#------------------------------------------------------------------------------ #$Date: 2019-04-30 15:49:59 +0300 (Tue, 30 Apr 2019) $ #$Revision: 214850 $ #$URL: file:///home/coder/svn-repositories/cod/cif/3/00/02/3000227.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_3000227 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 . III. Crystal structure of high-temperature Rb Cl O3 ; _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, Rb' _chemical_formula_sum 'Cl O3 Rb' _chemical_formula_weight 168.92 _chemical_name_systematic ; rubidium chlorate(V) ; _space_group_IT_number 62 _symmetry_cell_setting orthorhombic _symmetry_Int_Tables_number 62 _symmetry_space_group_name_Hall '-P 2ac 2n' _symmetry_space_group_name_H-M 'P n m a' _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 9.367(3) _cell_length_b 5.894(1) _cell_length_c 7.610(2) _cell_measurement_temperature 600(10) _cell_volume 420.14(19) _computing_cell_refinement 'Stoe DIF4' _computing_data_collection 'Stoe DIF4' _computing_data_reduction 'Stoe REDU4' _computing_molecular_graphics 'PLATON (Spek, 1990)' _computing_publication_material ; The CIF given by SHELXL was edited and finally checked with PLATON ; _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _diffrn_ambient_temperature 600(10) _diffrn_measured_fraction_theta_full 0.486 _diffrn_measured_fraction_theta_max 0.486 _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 0.1362 _diffrn_reflns_av_sigmaI/netI 0.1078 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_l_max 2 _diffrn_reflns_limit_l_min -2 _diffrn_reflns_number 211 _diffrn_reflns_theta_full 19.92 _diffrn_reflns_theta_max 19.92 _diffrn_reflns_theta_min 3.45 _diffrn_standards_decay_% 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 12.3 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.671 _exptl_crystal_F_000 312 _refine_diff_density_max 0.435 _refine_diff_density_min -0.293 _refine_diff_density_rms 0.128 _refine_ls_extinction_coef 0.022(6) _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 1.493 _refine_ls_matrix_type full _refine_ls_number_parameters 25 _refine_ls_number_reflns 108 _refine_ls_number_restraints 12 _refine_ls_restrained_S_all 1.396 _refine_ls_R_factor_all 0.0745 _refine_ls_R_factor_gt 0.0556 _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^)+(0.0200P)^2^+1.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0883 _refine_ls_wR_factor_ref 0.0978 _reflns_number_gt 81 _reflns_number_total 108 _reflns_threshold_expression >2sigma(I) _iucr_refine_instructions_details ; TITL RB CL O3 HTM 600K CELL .71073 9.367 5.894 7.610 90.00 90.00 90.00 ZERR 4 .003 .001 .002 0 0 0 REM V = 420.1 (V*3/4 = 315.1) LATT 1 SYMM .50-X,.50+Y,.50+Z SYMM X,.50-Y,Z SYMM .50-X,-Y,.50+Z SFAC RB CL O UNIT 4.0 4.0 12.0 ACTA L.S. 9 EQIV $1 X,1/2-Y,Z DFIX 1.448 0.001 CL O1 CL O2 CL O2_$1 CL O1' CL O2' CL O2'_$1 DFIX 2.32 0.001 O1 O2 O1 O2_$1 O2 O2_$1 DFIX 2.32 0.001 O1' O2' O1' O2'_$1 O2' O2'_$1 WGHT 0.020000 1.000000 EXTI 0.021585 FVAR 0.24873 0.16314 RB 1 0.173685 0.250000 0.148007 10.50000 0.12786 0.11106 = 0.10355 0.00000 -0.00433 0.00000 CL 2 0.061556 0.250000 0.661583 10.50000 0.14431 0.09860 = 0.10649 0.00000 -0.03358 0.00000 O1 3 0.189111 0.250000 0.554105 10.40000 21.00000 O2 3 0.071417 0.053196 0.774831 10.80000 21.00000 O1' 3 -0.091041 0.250000 0.691981 10.10000 21.00000 O2' 3 0.117847 0.053191 0.751965 10.20000 21.00000 HKLF 4 REM RB CL O3 HTM 600K REM R1 = 0.0556 for 81 Fo > 4sig(Fo) and 0.0745 for all 108 data REM 25 parameters refined using 12 restraints END WGHT 0.0685 1.7222 REM Highest difference peak 0.435, deepest hole -0.293, 1-sigma level 0.128 Q1 1 0.1834 0.2500 0.8515 10.50000 0.05 0.43 Q2 1 0.1388 0.1345 0.3875 11.00000 0.05 0.41 Q3 1 0.0548 0.2500 0.3825 10.50000 0.05 0.35 Q4 1 0.2431 -0.0293 0.8542 11.00000 0.05 0.23 ; _journal_article_reference '16 S' _cod_data_source_file reinrb.ci4 _cod_data_source_block wart_reinrb _cod_depositor_comments ;Releasing structure 3000227 into public domain as published material per request from Rudolf Wartchow. ; _cod_database_code 3000227 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, z+1/2' 'x, -y+1/2, z' '-x+1/2, -y, z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, -z-1/2' '-x, y-1/2, -z' '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 _atom_site_disorder_assembly _atom_site_disorder_group Rb Rb 0.1737(2) 0.2500 0.1480(6) 0.114(4) Uani 1 2 d S . . Cl Cl 0.0616(6) 0.2500 0.6616(11) 0.116(7) Uani 1 2 d SD . . O1 O 0.1891(16) 0.2500 0.554(2) 0.163(5) Uiso 0.80 2 d SPD A 1 O2 O 0.0714(11) 0.05320(9) 0.7748(10) 0.163(5) Uiso 0.80 1 d PD A 1 O1' O -0.0910(16) 0.2500 0.692(12) 0.163(5) Uiso 0.20 2 d SPD A 2 O2' O 0.118(5) 0.05319(9) 0.752(5) 0.163(5) Uiso 0.20 1 d PD A 2 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 Rb 0.128(2) 0.111(2) 0.104(12) 0.000 -0.004(3) 0.000 Cl 0.144(5) 0.099(4) 0.11(2) 0.000 -0.034(8) 0.000 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Rb Rb -0.9393 2.9676 '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_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Rb O2' 2.76(4) 2_554 Rb O2' 2.76(4) 4_554 Rb O2 2.968(8) 5_556 Rb O2 2.968(8) 7_566 Rb O1 3.094(16) . Rb O2 3.135(8) 2_554 Rb O2 3.135(8) 4_554 Rb O2 3.214(10) 1_554 Rb O2 3.214(10) 3_554 Rb O1' 3.28(3) 5_566 Rb O1' 3.28(3) 5_556 Rb O2' 3.27(3) 1_554