0.7725(17) 0.108(8) Uani 1 1 d . . . F3 F 1.1071(16) 0.861(3) 0.6746(15) 0.114(9) Uani 1 1 d . . . F4 F 1.087(5) 0.9386(16) 0.9245(15) 0.193(19) Uani 1 1 d . . . F5 F 0.8731(14) 0.6803(18) 0.8212(19) 0.094(7) Uani 1 1 d . . . F6 F 0.8314(19) 0.7510(15) 1.0431(13) 0.067(4) Uani 1 1 d . . . F7 F 0.5941(11) 0.6673(11) 0.8215(11) 0.040(2) Uani 1 1 d . . . F8 F 0.577(5) 0.9235(18) 0.9307(15) 0.183(18) Uani 1 1 d . . . O1L O 1.2262(13) 0.6461(12) 0.8473(11) 0.030(2) Uani 1 1 d . . . O2L O 0.7309(15) 0.851(2) 0.6443(14) 0.064(6) Uani 1 1 d . . . C1L C 1.210(5) 0.459(4) 0.706(4) 0.094(10) Uiso 1 1 d . . . H1L1 H 1.1893 0.4757 0.6138 0.141 Uiso 1 1 calc R . . H1L2 H 1.1749 0.3583 0.7117 0.141 Uiso 1 1 calc R . . H1L3 H 1.3254 0.4959 0.7502 0.141 Uiso 1 1 calc R . . C2L C 1.123(4) 0.529(3) 0.769(3) 0.073(7) Uiso 1 1 d . . . H2L1 H 1.0407 0.5564 0.7011 0.088 Uiso 1 1 calc R . . H2L2 H 1.0682 0.4652 0.8215 0.088 Uiso 1 1 calc R . . C3L C 1.305(2) 0.614(2) 0.9812(19) 0.042(4) Uiso 1 1 d . . . H3L1 H 1.2891 0.5111 0.9782 0.051 Uiso 1 1 calc R . . H3L2 H 1.4218 0.6600 1.0037 0.051 Uiso 1 1 calc R . . C4L C 1.245(4) 0.657(3) 1.081(3) 0.069(7) Uiso 1 1 d . . . H4L1 H 1.2470 0.7561 1.0772 0.104 Uiso 1 1 calc R . . H4L2 H 1.3126 0.6469 1.1665 0.104 Uiso 1 1 calc R . . H4L3 H 1.1347 0.5996 1.0684 0.104 Uiso 1 1 calc R . . C5L C 0.675(5) 0.683(4) 0.538(4) 0.093(10) Uiso 1 1 d . . . H5L1 H 0.7567 0.6772 0.4928 0.111 Uiso 1 1 calc R . . H5L2 H 0.6504 0.6003 0.5854 0.111 Uiso 1 1 calc R . . C6L C 0.534(4) 0.708(4) 0.452(4) 0.086(9) Uiso 1 1 d . . . H6L1 H 0.4476 0.6190 0.4268 0.130 Uiso 1 1 calc R . . H6L2 H 0.5585 0.7441 0.3739 0.130 Uiso 1 1 calc R . . H6L3 H 0.4991 0.7758 0.4982 0.130 Uiso 1 1 calc R . . C7L C 0.748(5) 1.031(4) 0.651(4) 0.087(9) Uiso 1 1 d . . . H7L1 H 0.6588 1.0411 0.5787 0.105 Uiso 1 1 calc R . . H7L2 H 0.7257 1.0567 0.7336 0.105 Uiso 1 1 calc R . . C8L C 0.868(5) 1.122(4) 0.647(4) 0.104(12) Uiso 1 1 d . . . H8L1 H 0.9589 1.1220 0.7209 0.156 Uiso 1 1 calc R . . H8L2 H 0.8471 1.2141 0.6505 0.156 Uiso 1 1 calc R . . H8L3 H 0.8930 1.1041 0.5643 0.156 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 0.0118(3) 0.0227(4) 0.0212(4) -0.0002(3) 0.0063(3) 0.0045(3) Te2 0.0091(3) 0.0191(4) 0.0190(4) -0.0014(3) 0.0047(3) 0.0022(3) F1 0.025(5) 0.102(11) 0.044(6) -0.036(7) 0.010(4) 0.015(6) F2 0.23(3) 0.030(7) 0.070(10) 0.022(7) 0.068(14) 0.020(11) F3 0.030(6) 0.25(3) 0.055(8) -0.068(12) -0.015(5) 0.069(11) F4 0.42(5) 0.026(7) 0.031(7) -0.005(6) -0.013(15) -0.037(15) F5 0.022(5) 0.101(12) 0.133(14) -0.092(11) -0.017(7) 0.029(6) F6 0.077(9) 0.052(7) 0.046(7) 0.032(6) -0.005(6) -0.008(7) F7 0.023(4) 0.041(5) 0.045(6) -0.009(4) 0.017(4) -0.015(4) F8 0.44(5) 0.042(9) 0.027(7) -0.006(6) -0.003(15) 0.077(17) O1L 0.023(5) 0.032(6) 0.033(5) 0.007(5) 0.004(4) 0.009(4) O2L 0.018(5) 0.147(17) 0.035(7) 0.043(9) 0.010(5) 0.030(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Te1 F2 1.848(13) . ? Te1 F3 1.852(12) . ? Te1 F1 1.887(10) . ? Te1 F8 2.41(4) 1_655 ? Te1 O1L 2.443(12) . ? Te1 F4 2.45(4) . ? Te2 F6 1.845(11) . ? Te2 F5 1.866(12) . ? Te2 F7 1.899(9) . ? Te2 O2L 2.417(12) . ? Te2 F4 2.47(4) . ? Te2 F8 2.50(4) . ? F8 Te1 2.41(4) 1_455 ? O1L C2L 1.33(3) . ? O1L C3L 1.47(2) . ? O2L C7L 1.71(4) . ? O2L C5L 1.81(4) . ? C1L C2L 1.41(5) . ? C3L C4L 1.38(3) . ? C5L C6L 1.41(5) . ? C7L C8L 1.20(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F2 Te1 F3 85.6(12) . . ? F2 Te1 F1 87.5(8) . . ? F3 Te1 F1 79.4(5) . . ? F2 Te1 F8 93.7(10) . 1_655 ? F3 Te1 F8 155.3(7) . 1_655 ? F1 Te1 F8 76.0(6) . 1_655 ? F2 Te1 O1L 171.8(6) . . ? F3 Te1 O1L 88.6(9) . . ? F1 Te1 O1L 85.8(6) . . ? F8 Te1 O1L 89.1(5) 1_655 . ? F2 Te1 F4 92.2(8) . . ? F3 Te1 F4 78.0(6) . . ? F1 Te1 F4 157.3(6) . . ? F8 Te1 F4 126.6(7) 1_655 . ? O1L Te1 F4 92.3(4) . . ? F6 Te2 F5 86.0(9) . . ? F6 Te2 F7 88.2(6) . . ? F5 Te2 F7 80.4(6) . . ? F6 Te2 O2L 165.3(7) . . ? F5 Te2 O2L 80.8(8) . . ? F7 Te2 O2L 83.3(5) . . ? F6 Te2 F4 89.4(6) . . ? F5 Te2 F4 75.3(8) . . ? F7 Te2 F4 155.7(7) . . ? O2L Te2 F4 93.5(5) . . ? F6 Te2 F8 92.0(7) . . ? F5 Te2 F8 156.5(8) . . ? F7 Te2 F8 76.1(7) . . ? O2L Te2 F8 97.5(5) . . ? F4 Te2 F8 128.1(8) . . ? Te1 F4 Te2 132.8(6) . . ? Te1 F8 Te2 134.6(6) 1_455 . ? C2L O1L C3L 112.3(18) . . ? C2L O1L Te1 132.9(15) . . ? C3L O1L Te1 114.6(10) . . ? C7L O2L C5L 146.4(19) . . ? C7L O2L Te2 100.8(15) . . ? C5L O2L Te2 112.6(15) . . ? O1L C2L C1L 110(3) . . ? C4L C3L O1L 113.9(19) . . ? C6L C5L O2L 94(3) . . ? C8L C7L O2L 125(4) . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 30.67 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 7.931 _refine_diff_density_min -4.163 _refine_diff_density_rms 0.528 # Attachment 'tef4dioxan.cif' data_c2c _database_code_depnum_ccdc_archive 'CCDC 750377' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'Tellurium Tetrafluoride 1,4-Dioxane Solvate' ; _chemical_name_common "'Tellurium Tetrafluoride 1,4-Dioxane Solvate'" _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H8 F4 O2 Te' _chemical_formula_weight 291.70 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' 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 C2/c 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' '-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 15.342(3) _cell_length_b 6.9770(10) _cell_length_c 8.1064(11) _cell_angle_alpha 90.00 _cell_angle_beta 119.174(4) _cell_angle_gamma 90.00 _cell_volume 757.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 836 _cell_measurement_theta_min 2.9 _cell_measurement_theta_max 30.5 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.557 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 544 _exptl_absorpt_coefficient_mu 3.950 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.808 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'SADABS 2.10 (Bruker-AXS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART CCD (Bruker-AXS)' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4468 _diffrn_reflns_av_R_equivalents 0.0121 _diffrn_reflns_av_sigmaI/netI 0.0108 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 30.56 _reflns_number_total 1146 _reflns_number_gt 1127 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker-AXS)' _computing_cell_refinement 'SAINT (Bruker-AXS)' _computing_data_reduction 'SAINT (Bruker-AXS)' _computing_structure_solution 'SHELXS-97 (Sheldrick,1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond (Brandenburg, 2000)' _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^)+(0.0110P)^2^+0.9708P] 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 0.0133(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1146 _refine_ls_number_parameters 52 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0122 _refine_ls_R_factor_gt 0.0118 _refine_ls_wR_factor_ref 0.0287 _refine_ls_wR_factor_gt 0.0285 _refine_ls_goodness_of_fit_ref 1.182 _refine_ls_restrained_S_all 1.182 _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 1.083364(17) 0.2500 0.01274(6) Uani 1 2 d S . . F1 F 0.44625(8) 1.15502(16) -0.01586(13) 0.0260(2) Uani 1 1 d . . . F2 F 0.40454(7) 1.26219(15) 0.22822(14) 0.0252(2) Uani 1 1 d . . . O1 O 0.67046(8) 0.88308(15) 0.43460(16) 0.0172(2) Uani 1 1 d . . . C1 C 0.75783(11) 0.9207(2) 0.4164(2) 0.0181(3) Uani 1 1 d . . . H1A H 0.7701 1.0577 0.4231 0.022 Uiso 1 1 calc R . . H1B H 0.7471 0.8751 0.2948 0.022 Uiso 1 1 calc R . . C2 C 0.65280(11) 0.6796(2) 0.4268(2) 0.0174(3) Uani 1 1 d . . . H2A H 0.6405 0.6300 0.3055 0.021 Uiso 1 1 calc R . . H2B H 0.5942 0.6548 0.4396 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 0.01273(8) 0.01372(8) 0.00975(7) 0.000 0.00391(5) 0.000 F1 0.0281(5) 0.0322(5) 0.0135(4) 0.0065(4) 0.0067(4) -0.0008(4) F2 0.0240(5) 0.0207(5) 0.0274(5) 0.0001(4) 0.0099(4) 0.0079(4) O1 0.0134(5) 0.0158(5) 0.0203(5) 0.0005(4) 0.0066(4) 0.0021(4) C1 0.0147(7) 0.0187(7) 0.0184(6) 0.0028(5) 0.0062(5) 0.0003(5) C2 0.0131(6) 0.0169(6) 0.0189(6) 0.0006(5) 0.0051(5) 0.0003(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 F2 1.8657(10) 2_655 ? Te1 F2 1.8657(10) . ? Te1 F1 1.9601(10) 2_655 ? Te1 F1 1.9601(10) . ? Te1 O1 2.6864(11) . ? O1 C2 1.4407(18) . ? O1 C1 1.4424(18) . ? C1 C2 1.512(2) 7_666 ? C2 C1 1.512(2) 7_666 ? 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 F2 Te1 F2 96.06(7) 2_655 . ? F2 Te1 F1 80.52(5) 2_655 2_655 ? F2 Te1 F1 79.84(4) . 2_655 ? F2 Te1 F1 79.84(4) 2_655 . ? F2 Te1 F1 80.52(5) . . ? F1 Te1 F1 150.44(7) 2_655 . ? F2 Te1 O1 77.82(4) 2_655 . ? F2 Te1 O1 155.06(4) . . ? F1 Te1 O1 75.32(4) 2_655 . ? F1 Te1 O1 121.25(4) . . ? C2 O1 C1 109.84(11) . . ? C2 O1 Te1 112.14(8) . . ? C1 O1 Te1 123.31(8) . . ? O1 C1 C2 109.67(12) . 7_666 ? O1 C2 C1 110.20(12) . 7_666 ? 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 F2 Te1 O1 C2 -162.77(10) 2_655 . . . ? F2 Te1 O1 C2 119.25(12) . . . . ? F1 Te1 O1 C2 113.99(10) 2_655 . . . ? F1 Te1 O1 C2 -92.77(10) . . . . ? F2 Te1 O1 C1 -27.89(10) 2_655 . . . ? F2 Te1 O1 C1 -105.87(13) . . . . ? F1 Te1 O1 C1 -111.13(11) 2_655 . . . ? F1 Te1 O1 C1 42.11(12) . . . . ? C2 O1 C1 C2 -58.75(17) . . . 7_666 ? Te1 O1 C1 C2 165.49(9) . . . 7_666 ? C1 O1 C2 C1 59.07(16) . . . 7_666 ? Te1 O1 C2 C1 -159.94(9) . . . 7_666 ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 30.56 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.586 _refine_diff_density_min -0.536 _refine_diff_density_rms 0.071 # Attachment 'tef4dme.cif' data_tefdme _database_code_depnum_ccdc_archive 'CCDC 750378' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'Tellurium Tetrafluoride 1,2-Dimethoxyethane Solvate' ; _chemical_name_common "'Tellurium Tetrafluoride 1,2-Dimethoxyethane Solvate'" _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H20 F4 O4 Te' _chemical_formula_weight 383.84 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' 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 P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 7.587(3) _cell_length_b 12.256(4) _cell_length_c 8.272(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.259(7) _cell_angle_gamma 90.00 _cell_volume 721.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 948 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 30.6 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.767 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 376 _exptl_absorpt_coefficient_mu 2.107 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.829 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'SADABS 2.10 (Bruker-AXS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART CCD (Bruker-AXS)' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7732 _diffrn_reflns_av_R_equivalents 0.0202 _diffrn_reflns_av_sigmaI/netI 0.0305 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 30.57 _reflns_number_total 3669 _reflns_number_gt 3318 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker-AXS)' _computing_cell_refinement 'SAINT (Bruker-AXS)' _computing_data_reduction 'SAINT (Bruker-AXS)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep3 ( Farrugia, 1997)' _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^)+(0.0509P)^2^+2.4995P] 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 0.23(5) _refine_ls_number_reflns 3669 _refine_ls_number_parameters 159 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0427 _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_ref 0.1122 _refine_ls_wR_factor_gt 0.1089 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.105 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Te1 Te 0.26390(4) 0.59771(4) 0.82864(4) 0.02742(10) Uani 1 1 d . . . F1 F 0.4368(6) 0.5966(10) 1.0624(5) 0.082(2) Uani 1 1 d . . . F2 F 0.0471(7) 0.6392(5) 0.6290(7) 0.0640(17) Uani 1 1 d . . . F3 F 0.0917(6) 0.5701(3) 0.9407(6) 0.0427(12) Uani 1 1 d . . . F4 F 0.3234(7) 0.4502(4) 0.8139(7) 0.0466(11) Uani 1 1 d . . . O1L O 0.6352(8) 0.6556(5) 0.8486(8) 0.0499(14) Uani 1 1 d . . . O2L O 0.3858(6) 0.5929(10) 0.5357(6) 0.0525(15) Uani 1 1 d . . . O3L O 0.0671(8) 0.7974(5) 0.6499(7) 0.0440(12) Uani 1 1 d . . . O4L O 0.2671(8) 0.7912(5) 0.9917(7) 0.0430(12) Uani 1 1 d . . . C1L C 0.7343(14) 0.7290(10) 0.9857(16) 0.073(4) Uani 1 1 d . . . H1L1 H 0.8698 0.7166 1.0185 0.110 Uiso 1 1 calc R . . H1L2 H 0.6955 0.7158 1.0854 0.110 Uiso 1 1 calc R . . H1L3 H 0.7050 0.8045 0.9467 0.110 Uiso 1 1 calc R . . C2L C 0.6624(11) 0.6816(8) 0.6916(13) 0.050(2) Uani 1 1 d . . . H2L1 H 0.7983 0.6886 0.7116 0.060 Uiso 1 1 calc R . . H2L2 H 0.6012 0.7521 0.6469 0.060 Uiso 1 1 calc R . . C3L C 0.5823(9) 0.5964(14) 0.5681(8) 0.0439(16) Uani 1 1 d . . . H3L1 H 0.6061 0.6113 0.4598 0.053 Uiso 1 1 calc R . . H3L2 H 0.6402 0.5253 0.6142 0.053 Uiso 1 1 calc R . . C4L C 0.2971(16) 0.4985(9) 0.4160(12) 0.063(3) Uani 1 1 d . . . H4L1 H 0.2956 0.5152 0.2996 0.095 Uiso 1 1 calc R . . H4L2 H 0.1682 0.4875 0.4131 0.095 Uiso 1 1 calc R . . H4L3 H 0.3705 0.4320 0.4579 0.095 Uiso 1 1 calc R . . C5L C 0.044(2) 0.7867(10) 0.4701(11) 0.076(4) Uani 1 1 d . . . H5L1 H 0.0029 0.8567 0.4118 0.114 Uiso 1 1 calc R . . H5L2 H -0.0510 0.7308 0.4172 0.114 Uiso 1 1 calc R . . H5L3 H 0.1637 0.7654 0.4592 0.114 Uiso 1 1 calc R . . C6L C 0.1994(11) 0.8799(7) 0.7281(12) 0.0452(18) Uani 1 1 d . . . H6L1 H 0.1597 0.9498 0.6662 0.054 Uiso 1 1 calc R . . H6L2 H 0.3240 0.8601 0.7233 0.054 Uiso 1 1 calc R . . C7L C 0.2109(12) 0.8915(7) 0.9094(12) 0.049(2) Uani 1 1 d . . . H7L1 H 0.3031 0.9489 0.9674 0.059 Uiso 1 1 calc R . . H7L2 H 0.0870 0.9126 0.9144 0.059 Uiso 1 1 calc R . . C8L C 0.2910(15) 0.7990(10) 1.1744(11) 0.063(3) Uani 1 1 d . . . H8L1 H 0.3431 0.8707 1.2185 0.094 Uiso 1 1 calc R . . H8L2 H 0.3771 0.7417 1.2384 0.094 Uiso 1 1 calc R . . H8L3 H 0.1690 0.7899 1.1887 0.094 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 0.02768(14) 0.02536(16) 0.03131(16) 0.0027(3) 0.01287(11) -0.0004(3) F1 0.049(2) 0.160(6) 0.0334(19) -0.027(5) 0.0074(17) 0.046(5) F2 0.039(2) 0.096(5) 0.052(3) 0.017(3) 0.009(2) 0.016(2) F3 0.044(2) 0.042(3) 0.055(2) 0.0041(18) 0.0345(19) -0.0033(16) F4 0.055(3) 0.031(2) 0.059(3) 0.002(2) 0.027(2) 0.0010(19) O1L 0.042(3) 0.056(4) 0.057(3) -0.015(3) 0.024(3) -0.014(3) O2L 0.042(2) 0.075(4) 0.046(2) -0.028(5) 0.0234(19) -0.003(5) O3L 0.054(3) 0.046(3) 0.040(3) 0.005(2) 0.025(2) 0.006(2) O4L 0.060(3) 0.033(3) 0.039(3) -0.006(2) 0.021(2) -0.001(2) C1L 0.047(5) 0.083(8) 0.089(8) -0.050(7) 0.025(5) -0.025(5) C2L 0.034(3) 0.049(5) 0.074(6) 0.007(4) 0.027(4) -0.003(3) C3L 0.041(3) 0.051(4) 0.048(3) 0.010(7) 0.027(3) 0.021(6) C4L 0.088(7) 0.061(7) 0.048(5) -0.023(4) 0.031(5) -0.025(5) C5L 0.127(10) 0.070(7) 0.036(4) 0.023(4) 0.035(5) 0.047(7) C6L 0.042(4) 0.033(4) 0.068(5) 0.016(4) 0.028(4) 0.006(3) C7L 0.042(4) 0.032(4) 0.070(5) 0.002(4) 0.016(4) -0.010(3) C8L 0.066(5) 0.073(7) 0.050(5) -0.026(5) 0.022(4) 0.005(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 F3 1.876(4) . ? Te1 F4 1.878(5) . ? Te1 F1 1.924(4) . ? Te1 F2 1.952(5) . ? Te1 O4L 2.725(6) . ? Te1 O1L 2.854(6) . ? Te1 O2L 2.878(5) . ? Te1 O3L 2.979(6) . ? O1L C2L 1.420(11) . ? O1L C1L 1.439(10) . ? O2L C3L 1.422(7) . ? O2L C4L 1.520(12) . ? O3L C6L 1.414(10) . ? O3L C5L 1.441(9) . ? O4L C7L 1.398(10) . ? O4L C8L 1.461(10) . ? C2L C3L 1.441(16) . ? C6L C7L 1.479(14) . ? 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 F3 Te1 F4 94.8(2) . . ? F3 Te1 F1 81.4(2) . . ? F4 Te1 F1 87.9(4) . . ? F3 Te1 F2 86.4(2) . . ? F4 Te1 F2 110.3(2) . . ? F1 Te1 F2 159.0(3) . . ? F3 Te1 O4L 78.48(18) . . ? F4 Te1 O4L 155.4(2) . . ? F1 Te1 O4L 67.8(4) . . ? F2 Te1 O4L 93.0(2) . . ? F3 Te1 O1L 149.15(19) . . ? F4 Te1 O1L 89.3(2) . . ? F1 Te1 O1L 68.1(3) . . ? F2 Te1 O1L 120.7(2) . . ? O4L Te1 O1L 85.15(18) . . ? F3 Te1 O2L 153.4(2) . . ? F4 Te1 O2L 76.8(3) . . ? F1 Te1 O2L 122.67(17) . . ? F2 Te1 O2L 73.5(2) . . ? O4L Te1 O2L 119.0(3) . . ? O1L Te1 O2L 57.00(17) . . ? F3 Te1 O3L 94.48(17) . . ? F4 Te1 O3L 148.12(19) . . ? F1 Te1 O3L 123.7(4) . . ? F2 Te1 O3L 40.1(2) . . ? O4L Te1 O3L 56.47(16) . . ? O1L Te1 O3L 98.02(18) . . ? O2L Te1 O3L 81.4(2) . . ? C2L O1L C1L 112.3(8) . . ? C2L O1L Te1 117.1(4) . . ? C1L O1L Te1 115.9(5) . . ? C3L O2L C4L 110.1(9) . . ? C3L O2L Te1 117.6(4) . . ? C4L O2L Te1 111.4(6) . . ? C6L O3L C5L 110.5(8) . . ? C6L O3L Te1 101.9(4) . . ? C5L O3L Te1 107.4(5) . . ? C7L O4L C8L 110.7(8) . . ? C7L O4L Te1 125.1(5) . . ? C8L O4L Te1 123.1(6) . . ? O1L C2L C3L 109.1(7) . . ? O2L C3L C2L 108.2(8) . . ? O3L C6L C7L 108.4(6) . . ? O4L C7L C6L 108.1(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 F3 Te1 O1L C2L -168.7(5) . . . . ? F4 Te1 O1L C2L 93.1(6) . . . . ? F1 Te1 O1L C2L -179.0(7) . . . . ? F2 Te1 O1L C2L -20.3(7) . . . . ? O4L Te1 O1L C2L -110.9(6) . . . . ? O2L Te1 O1L C2L 18.5(6) . . . . ? O3L Te1 O1L C2L -55.8(6) . . . . ? F3 Te1 O1L C1L -32.5(9) . . . . ? F4 Te1 O1L C1L -130.7(8) . . . . ? F1 Te1 O1L C1L -42.7(8) . . . . ? F2 Te1 O1L C1L 116.0(8) . . . . ? O4L Te1 O1L C1L 25.3(8) . . . . ? O2L Te1 O1L C1L 154.7(9) . . . . ? O3L Te1 O1L C1L 80.5(8) . . . . ? F3 Te1 O2L C3L -156.2(8) . . . . ? F4 Te1 O2L C3L -82.4(10) . . . . ? F1 Te1 O2L C3L -3.7(12) . . . . ? F2 Te1 O2L C3L 161.4(11) . . . . ? O4L Te1 O2L C3L 77.2(10) . . . . ? O1L Te1 O2L C3L 15.5(9) . . . . ? O3L Te1 O2L C3L 121.0(10) . . . . ? F3 Te1 O2L C4L -27.8(11) . . . . ? F4 Te1 O2L C4L 46.0(7) . . . . ? F1 Te1 O2L C4L 124.7(8) . . . . ? F2 Te1 O2L C4L -70.2(7) . . . . ? O4L Te1 O2L C4L -154.4(7) . . . . ? O1L Te1 O2L C4L 144.0(8) . . . . ? O3L Te1 O2L C4L -110.6(7) . . . . ? F3 Te1 O3L C6L 113.7(5) . . . . ? F4 Te1 O3L C6L -139.8(5) . . . . ? F1 Te1 O3L C6L 31.0(5) . . . . ? F2 Te1 O3L C6L -167.2(6) . . . . ? O4L Te1 O3L C6L 40.7(4) . . . . ? O1L Te1 O3L C6L -38.0(5) . . . . ? O2L Te1 O3L C6L -92.7(5) . . . . ? F3 Te1 O3L C5L -130.1(7) . . . . ? F4 Te1 O3L C5L -23.6(8) . . . . ? F1 Te1 O3L C5L 147.2(7) . . . . ? F2 Te1 O3L C5L -51.0(7) . . . . ? O4L Te1 O3L C5L 156.9(8) . . . . ? O1L Te1 O3L C5L 78.2(7) . . . . ? O2L Te1 O3L C5L 23.5(7) . . . . ? F3 Te1 O4L C7L -117.3(6) . . . . ? F4 Te1 O4L C7L 166.7(6) . . . . ? F1 Te1 O4L C7L 157.4(7) . . . . ? F2 Te1 O4L C7L -31.5(6) . . . . ? O1L Te1 O4L C7L 89.0(6) . . . . ? O2L Te1 O4L C7L 41.2(6) . . . . ? O3L Te1 O4L C7L -13.9(5) . . . . ? F3 Te1 O4L C8L 49.6(7) . . . . ? F4 Te1 O4L C8L -26.4(9) . . . . ? F1 Te1 O4L C8L -35.7(7) . . . . ? F2 Te1 O4L C8L 135.4(7) . . . . ? O1L Te1 O4L C8L -104.1(7) . . . . ? O2L Te1 O4L C8L -151.9(6) . . . . ? O3L Te1 O4L C8L 153.0(7) . . . . ? C1L O1L C2L C3L 171.8(8) . . . . ? Te1 O1L C2L C3L -50.4(8) . . . . ? C4L O2L C3L C2L -175.8(9) . . . . ? Te1 O2L C3L C2L -46.8(12) . . . . ? O1L C2L C3L O2L 62.7(10) . . . . ? C5L O3L C6L C7L 177.1(7) . . . . ? Te1 O3L C6L C7L -69.0(6) . . . . ? C8L O4L C7L C6L 176.9(7) . . . . ? Te1 O4L C7L C6L -14.8(8) . . . . ? O3L C6L C7L O4L 59.6(8) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 30.57 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 2.198 _refine_diff_density_min -1.067 _refine_diff_density_rms 0.146 # Attachment 'TECL4_Dioxan.CIF' data_tecl4d _database_code_depnum_ccdc_archive 'CCDC 750379' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'Tellurium Tetrachloride 1,4-Dioxane Solvate' ; _chemical_name_common "'Tellurium Tetrachloride 1,4-Dioxane Solvate'" _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H8 Cl4 O2 Te' _chemical_formula_weight 357.50 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' 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 P2(1)/m 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 6.168(2) _cell_length_b 12.863(5) _cell_length_c 6.684(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.181(6) _cell_angle_gamma 90.00 _cell_volume 530.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 941 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 30.5 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.239 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 336 _exptl_absorpt_coefficient_mu 3.767 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.661 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'SADABS 2.10 (BRUKER-AXS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART CCD (BRUKER-AXS)' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6390 _diffrn_reflns_av_R_equivalents 0.0227 _diffrn_reflns_av_sigmaI/netI 0.0189 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 30.48 _reflns_number_total 1629 _reflns_number_gt 1495 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker-AXS)' _computing_cell_refinement 'SAINT (Bruker-AXS)' _computing_data_reduction 'SAINT (Bruker-AXS)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond (Brandenburg, 2000)' _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^)+(0.0899P)^2^+0.6577P] 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 1629 _refine_ls_number_parameters 55 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0488 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.1297 _refine_ls_wR_factor_gt 0.1257 _refine_ls_goodness_of_fit_ref 1.167 _refine_ls_restrained_S_all 1.167 _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 0.28366(6) 0.2500 0.24613(5) 0.02138(16) Uani 1 2 d S . . Cl1 Cl 0.0062(3) 0.2500 -0.0235(3) 0.0335(3) Uani 1 2 d S . . Cl2 Cl 0.5762(3) 0.2500 0.5016(3) 0.0373(4) Uani 1 2 d S . . Cl3 Cl 0.46587(19) 0.11905(8) 0.07327(16) 0.0311(2) Uani 1 1 d . . . O1 O 0.0994(5) 0.0868(2) 0.4097(4) 0.0283(6) Uani 1 1 d . . . C1 C -0.0042(10) 0.0072(4) 0.2924(6) 0.0401(12) Uani 1 1 d . . . H1A H 0.1037 -0.0463 0.2552 0.048 Uiso 1 1 calc R . . H1B H -0.0629 0.0380 0.1678 0.048 Uiso 1 1 calc R . . C2 C -0.1850(9) -0.0424(4) 0.4087(7) 0.0371(10) Uani 1 1 d . . . H2A H -0.2963 0.0103 0.4413 0.044 Uiso 1 1 calc R . . H2B H -0.2544 -0.0974 0.3269 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 0.0283(2) 0.0108(2) 0.0251(2) 0.000 0.00124(14) 0.000 Cl1 0.0340(7) 0.0255(7) 0.0409(8) 0.000 -0.0079(6) 0.000 Cl2 0.0476(9) 0.0259(7) 0.0382(8) 0.000 -0.0124(7) 0.000 Cl3 0.0372(5) 0.0198(4) 0.0363(5) -0.0062(3) 0.0025(4) 0.0061(4) O1 0.0378(16) 0.0206(13) 0.0266(13) 0.0039(10) -0.0015(12) -0.0076(12) C1 0.058(3) 0.037(2) 0.0246(18) 0.0022(17) -0.0037(19) -0.021(2) C2 0.044(2) 0.034(2) 0.033(2) 0.0097(17) -0.0091(19) -0.012(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Te1 Cl3 2.3331(12) 4_565 ? Te1 Cl3 2.3331(11) . ? Te1 Cl2 2.4804(17) . ? Te1 Cl1 2.4817(17) . ? O1 C1 1.438(5) . ? O1 C2 1.441(5) 3_556 ? C1 C2 1.504(7) . ? C2 O1 1.441(5) 3_556 ? 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 92.42(6) 4_565 . ? Cl3 Te1 Cl2 89.44(5) 4_565 . ? Cl3 Te1 Cl2 89.44(5) . . ? Cl3 Te1 Cl1 88.42(5) 4_565 . ? Cl3 Te1 Cl1 88.42(5) . . ? Cl2 Te1 Cl1 176.92(6) . . ? C1 O1 C2 109.8(3) . 3_556 ? O1 C1 C2 110.5(4) . . ? O1 C2 C1 109.5(4) 3_556 . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 30.48 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 6.105 _refine_diff_density_min -1.082 _refine_diff_density_rms 0.364