#------------------------------------------------------------------------------ #$Date: 2008-02-08 10:23:56 +0000 (Fri, 08 Feb 2008) $ #$Revision: 101 $ #$URL: svn://www.crystallography.net/cod/cif/2/2203563.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_2203563 loop_ _publ_author_name 'N\"arhi, Sari M.' 'Oilunkaniemi, Raija' 'Laitinen, Risto S.' 'Ahlgr\'en, Markku' _publ_section_title ' Bis(triphenyltelluronium) hexachlorotellurate' _journal_issue 5 _journal_name_full 'Acta Crystallographica, Section E' _journal_page_first o798 _journal_page_last o800 _journal_volume 60 _journal_year 2004 _chemical_formula_iupac '2C18 H15 Te +, Cl6 Te 2-' _chemical_formula_moiety '2C18 H15 Te +, Cl6 Te 2-' _chemical_formula_sum 'C36 H30 Cl6 Te3' _chemical_formula_weight 1058.10 _chemical_name_systematic ; Bis(triphenyltelluronium) hexachlorotellurate ; _symmetry_cell_setting hexagonal _symmetry_space_group_name_Hall '-R 3' _symmetry_space_group_name_H-M 'R -3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_formula_units_Z 3 _cell_length_a 14.217(2) _cell_length_b 14.217(2) _cell_length_c 15.852(3) _cell_measurement_reflns_used 1137 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 25.98 _cell_measurement_theta_min 3.06 _cell_volume 2774.8(8) _computing_cell_refinement 'DENZO--SMN (Otwinowski & Minor, 1997)' _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_data_reduction DENZO--SMN _computing_molecular_graphics 'DIAMOND (Branderburg & Berndt, 1999)' _computing_publication_material 'WinGX (Farrugia, 1999)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker-Nonius KappaCCD' _diffrn_measurement_method '\f scans, and \w scans with \k offsets' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0675 _diffrn_reflns_av_sigmaI/netI 0.0234 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 14235 _diffrn_reflns_theta_full 25.98 _diffrn_reflns_theta_max 25.98 _diffrn_reflns_theta_min 3.06 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.809 _exptl_absorpt_correction_T_max 0.6002 _exptl_absorpt_correction_T_min 0.5132 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(SHELXTL; Bruker, 2001)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.900 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1512 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _refine_diff_density_max 1.247 _refine_diff_density_min -0.851 _refine_ls_extinction_coef 0.00072(16) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL97 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 70 _refine_ls_number_reflns 1210 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.103 _refine_ls_R_factor_all 0.0373 _refine_ls_R_factor_gt 0.0320 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0462P)^2^+22.1387P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0811 _refine_ls_wR_factor_ref 0.0828 _reflns_number_gt 1137 _reflns_number_total 1210 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file ci6357.cif loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol Te1 0.3333 0.6667 0.39175(3) 0.0169(2) Uani d S 1 Te Te2 0.3333 0.6667 0.6667 0.0134(2) Uani d S 1 Te Cl1 0.24785(9) 0.49939(8) 0.76098(6) 0.0237(3) Uani d . 1 Cl C1 0.2171(3) 0.5268(3) 0.3257(2) 0.0177(8) Uani d . 1 C C2 0.1097(3) 0.4807(3) 0.3509(3) 0.0230(8) Uani d . 1 C H2 0.0898 0.5119 0.3956 0.028 Uiso calc R 1 H C3 0.0312(3) 0.3878(4) 0.3096(3) 0.0262(9) Uani d . 1 C H3 -0.0429 0.3557 0.3257 0.031 Uiso calc R 1 H C4 0.0612(4) 0.3423(3) 0.2451(3) 0.0243(9) Uani d . 1 C H4 0.0073 0.2792 0.2170 0.029 Uiso calc R 1 H C5 0.1683(4) 0.3875(3) 0.2215(3) 0.0235(8) Uani d . 1 C H5 0.1881 0.3546 0.1782 0.028 Uiso calc R 1 H C6 0.2479(3) 0.4817(3) 0.2609(3) 0.0218(8) Uani d . 1 C H6 0.3217 0.5144 0.2439 0.026 Uiso calc R 1 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Te1 0.0182(2) 0.0182(2) 0.0143(3) 0.00909(11) 0.000 0.000 Te2 0.0145(2) 0.0145(2) 0.0114(3) 0.00724(12) 0.000 0.000 Cl1 0.0299(5) 0.0170(5) 0.0191(5) 0.0078(4) 0.0012(4) 0.0016(3) C1 0.0187(18) 0.0160(18) 0.0165(18) 0.0072(15) -0.0007(14) 0.0013(14) C2 0.022(2) 0.024(2) 0.025(2) 0.0128(17) 0.0033(16) -0.0031(16) C3 0.020(2) 0.024(2) 0.033(2) 0.0091(17) 0.0029(17) 0.0017(17) C4 0.029(2) 0.0190(19) 0.024(2) 0.0111(17) -0.0032(17) -0.0008(16) C5 0.030(2) 0.022(2) 0.0193(19) 0.0142(18) 0.0004(16) -0.0014(16) C6 0.0191(19) 0.021(2) 0.024(2) 0.0094(16) 0.0034(15) -0.0005(16) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Te1 C1 3_565 2.120(4) yes Te1 C1 . 2.120(4) no Te1 C1 2_665 2.120(4) no Te2 Cl1 3_565 2.5451(10) yes Te2 Cl1 14_456 2.5451(10) no Te2 Cl1 13_566 2.5451(10) no Te2 Cl1 2_665 2.5451(10) no Te2 Cl1 . 2.5451(10) no Te2 Cl1 15_556 2.5451(10) no C1 C2 . 1.386(6) no C1 C6 . 1.392(6) no C2 C3 . 1.394(6) no C2 H2 . 0.9500 no C3 C4 . 1.387(6) no C3 H3 . 0.9500 no C4 C5 . 1.375(6) no C4 H4 . 0.9500 no C5 C6 . 1.396(6) no C5 H5 . 0.9500 no C6 H6 . 0.9500 no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C1 Te1 C1 3_565 . 97.72(13) yes C1 Te1 C1 3_565 2_665 97.72(13) no C1 Te1 C1 . 2_665 97.72(13) no Cl1 Te2 Cl1 3_565 14_456 91.01(3) yes Cl1 Te2 Cl1 3_565 13_566 91.01(3) no Cl1 Te2 Cl1 14_456 13_566 88.99(3) yes Cl1 Te2 Cl1 3_565 2_665 88.99(3) no Cl1 Te2 Cl1 14_456 2_665 180.0 yes Cl1 Te2 Cl1 13_566 2_665 91.01(3) no Cl1 Te2 Cl1 3_565 . 88.99(3) no Cl1 Te2 Cl1 14_456 . 91.01(3) no Cl1 Te2 Cl1 13_566 . 180.0 no Cl1 Te2 Cl1 2_665 . 88.99(3) no Cl1 Te2 Cl1 3_565 15_556 180.00(3) no Cl1 Te2 Cl1 14_456 15_556 88.99(3) no Cl1 Te2 Cl1 13_566 15_556 88.99(3) no Cl1 Te2 Cl1 2_665 15_556 91.01(3) no Cl1 Te2 Cl1 . 15_556 91.01(3) ? C2 C1 C6 . . 121.4(4) no C2 C1 Te1 . . 117.3(3) no C6 C1 Te1 . . 121.3(3) no C1 C2 C3 . . 118.9(4) no C1 C2 H2 . . 120.5 no C3 C2 H2 . . 120.5 no C4 C3 C2 . . 120.1(4) no C4 C3 H3 . . 120.0 no C2 C3 H3 . . 120.0 no C5 C4 C3 . . 120.6(4) no C5 C4 H4 . . 119.7 no C3 C4 H4 . . 119.7 no C4 C5 C6 . . 120.3(4) no C4 C5 H5 . . 119.9 no C6 C5 H5 . . 119.9 no C1 C6 C5 . . 118.7(4) no C1 C6 H6 . . 120.6 no C5 C6 H6 . . 120.6 no 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_site_symmetry_1 _geom_torsion _geom_torsion_publ_flag C1 Te1 C1 C2 3_565 -82.3(4) no C1 Te1 C1 C2 2_665 178.7(3) no C1 Te1 C1 C6 3_565 99.1(2) no C1 Te1 C1 C6 2_665 0.2(4) no C6 C1 C2 C3 . -0.6(6) no Te1 C1 C2 C3 . -179.2(3) no C1 C2 C3 C4 . 0.7(6) no C2 C3 C4 C5 . 0.4(6) no C3 C4 C5 C6 . -1.6(6) no C2 C1 C6 C5 . -0.6(6) no Te1 C1 C6 C5 . 177.9(3) no C4 C5 C6 C1 . 1.7(6) no