#------------------------------------------------------------------------------ #$Date: 2019-04-29 16:42:59 +0300 (Mon, 29 Apr 2019) $ #$Revision: 214825 $ #$URL: file:///home/coder/svn-repositories/cod/cif/3/00/02/3000225.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_3000225 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 (2019) ; _publ_section_title ; On Potassiumchlorate, K Cl O3, Rubidiumchlorate, Rb Cl O3, and Cesiumchlorat, Cs Cl O3 . I. Crystal structure of twinned K Cl O3 at 415 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) ; _space_group_IT_number 11 _symmetry_cell_setting monoclinic _symmetry_Int_Tables_number 13 _symmetry_space_group_name_Hall '-P 2yb (1/2*x,y,-1/2*x+z)' _symmetry_space_group_name_H-M 'B 1 21/m 1' _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 4.684(1) _cell_length_b 5.614(1) _cell_length_c 13.528(3) _cell_measurement_temperature 415(5) _cell_volume 355.73(13) _computing_cell_refinement 'Stoe AED2 software' _computing_data_collection 'Stoe AED2 software' _computing_data_reduction '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 415(5) _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 0.055 _diffrn_reflns_av_sigmaI/netI 0.034 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 2385 _diffrn_reflns_theta_full 31.0 _diffrn_reflns_theta_max 31.0 _diffrn_reflns_theta_min 3.0 _diffrn_standards_decay_% 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.05 _exptl_absorpt_correction_T_max 0.882 _exptl_absorpt_correction_T_min 0.588 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Numerical absorption correction with SHELX76 ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.288 _exptl_crystal_description 'plate || (001)' _exptl_crystal_F_000 240 _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.06 _refine_diff_density_max 0.277 _refine_diff_density_min -0.508 _refine_diff_density_rms 0.109 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_matrix_type full _refine_ls_number_parameters 29 _refine_ls_number_reflns 624 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.098 _refine_ls_R_factor_all 0.0342 _refine_ls_R_factor_gt 0.0329 _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^)+(0.0500P)^2^+0.0300P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0733 _refine_ls_wR_factor_ref 0.0754 _reflns_number_gt 603 _reflns_number_total 624 _reflns_threshold_expression >2sigma(I) _iucr_refine_instructions_details ; TITL K Cl O3 415 K Zwilling REM TRAF 1 0 0 0 1 0 1 0 2 REM Zelle von der Guinier-Kamera CELL 0.71073 4.684 5.614 13.528 90.00 90.00 90.00 ZERR 4 .001 .001 .003 0 0 0 LATT 6 SYMM -X, 1/2+Y, -Z SFAC K CL O UNIT 4 4 12 ACTA L.S. 5 TWIN 1 0 0 0 1 0 0 0 -1 WGHT 0.050000 0.030000 BASF 0.66150 FVAR 0.21286 K 1 -0.002893 0.250000 0.354774 10.50000 0.03859 0.04208 = 0.04565 0.00000 0.00673 0.00000 CL 2 0.033846 0.250000 0.088664 10.50000 0.03848 0.03753 = 0.03832 0.00000 -0.00169 0.00000 O1 3 0.335319 0.250000 0.057569 10.50000 0.04491 0.08674 = 0.06343 0.00000 0.02071 0.00000 O2 3 -0.005275 0.459550 0.153002 11.00000 0.06182 0.03866 = 0.07608 -0.01352 0.00262 0.00633 HKLF 4 REM K Cl O3 415 K Zwilling REM R1 = 0.0329 for 603 Fo > 4sig(Fo) and 0.0342 for all 624 data REM 29 parameters refined using 0 restraints END WGHT 0.0403 0.0775 REM Highest difference peak 0.277, deepest hole -0.508, 1-sigma level 0.109 ; _journal_article_reference '16 S' _cod_data_source_file kclo3415.ci4 _cod_data_source_block wart_kclo3415 _cod_depositor_comments ;Releasing structure 3000225 into public domain as published material per request from Rudolf Wartchow. ; _cod_original_sg_symbol_H-M 'B 21/m' _cod_database_code 3000225 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' 'x+1/2, y, z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z' '-x+1/2, -y, -z+1/2' '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 -0.00289(12) 0.2500 0.35477(4) 0.04211(17) Uani 1 2 d S . . Cl Cl 0.03385(14) 0.2500 0.08866(4) 0.03811(17) Uani 1 2 d S . . O1 O 0.3353(6) 0.2500 0.0576(2) 0.0650(7) Uani 1 2 d S . . O2 O -0.0053(4) 0.4596(3) 0.15300(10) 0.0589(4) 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 0.0386(3) 0.0421(2) 0.0456(3) 0.000 0.0067(3) 0.000 Cl 0.0385(3) 0.0375(2) 0.0383(2) 0.000 -0.0017(2) 0.000 O1 0.0449(14) 0.0867(17) 0.0634(13) 0.000 0.0207(11) 0.000 O2 0.0618(10) 0.0387(6) 0.0761(8) -0.0135(6) 0.0026(10) 0.0063(5) 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 O1 Cl O2 106.71(11) . 6_565 O1 Cl O2 106.71(11) . . O2 Cl O2 105.82(13) 6_565 . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 K O2 2.8244(18) 4_445 K O2 2.8244(17) 7_465 K O1 2.846(3) 3_455 K O2 2.8871(19) 7_565 K O2 2.8871(19) 4_545 K O2 2.9723(16) 6_565 K O2 2.9723(16) . K O1 3.1467(16) 7_565 K O1 3.1467(16) 7 K Cl 3.6040(11) . K Cl 3.6458(7) 7_565 K Cl 3.6458(7) 7 Cl O1 1.473(3) . Cl O2 1.4748(13) 6_565 Cl O2 1.4748(13) .