#------------------------------------------------------------------------------ #$Date: 2019-04-29 16:48:35 +0300 (Mon, 29 Apr 2019) $ #$Revision: 214828 $ #$URL: file:///home/coder/svn-repositories/cod/cif/3/00/02/3000228.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_3000228 loop_ _publ_author_name 'Reiner, G.' 'Wartchow, R.' _publ_contact_author ; Concerning the crystal structure : Rudolf Wartchow Institut f\"ur Anorganische Chemie Leibniz-Universit\"at Hannover Callinstr. 9 D-30167 Hannover ; _publ_section_related_literature ; Reiner, G., Wartchow, R. (2019). Ueber Kaliumchlorat, K Cl O3, Rubidiumchlorat, Rb Cl O3, und Caesiumchlorat, Cs Cl O3 . Institutionelles Repositorium der Leibniz Universitaet Hannover ; _publ_section_title ; On Potassiumchlorate, K Cl O3, Rubidiumchlorate, Rb Cl O3, and Cesiumchlorate, Cs Cl O3 . IV. Crystal structure of Cs Cl O3 at 298 K ; _journal_name_full 'Institutionelles Repositorium der Leibniz Universitaet Hannover' _journal_paper_doi 10.15488/4740 _journal_year 2019 _chemical_compound_source synthetic _chemical_formula_moiety 'Cl O3, Cs' _chemical_formula_sum 'Cl Cs O3' _chemical_formula_weight 216.36 _chemical_name_systematic ; cesium chlorate(V) ; _space_group_IT_number 160 _symmetry_cell_setting trigonal _symmetry_Int_Tables_number 160 _symmetry_space_group_name_Hall 'R 3 -2"' _symmetry_space_group_name_H-M 'R 3 m :H' _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 6.424(1) _cell_length_b 6.424(1) _cell_length_c 8.254(1) _cell_measurement_temperature 298(2) _cell_volume 294.99(7) _computing_data_collection 'Stoe two circle software' _computing_data_reduction ; Stoe two circle software and SHELX76 (Sheldrick, 1976) ; _computing_molecular_graphics 'PLATON (Spek, 1990)' _computing_publication_material ; The CIF given by SHELXL was edited and finally checked with PLATON ; _computing_structure_refinement 'SHELXL (Sheldrick, 1997)' _diffrn_ambient_temperature 298(2) _diffrn_measured_fraction_theta_max 1.0 _diffrn_measurement_device_type 'Stoe two circle diffractometer ' _diffrn_measurement_method 'background-peak-background method' _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 0.03 _diffrn_reflns_av_sigmaI/netI 0.0585 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_limit_l_min -2 _diffrn_reflns_number 1656 _diffrn_reflns_theta_full 50.36 _diffrn_reflns_theta_max 50.36 _diffrn_reflns_theta_min 4.42 _diffrn_standards_decay_% 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 9.92 _exptl_absorpt_correction_T_max 0.187 _exptl_absorpt_correction_T_min 0.073 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Numerical absorption correction with SHELX76 ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 3.654 _exptl_crystal_description 'prism || c' _exptl_crystal_F_000 288 _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.25 _refine_diff_density_max 1.610 _refine_diff_density_min -1.555 _refine_diff_density_rms 0.286 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.05(5) _refine_ls_extinction_coef 0.162(13) _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 1.172 _refine_ls_matrix_type full _refine_ls_number_parameters 13 _refine_ls_number_reflns 316 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.172 _refine_ls_R_factor_all 0.0278 _refine_ls_R_factor_gt 0.0278 _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^)+(0.0400P)^2^+0.0500P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0542 _refine_ls_wR_factor_ref 0.0542 _reflns_number_gt 316 _reflns_number_total 316 _reflns_threshold_expression >2sigma(I) _iucr_refine_instructions_details ; TITL CsClO3 hexagonal REM Start-Parameter von Rb Cl O3 rtm brunton CELL .71073 6.424 6.424 8.254 90.000 90.000 120.000 ZERR 3 .001 .001 .001 .000 .000 .000 REM Zelle Swanson et al. NBS Circular 539 vol. 8 p. 20 LATT -3 SYMM - Y, X - Y, Z SYMM Y - X, - X, Z SYMM - Y, - X, Z SYMM X, X - Y, Z SYMM Y - X, Y, Z SFAC CS Cl O UNIT 3 3 9 ACTA L.S. 3 WGHT 0.040000 0.050000 EXTI 0.161907 FVAR 1.30874 CS 1 0.000000 0.000000 10.000000 10.16667 0.02334 0.02334 = 0.03559 0.00000 0.00000 0.01167 CL 2 0.000000 0.000000 0.465197 10.16667 0.02237 0.02237 = 0.02051 0.00000 0.00000 0.01119 O 3 0.123735 -0.123735 0.397927 10.50000 0.03236 0.03236 = 0.05322 -0.00307 0.00307 0.02077 HKLF 3 REM CsClO3 hexagonal REM R1 = 0.0278 for 316 Fo > 4sig(Fo) and 0.0278 for all 316 data REM 13 parameters refined using 0 restraints END WGHT 0.0393 0.0850 REM Highest difference peak 1.610, deepest hole -1.555, 1-sigma level 0.286 ; _journal_article_reference '16 S' _cod_data_source_file csclo3.ci3 _cod_data_source_block wart_csclo3 _cod_depositor_comments ;Releasing structure 3000228 into public domain as published material per request from Rudolf Wartchow. ; _cod_original_cell_volume 295.0 _cod_original_sg_symbol_H-M 'R 3 m ' _cod_original_formula_sum 'Cl O3 Cs' _cod_database_code 3000228 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, z' 'x, x-y, z' '-x+y, y, 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' '-y+2/3, -x+1/3, z+1/3' 'x+2/3, x-y+1/3, z+1/3' '-x+y+2/3, y+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' '-y+1/3, -x+2/3, z+2/3' 'x+1/3, x-y+2/3, z+2/3' '-x+y+1/3, y+2/3, z+2/3' 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 Cs Cs 0.0000 0.0000 0.0000 0.0274(3) Uani 1 6 d S . . Cl Cl 0.0000 0.0000 0.4652(4) 0.0217(15) Uani 1 6 d S . . O O 0.1237(3) -0.1237(3) 0.3979(10) 0.0373(14) Uani 1 2 d S . . 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 Cs 0.02334(11) 0.02334(11) 0.0356(7) 0.000 0.000 0.01167(5) Cl 0.02237(19) 0.02237(19) 0.021(5) 0.000 0.000 0.01119(9) O 0.0324(8) 0.0324(8) 0.053(5) -0.0031(7) 0.0031(7) 0.0208(9) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cs Cs -0.3680 2.1192 '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' O O 0.0106 0.0060 '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 O Cl O 106.9(4) 3 2 O Cl O 106.9(4) 3 . O Cl O 106.9(4) 2 . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Cs O 3.219(6) 8_444 Cs O 3.219(6) 9_554 Cs O 3.219(6) 7_454 Cs O 3.2908(14) 15_554 Cs O 3.2908(14) 14_444 Cs O 3.2908(14) 13_554 Cs O 3.2908(14) 13_444 Cs O 3.2908(14) 14_544 Cs O 3.2908(14) 15_544 Cs O 3.561(8) 2 Cs O 3.561(8) . Cs O 3.561(8) 3 Cl O 1.485(4) 3 Cl O 1.485(4) 2 Cl O 1.485(4) . Cl Cs 3.8653(10) 7_445 Cl Cs 3.8653(10) 7 Cl Cs 3.8653(10) 7_455 Cl Cs 4.0646(14) 13 Cl Cs 4.0646(14) 13_445 Cl Cs 4.0647(14) 13_545