#------------------------------------------------------------------------------ #$Date: 2019-04-29 16:46:04 +0300 (Mon, 29 Apr 2019) $ #$Revision: 214826 $ #$URL: file:///home/coder/svn-repositories/cod/cif/3/00/02/3000226.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_3000226 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 . II. Crystal structure of high-temperature K Cl O3 at 296 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, K' _chemical_formula_sum 'Cl K O3' _chemical_formula_weight 122.55 _chemical_name_systematic ; potassium chlorate(V) (HTM) ; _space_group_IT_number 62 _symmetry_cell_setting orthorhombic _symmetry_Int_Tables_number 62 _symmetry_space_group_name_Hall '-P 2n 2ac' _symmetry_space_group_name_H-M 'P c m n' _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 4.650(1) _cell_length_b 5.582(1) _cell_length_c 13.368(2) _cell_measurement_temperature 296(2) _cell_volume 346.98(11) _computing_cell_refinement 'Stoe AED2 software' _computing_data_collection 'Stoe AED2 software' _computing_data_reduction 'Stoe AED2 software' _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 296(2) _diffrn_measured_fraction_theta_full 1.0 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Stoe four 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 0.11 _diffrn_reflns_av_sigmaI/netI 0.03 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 1687 _diffrn_reflns_theta_full 18.0 _diffrn_reflns_theta_max 18.0 _diffrn_reflns_theta_min 3.05 _diffrn_standards_decay_% 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.1 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.346 _exptl_crystal_description fragment _exptl_crystal_F_000 240 _refine_diff_density_max 0.191 _refine_diff_density_min -0.251 _refine_diff_density_rms 0.056 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.286 _refine_ls_matrix_type full _refine_ls_number_parameters 28 _refine_ls_number_reflns 138 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.286 _refine_ls_R_factor_all 0.0524 _refine_ls_R_factor_gt 0.0404 _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^)+(0.0100P)^2^+0.2000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0418 _refine_ls_wR_factor_ref 0.0440 _reflns_number_gt 112 _reflns_number_total 138 _reflns_threshold_expression >2sigma(I) _iucr_refine_instructions_details ; TITL kclo3 htm vereint REM Zelle von Guinier 296 K CELL 0.71073 4.650 5.582 13.368 90 90 90 ZERR 4 .001 .001 .002 0 0 0 REM SPGR P c m n LATT 1 SYMM 1/2+X,-Y,1/2-Z SYMM -X,1/2+Y,-Z SYMM 1/2-X,1/2-Y,1/2+Z SFAC K CL O UNIT 4 4 12 ACTA L.S. 5 WGHT 0.010000 0.200000 FVAR 0.26398 K 1 0.503004 0.250000 -0.145355 10.50000 0.02670 0.02730 = 0.02978 0.00000 0.00109 0.00000 CL 2 0.030783 0.250000 0.087870 10.50000 0.02699 0.02817 = 0.02584 0.00000 -0.00284 0.00000 O1 3 0.337708 0.250000 0.057612 10.50000 0.02886 0.06386 = 0.03669 0.00000 0.01205 0.00000 O2 3 -0.007309 0.461371 0.152022 11.00000 0.03785 0.02202 = 0.04930 -0.00981 0.00084 0.00587 HKLF 4 REM kclo3 htm verein REM R1 = 0.0404 for 112 Fo > 4sig(Fo) and 0.0524 for all 138 data REM 28 parameters refined using 0 restraints END WGHT 0.0109 0.2641 REM Highest difference peak 0.191, deepest hole -0.251, 1-sigma level 0.056 ; _journal_article_reference '16 S' _cod_data_source_file kclbc.ci3 _cod_data_source_block wart_kclbc _cod_depositor_comments ;Releasing structure 3000226 into public domain as published material per request from Rudolf Wartchow. ; _cod_original_cell_volume 347.0(1) _cod_database_code 3000226 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, -z+1/2' '-x, y+1/2, -z' '-x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y, z-1/2' 'x, -y-1/2, 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 _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group K K 0.5030(7) 0.2500 -0.14535(11) 0.0279(7) Uani 1 2 d S . . Cl Cl 0.0308(6) 0.2500 0.08787(14) 0.0270(8) Uani 1 2 d S . . O1 O 0.3377(14) 0.2500 0.0576(4) 0.043(2) Uani 1 2 d S . . O2 O -0.0073(10) 0.4614(6) 0.1520(3) 0.0364(11) 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 K 0.0267(13) 0.0273(12) 0.0298(13) 0.000 0.0011(13) 0.000 Cl 0.027(2) 0.0282(18) 0.0258(15) 0.000 -0.0028(18) 0.000 O1 0.029(5) 0.064(5) 0.037(4) 0.000 0.012(3) 0.000 O2 0.038(2) 0.022(2) 0.049(3) -0.010(2) 0.001(3) 0.006(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source K K 0.2009 0.2494 '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 O2 Cl O2 106.8(3) . 7_565 O2 Cl O1 106.0(2) . . O2 Cl O1 106.0(2) 7_565 . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 K O2 2.814(5) 3_545 K O2 2.814(5) 5_565 K O1 2.820(5) . K O2 2.847(5) 5_665 K O2 2.847(5) 3_645 K O2 2.955(4) 4_554 K O2 2.955(4) 6_655 K O1 3.117(3) 5_665 K O1 3.117(3) 5_655 K Cl 3.570(2) 6_655 K Cl 3.617(2) 5_665 K Cl 3.617(2) 5_655 Cl O2 1.469(4) . Cl O2 1.469(4) 7_565 Cl O1 1.483(7) .