#------------------------------------------------------------------------------ #$Date: 2025-08-20 15:59:05 +0100 (Wed, 20 Aug 2025) $ #$Revision: 301833 $ #$URL: svn://www.crystallography.net/cod/cif/4/11/63/4116386.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_4116386 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 'As Cl3 F6' _chemical_formula_weight 295.27 _chemical_name_systematic ; Trichloroniumhexafluoroarsenate ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _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 94.42(4) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 7.045(2) _cell_length_b 11.001(3) _cell_length_c 9.299(4) _cell_measurement_reflns_used 25 _cell_measurement_temperature 130 _cell_measurement_theta_max 21 _cell_measurement_theta_min 20 _cell_volume 718.5(4) _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 0.0196 _diffrn_reflns_av_sigmaI/netI 0.0271 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 1868 _diffrn_reflns_theta_full 27.97 _diffrn_reflns_theta_max 27.97 _diffrn_reflns_theta_min 2.87 _diffrn_standards_interval_time '14400 sec' _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 5.880 _exptl_absorpt_correction_T_max 0.96 _exptl_absorpt_correction_T_min 0.91 _exptl_absorpt_correction_type psi-scan _exptl_crystal_colour orange-yellow _exptl_crystal_density_diffrn 2.729 _exptl_crystal_F_000 552 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _refine_diff_density_max 0.413 _refine_diff_density_min -0.696 _refine_diff_density_rms 0.095 _refine_ls_extinction_coef 0.0040(5) _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 1.118 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 92 _refine_ls_number_reflns 1732 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.118 _refine_ls_R_factor_all 0.0301 _refine_ls_R_factor_gt 0.0255 _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^)+(0.0247P)^2^+0.7072P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0611 _refine_ls_wR_factor_ref 0.0634 _reflns_number_gt 1546 _reflns_number_total 1732 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ja984474y_6.cif _cod_data_source_block cl3asf6 _cod_database_code 4116386 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' 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 As1 As 0.18387(4) 0.21483(2) 0.82550(3) 0.01812(10) Uani 1 1 d Cl1 Cl -0.34975(9) 0.42144(6) 0.72374(6) 0.01988(15) Uani 1 1 d Cl2 Cl -0.31478(10) 0.40780(6) 0.93641(7) 0.02283(16) Uani 1 1 d Cl3 Cl -0.14223(9) 0.52991(6) 0.66998(7) 0.02337(16) Uani 1 1 d F1 F 0.1601(3) 0.33316(18) 0.9407(2) 0.0391(5) Uani 1 1 d F2 F 0.0743(2) 0.11876(16) 0.94039(16) 0.0273(4) Uani 1 1 d F3 F -0.0316(3) 0.24545(19) 0.73616(19) 0.0332(4) Uani 1 1 d F4 F 0.2099(3) 0.09274(15) 0.71096(17) 0.0268(4) Uani 1 1 d F5 F 0.4011(2) 0.17782(17) 0.91477(19) 0.0310(4) Uani 1 1 d F6 F 0.2987(3) 0.30637(19) 0.7104(2) 0.0406(5) 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 As1 0.01709(15) 0.01681(15) 0.02056(16) -0.00083(10) 0.00218(10) -0.00023(10) Cl1 0.0173(3) 0.0243(3) 0.0177(3) 0.0013(2) -0.0006(2) -0.0018(2) Cl2 0.0237(3) 0.0274(4) 0.0173(3) -0.0002(2) 0.0014(2) -0.0002(3) Cl3 0.0196(3) 0.0251(3) 0.0257(3) 0.0009(2) 0.0035(2) -0.0033(3) F1 0.0399(11) 0.0280(10) 0.0496(12) -0.0181(9) 0.0050(9) 0.0021(9) F2 0.0318(9) 0.0326(9) 0.0174(8) 0.0028(7) 0.0014(6) -0.0088(8) F3 0.0249(9) 0.0400(10) 0.0336(9) 0.0078(8) -0.0052(7) 0.0082(8) F4 0.0338(10) 0.0268(9) 0.0198(8) -0.0062(7) 0.0017(7) 0.0021(7) F5 0.0201(8) 0.0369(10) 0.0352(9) -0.0087(8) -0.0038(7) 0.0025(8) F6 0.0414(12) 0.0373(11) 0.0443(11) 0.0104(9) 0.0118(9) -0.0126(9) 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' As As 0.0499 2.0058 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle F1 As1 F3 91.62(10) F1 As1 F6 91.01(11) F3 As1 F6 91.43(10) F1 As1 F2 90.47(10) F3 As1 F2 89.91(9) F6 As1 F2 177.97(10) F1 As1 F5 90.26(10) F3 As1 F5 177.78(9) F6 As1 F5 89.74(10) F2 As1 F5 88.88(9) F1 As1 F4 178.92(9) F3 As1 F4 89.20(9) F6 As1 F4 89.67(10) F2 As1 F4 88.82(9) F5 As1 F4 88.91(9) Cl2 Cl1 Cl3 105.09(5) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance As1 F1 1.7022(18) As1 F3 1.7070(18) As1 F6 1.7165(19) As1 F2 1.7268(17) As1 F5 1.7325(18) As1 F4 1.7327(16) Cl1 Cl2 1.9796(12) Cl1 Cl3 1.9809(10) loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 PubChem 139120499