#------------------------------------------------------------------------------ #$Date: 2016-03-22 10:06:16 +0000 (Tue, 22 Mar 2016) $ #$Revision: 178934 $ #$URL: svn://www.crystallography.net/cod/cif/4/11/63/4116383.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_4116383 loop_ _publ_author_name 'Thomas Drews' 'Wolfram Koch' 'Konrad Seppelt' _publ_contact_author ; Prof. Dr. Konrad Seppelt Institut f\"ur Anorganische und Analytische Chemie Freie Universit\"at Berlin Fabeckstr. 34-36 14195 Berlin Bundesrepublik Deutschland ; _publ_contact_author_email seppelt@chemie.fu-berlin.de _publ_contact_author_fax '049 30 8382424' _publ_contact_author_phone '049 30 8384289' _publ_section_title ; The Cl2O2+ Cation: Preparation and Structural Investigation of Cl2O2+SbF6- and Cl2O2+Sb2F11- ; _journal_name_full 'Journal of the American Chemical Society' _journal_page_first 4379 _journal_page_last 4384 _journal_paper_doi 10.1021/ja984474y _journal_volume 121 _journal_year 1999 _chemical_formula_sum 'Cl3 F6 Sb' _chemical_formula_weight 342.10 _chemical_name_systematic ; Trichloroniumhexafluoroantimonate ; _space_group_IT_number 64 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-C 2ac 2' _symmetry_space_group_name_H-M 'C m c a' _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 90.00 _cell_formula_units_Z 8 _cell_length_a 10.553(2) _cell_length_b 11.361(3) _cell_length_c 12.081(3) _cell_measurement_reflns_used 25 _cell_measurement_temperature 130 _cell_measurement_theta_max 21 _cell_measurement_theta_min 20 _cell_volume 1448.4(6) _computing_cell_refinement 'Enraf-Nonius CAD4' _computing_data_collection 'Enraf-Nonius CAD4' _computing_data_reduction 'Molen Delft Instruments' _computing_molecular_graphics Schakal _computing_publication_material SHELXL-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Enraf-Nonius CAD4' _diffrn_measurement_method Omega-scan _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0158 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 1103 _diffrn_reflns_theta_full 29.96 _diffrn_reflns_theta_max 29.96 _diffrn_reflns_theta_min 3.13 _diffrn_standards_interval_time '14400 sec' _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 4.950 _exptl_absorpt_correction_T_max 0.98 _exptl_absorpt_correction_T_min 0.81 _exptl_absorpt_correction_type psi-scan _exptl_crystal_colour orange-yellow _exptl_crystal_density_diffrn 3.138 _exptl_crystal_description needles _exptl_crystal_F_000 1248 _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _refine_diff_density_max 1.238 _refine_diff_density_min -1.030 _refine_diff_density_rms 0.137 _refine_ls_extinction_coef 0.00088(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 52 _refine_ls_number_reflns 1103 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.013 _refine_ls_R_factor_all 0.0220 _refine_ls_R_factor_gt 0.0189 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0239P)^2^+8.0794P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0461 _refine_ls_wR_factor_ref 0.0489 _reflns_number_gt 1024 _reflns_number_total 1103 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ja984474y_3.cif _cod_data_source_block cl3sbf6 _cod_database_code 4116383 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, -z' 'x, -y+1/2, z+1/2' 'x, y+1/2, -z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, -z' 'x+1/2, -y+1, z+1/2' 'x+1/2, y+1, -z+1/2' '-x, -y, -z' '-x, y, z' '-x, y-1/2, -z-1/2' '-x, -y-1/2, z-1/2' '-x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, z' '-x+1/2, y, -z-1/2' '-x+1/2, -y, z-1/2' 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 Sb1 Sb 0.0000 0.206482(18) 0.556678(17) 0.01002(9) Uani 1 2 d S F1 F 0.0000 0.35707(19) 0.48840(19) 0.0197(4) Uani 1 2 d S F2 F 0.12732(16) 0.15965(16) 0.45911(14) 0.0223(3) Uani 1 1 d . F3 F 0.12386(15) 0.26198(14) 0.65557(13) 0.0200(3) Uani 1 1 d . F4 F 0.0000 0.06102(19) 0.62881(19) 0.0204(5) Uani 1 2 d S Cl2 Cl -0.2500 0.43690(7) 0.7500 0.01460(16) Uani 1 2 d S Cl3 Cl -0.16469(6) 0.54192(5) 0.64349(5) 0.01569(13) 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 Sb1 0.01153(12) 0.00903(12) 0.00951(12) -0.00009(7) 0.000 0.000 F1 0.0260(11) 0.0140(10) 0.0190(10) 0.0062(8) 0.000 0.000 F2 0.0202(8) 0.0250(8) 0.0218(7) -0.0054(6) 0.0088(6) 0.0021(7) F3 0.0202(8) 0.0187(7) 0.0210(7) -0.0013(6) -0.0080(6) -0.0030(6) F4 0.0301(12) 0.0098(9) 0.0213(11) 0.0046(8) 0.000 0.000 Cl2 0.0184(4) 0.0125(3) 0.0128(3) 0.000 0.0052(3) 0.000 Cl3 0.0182(3) 0.0159(3) 0.0130(2) 0.00237(19) 0.0035(2) -0.0010(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Sb Sb -0.5866 1.5461 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 F2 Sb1 F2 92.19(11) 10 . F2 Sb1 F4 92.43(8) 10 . F2 Sb1 F4 92.43(8) . . F2 Sb1 F3 176.78(7) 10 . F2 Sb1 F3 89.79(8) . . F4 Sb1 F3 90.01(7) . . F2 Sb1 F3 89.79(8) 10 10 F2 Sb1 F3 176.78(7) . 10 F4 Sb1 F3 90.02(7) . 10 F3 Sb1 F3 88.12(10) . 10 F2 Sb1 F1 89.00(7) 10 . F2 Sb1 F1 89.00(7) . . F4 Sb1 F1 177.94(10) . . F3 Sb1 F1 88.50(7) . . F3 Sb1 F1 88.50(7) 10 . Cl3 Cl2 Cl3 105.55(5) 15_457 . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Sb1 F2 1.8649(16) 10 Sb1 F2 1.8649(16) . Sb1 F4 1.868(2) . Sb1 F3 1.8797(15) . Sb1 F3 1.8797(15) 10 Sb1 F1 1.899(2) . Cl2 Cl3 1.9723(8) 15_457 Cl2 Cl3 1.9723(8) .