# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1729 data_global # 1. SUBMISSION DETAILS _publ_contact_autor_name ; Prof. em. Dr. mult. Dr.h.c. Alois Hass ; _publ_contact_autor_address ; Institut f\"ur Anorganische Chemie Rhur-Universit\"at Bochum Universit\"atsstr. 150 Geb\"aude FNO 034 44780 Bochum Bundesrepublik Deutschland ; _publ_contact_author_phone '049 234 700 3004' _publ_contact_author_fax '049 234 7094 541' _publ_contact_author_email 'alois.haas@ruhr-uni-bochum.de' _publ_requested_journal 'J. Chem. Soc., DALTON Trans.' #======================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Perfluoroalkyltellurocarbonyl fluorides, their cyclic dimers and perfluoroalkane-tellurenyl iodides: preparation and reactivity ; loop_ _publ_author_name 'Baum, Michael' 'Beck, Johannes' 'Haas, Alois' 'Herrendorf, Wolfgang' 'Monse, Christian' data_(CF3)2CTe _audit_creation_method SHELXL _chemical_name_systematic ; '2,2,4,4-Tetrakis(trifluormethyl)-1,3-ditelluretane' ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[(CF3)2CTe]2' _chemical_formula_analytical ? _chemical_formula_sum 'C6 F12 Te2' _chemical_formula_weight 555.26 _chemical_melting_point ? _chemical_compound_source 'synthetic' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Te' 'Te' -0.5310 1.6750 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0030 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0170 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.603(6) _cell_length_b 7.256(6) _cell_length_c 11.538(8) _cell_angle_alpha 90.00 _cell_angle_beta 105.715(7) _cell_angle_gamma 90.00 _cell_volume 613.0(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 94 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'plate' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid ? _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.008 _exptl_crystal_density_method ? _exptl_crystal_F_000 496 _exptl_absorpt_coefficient_mu 4.896 _exptl_absorpt_correction_type 'numerical' _exptl_absorpt_correction_T_min 0.6106 _exptl_absorpt_correction_T_max 0.6878 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'STOE STADI 4 four circle diffractometer' _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7100 _diffrn_reflns_av_R_equivalents 0.0272 _diffrn_reflns_av_sigmaI/netI 0.0187 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 29.99 _reflns_number_total 1789 _reflns_number_observed 1423 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 6 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0158P)^2^+0.6534P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0037(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1783 _refine_ls_number_parameters 92 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0397 _refine_ls_R_factor_obs 0.0249 _refine_ls_wR_factor_all 0.0570 _refine_ls_wR_factor_obs 0.0494 _refine_ls_goodness_of_fit_all 1.108 _refine_ls_goodness_of_fit_obs 1.108 _refine_ls_restrained_S_all 1.132 _refine_ls_restrained_S_obs 1.108 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Te Te 0.09495(3) 0.41920(4) 0.40042(2) 0.05660(11) Uani 1 d . . C1 C 0.1699(4) 0.5866(5) 0.5623(3) 0.0456(7) Uani 1 d . . C11 C 0.3169(5) 0.4929(6) 0.6615(3) 0.0595(9) Uani 1 d . . C21 C 0.2244(5) 0.7814(6) 0.5394(4) 0.0618(9) Uani 1 d . . F11 F 0.3531(4) 0.5875(4) 0.7635(2) 0.0960(9) Uani 1 d . . F12 F 0.4737(3) 0.4770(5) 0.6326(3) 0.0868(8) Uani 1 d . . F13 F 0.2705(4) 0.3259(4) 0.6858(3) 0.0885(8) Uani 1 d . . F21 F 0.2336(4) 0.8905(4) 0.6326(3) 0.0910(8) Uani 1 d . . F22 F 0.3866(4) 0.7884(4) 0.5166(3) 0.0910(8) Uani 1 d . . F23 F 0.1066(4) 0.8586(4) 0.4467(3) 0.0851(8) Uani 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 Te 0.04523(14) 0.0781(2) 0.05019(15) -0.01917(12) 0.01934(9) 0.00001(12) C1 0.0393(15) 0.056(2) 0.042(2) -0.0046(14) 0.0113(12) 0.0029(15) C11 0.046(2) 0.077(3) 0.052(2) 0.004(2) 0.008(2) 0.004(2) C21 0.056(2) 0.063(2) 0.066(2) -0.004(2) 0.016(2) 0.000(2) F11 0.094(2) 0.131(3) 0.0483(13) -0.0136(15) -0.0057(13) 0.010(2) F12 0.0455(12) 0.126(2) 0.088(2) 0.023(2) 0.0161(12) 0.0216(14) F13 0.079(2) 0.087(2) 0.089(2) 0.034(2) 0.0070(14) 0.0069(15) F21 0.106(2) 0.069(2) 0.096(2) -0.0310(14) 0.024(2) -0.0134(15) F22 0.069(2) 0.085(2) 0.130(2) 0.013(2) 0.045(2) -0.0094(14) F23 0.091(2) 0.070(2) 0.088(2) 0.0178(14) 0.0124(15) 0.0088(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 Te C1 2.171(3) 3_566 ? Te C1 2.172(3) . ? Te Te 3.2463(4) 3_566 ? C1 C21 1.517(5) . ? C1 C11 1.526(5) . ? C1 Te 2.171(3) 3_566 ? C11 F13 1.314(5) . ? C11 F11 1.325(5) . ? C11 F12 1.328(4) . ? C21 F23 1.320(5) . ? C21 F21 1.322(5) . ? C21 F22 1.329(4) . ? 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 C1 Te C1 83.23(13) 3_566 . ? C1 Te Te 41.63(8) 3_566 3_566 ? C1 Te Te 41.60(8) . 3_566 ? C21 C1 C11 111.6(3) . . ? C21 C1 Te 111.4(2) . 3_566 ? C11 C1 Te 111.9(2) . 3_566 ? C21 C1 Te 113.1(2) . . ? C11 C1 Te 111.3(2) . . ? Te C1 Te 96.77(12) 3_566 . ? F13 C11 F11 107.0(4) . . ? F13 C11 F12 106.6(4) . . ? F11 C11 F12 106.5(3) . . ? F13 C11 C1 112.8(3) . . ? F11 C11 C1 111.6(3) . . ? F12 C11 C1 112.0(3) . . ? F23 C21 F21 106.2(4) . . ? F23 C21 F22 106.6(3) . . ? F21 C21 F22 106.9(3) . . ? F23 C21 C1 112.3(3) . . ? F21 C21 C1 111.9(3) . . ? F22 C21 C1 112.5(3) . . ? _refine_diff_density_max 0.900 _refine_diff_density_min -0.879 _refine_diff_density_rms 0.083 #===END data_(CF3)ClCTe _audit_creation_method SHELXL _chemical_name_systematic ; trans-2,4-Bis(trifluormethyl)-2,4-dichloro-1,3,ditelluretane ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[(CF3)(Cl)CTe]2' _chemical_formula_analytical ? _chemical_formula_sum 'C4 Cl2 F6 Te2' _chemical_formula_weight 488.14 _chemical_melting_point ? _chemical_compound_source 'synthetic' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Te' 'Te' -0.5310 1.6750 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1480 0.1590 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0170 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0030 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.771(7) _cell_length_b 6.749(2) _cell_length_c 10.685(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.30(4) _cell_angle_gamma 90.00 _cell_volume 540.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'plate' _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid ? _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.999 _exptl_crystal_density_method ? _exptl_crystal_F_000 432 _exptl_absorpt_coefficient_mu 5.932 _exptl_absorpt_correction_type 'numerical' _exptl_absorpt_correction_T_min 0.413 _exptl_absorpt_correction_T_max 0.6030 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'STOE STADI 4 four circle diffractometer' _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6245 _diffrn_reflns_av_R_equivalents 0.0609 _diffrn_reflns_av_sigmaI/netI 0.0362 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 29.98 _reflns_number_total 1566 _reflns_number_observed 1369 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 3 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0609P)^2^+10.8639P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1563 _refine_ls_number_parameters 64 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1373 _refine_ls_R_factor_obs 0.1254 _refine_ls_wR_factor_all 0.2535 _refine_ls_wR_factor_obs 0.2431 _refine_ls_goodness_of_fit_all 1.228 _refine_ls_goodness_of_fit_obs 1.278 _refine_ls_restrained_S_all 1.257 _refine_ls_restrained_S_obs 1.278 _refine_ls_shift/esd_max 0.003 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group F1 F 0.4625(17) -0.0290(26) 0.1220(14) 0.115(5) Uani 1 d . . F2 F 0.3035(20) 0.1588(28) 0.1751(14) 0.119(5) Uani 1 d . . F3 F 0.3495(18) -0.0937(28) 0.2782(13) 0.125(5) Uani 1 d . . C2 C 0.3269(25) -0.0009(34) 0.1651(19) 0.072(5) Uani 1 d . . Cl Cl 0.2144(11) -0.3559(10) 0.0485(9) 0.127(3) Uani 1 d . . Te Te -0.08224(14) -0.0619(3) 0.12116(11) 0.0814(6) Uani 1 d . . C1 C 0.1639(19) -0.1021(17) 0.0652(14) 0.048(3) Uani 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 F1 0.066(7) 0.166(14) 0.112(10) 0.008(9) 0.020(7) -0.005(8) F2 0.105(10) 0.136(12) 0.101(9) -0.038(10) 0.000(8) -0.048(10) F3 0.088(8) 0.196(17) 0.084(8) 0.011(10) 0.007(7) 0.009(10) C2 0.065(10) 0.085(13) 0.067(10) 0.010(10) 0.022(8) 0.037(10) Cl 0.147(6) 0.083(4) 0.167(7) -0.012(4) 0.068(5) 0.017(4) Te 0.0494(6) 0.1420(14) 0.0550(6) 0.0248(7) 0.0178(4) 0.0150(7) C1 0.064(8) 0.022(5) 0.059(7) 0.005(5) 0.018(6) 0.013(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 F1 C2 1.27(2) . ? F2 C2 1.10(2) . ? F3 C2 1.33(2) . ? C2 C1 1.58(3) . ? Cl C1 1.777(13) . ? Te C1 2.166(14) . ? Te C1 2.220(13) 3 ? Te Te 3.284(2) 3 ? C1 Te 2.220(13) 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 F2 C2 F1 110.7(23) . . ? F2 C2 F3 111.0(20) . . ? F1 C2 F3 109.7(15) . . ? F2 C2 C1 111.4(15) . . ? F1 C2 C1 106.5(16) . . ? F3 C2 C1 107.5(18) . . ? C1 Te C1 83.1(5) . 3 ? C1 Te Te 42.1(4) . 3 ? C1 Te Te 40.9(4) 3 3 ? C2 C1 Cl 109.0(11) . . ? C2 C1 Te 111.6(10) . . ? Cl C1 Te 112.5(7) . . ? C2 C1 Te 112.3(10) . 3 ? Cl C1 Te 114.2(8) . 3 ? Te C1 Te 96.9(5) . 3 ? _refine_diff_density_max 1.713 _refine_diff_density_min -0.872 _refine_diff_density_rms 0.214