#------------------------------------------------------------------------------ #$Date: 2019-10-11 06:18:05 +0300 (Fri, 11 Oct 2019) $ #$Revision: 219269 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/23/45/7234537.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_7234537 loop_ _publ_author_name 'Mao, Yuanlv' 'Xie, Miao' 'Zhao, Wei' 'Yuan, Kaidi' 'Fang, Yuqiang' 'Huang, Fuqiang' _publ_section_title ; K0.36(H2O)yWS2: a new layered compound for reversible hydrated potassium ion intercalation in aqueous electrolyte ; _journal_issue 55 _journal_name_full 'RSC Advances' _journal_page_first 32323 _journal_paper_doi 10.1039/C9RA07718A _journal_volume 9 _journal_year 2019 _chemical_formula_sum 'K0.36 S2 W' _chemical_formula_weight 262.05 _space_group_crystal_system monoclinic _space_group_IT_number 11 _space_group_name_Hall '-P 2yb' _space_group_name_H-M_alt 'P 1 21/m 1' _symmetry_space_group_name_Hall '-P 2yb' _symmetry_space_group_name_H-M 'P 1 21/m 1' _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2019-08-13 deposited with the CCDC. 2019-10-03 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 100.317(7) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 5.693(2) _cell_length_b 3.2498(11) _cell_length_c 9.410(3) _cell_measurement_reflns_used 632 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 15 _cell_measurement_theta_min 7 _cell_volume 171.28(10) _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 298(2) _diffrn_measured_fraction_theta_full 0.943 _diffrn_measured_fraction_theta_max 0.944 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0327 _diffrn_reflns_av_unetI/netI 0.0311 _diffrn_reflns_Laue_measured_fraction_full 0.943 _diffrn_reflns_Laue_measured_fraction_max 0.944 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 1459 _diffrn_reflns_point_group_measured_fraction_full 0.943 _diffrn_reflns_point_group_measured_fraction_max 0.944 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.479 _diffrn_reflns_theta_min 2.200 _exptl_absorpt_coefficient_mu 35.079 _exptl_absorpt_correction_T_max 0.349 _exptl_absorpt_correction_T_min 0.140 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour black _exptl_crystal_density_diffrn 5.081 _exptl_crystal_description plate _exptl_crystal_F_000 226 _exptl_crystal_size_max 0.070 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_min 0.030 _refine_diff_density_max 1.295 _refine_diff_density_min -1.587 _refine_diff_density_rms 0.491 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.118 _refine_ls_hydrogen_treatment undef _refine_ls_matrix_type full _refine_ls_number_parameters 33 _refine_ls_number_reflns 439 _refine_ls_number_restraints 7 _refine_ls_restrained_S_all 1.108 _refine_ls_R_factor_all 0.0317 _refine_ls_R_factor_gt 0.0308 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0603P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0807 _refine_ls_wR_factor_ref 0.0811 _reflns_Friedel_coverage 0.000 _reflns_number_gt 419 _reflns_number_total 439 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9ra07718a2.cif _cod_data_source_block 0703-1_a _cod_database_code 7234537 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.193 _shelx_estimated_absorpt_t_max 0.419 _shelx_res_file ; 0703-1_a.res created by SHELXL-2014/7 TITL 0703-1_a.res in P2(1)/m REM Old TITL 0703-1 in P2(1) REM SHELXT solution in P2(1)/m REM R1 0.063, Rweak 0.011, Alpha 0.017, Orientation as input REM Formula found by SHELXT: S2 W CELL 0.71073 5.6928 3.2498 9.4105 90.000 100.317 90.000 ZERR 2.000 0.0020 0.0011 0.0033 0.000 0.007 0.000 LATT 1 SYMM -X, 1/2+Y, -Z SFAC K S W UNIT 0.7203 4 2 size 0.07 0.05 0.03 TEMP 0 L.S. 10 BOND LIST 4 ACTA sump 0.36 0.001 1.0 2 1.0 3 simu 0.001 K1 K2 delu 0.001 K1 K2 FMAP 2 PLAN 20 WGHT 0.060300 FVAR 0.63534 0.17713 0.18301 W 3 0.302017 0.750000 0.493713 10.50000 0.02004 0.02623 = 0.03140 0.00000 0.00458 0.00000 S1 2 0.643544 0.750000 0.685509 10.50000 0.02458 0.02458 = 0.03435 0.00000 0.00439 0.00000 S2 2 0.125262 0.250000 0.641246 10.50000 0.02296 0.02436 = 0.03290 0.00000 0.00556 0.00000 PART 1 K1 1 0.316138 0.750000 0.958254 20.50000 0.11507 0.22488 = 0.04603 0.00000 0.00957 0.00000 PART 2 K2 1 0.148000 0.750000 0.963548 30.50000 0.11507 0.22488 = 0.04605 0.00000 0.00949 0.00000 part 0 HKLF 4 REM 0703-1_a.res in P2(1)/m REM R1 = 0.0308 for 419 Fo > 4sig(Fo) and 0.0317 for all 439 data REM 33 parameters refined using 7 restraints END WGHT 0.0626 0.0000 REM Highest difference peak 1.295, deepest hole -1.587, 1-sigma level 0.491 Q1 1 0.3669 0.7500 1.0062 10.50000 0.05 1.30 Q2 1 0.4612 0.9632 0.9791 11.00000 0.05 1.19 Q3 1 0.2777 0.7500 0.5733 10.50000 0.05 1.18 Q4 1 0.2236 0.7500 0.9668 10.50000 0.05 1.15 Q5 1 0.0102 0.7500 0.9974 10.50000 0.05 1.15 Q6 1 0.0337 1.0443 0.9742 11.00000 0.05 1.13 Q7 1 0.2516 0.9587 0.4555 11.00000 0.05 1.09 Q8 1 0.3350 0.7500 0.4175 10.50000 0.05 1.08 Q9 1 0.3764 0.8613 0.5539 11.00000 0.05 1.04 Q10 1 0.1857 0.7500 0.3046 10.50000 0.05 0.90 Q11 1 0.1514 0.2500 0.8811 10.50000 0.05 0.74 Q12 1 0.2786 0.2500 0.8831 10.50000 0.05 0.70 Q13 1 0.3024 1.1909 0.9958 11.00000 0.05 0.69 Q14 1 0.3857 0.7500 0.6772 10.50000 0.05 0.68 Q15 1 0.0694 0.7500 1.0895 10.50000 0.05 0.67 Q16 1 0.5298 0.7500 0.8872 10.50000 0.05 0.66 Q17 1 0.1251 0.7500 0.8458 10.50000 0.05 0.66 Q18 1 0.1644 0.2500 0.7615 10.50000 0.05 0.65 Q19 1 0.2578 0.7500 0.8025 10.50000 0.05 0.62 Q20 1 0.8242 0.7500 0.7477 10.50000 0.05 0.59 ; _shelx_res_checksum 25049 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group W W 0.30202(6) 0.7500 0.49371(4) 0.0259(2) Uani 1 2 d S T P A . S1 S 0.6435(5) 0.7500 0.6855(3) 0.0279(6) Uani 1 2 d S T P . . S2 S 0.1253(5) 0.2500 0.6412(3) 0.0267(5) Uani 1 2 d S T P . . K1 K 0.316(10) 0.7500 0.958(4) 0.129(9) Uani 0.177(14) 2 d S TU P A 1 K2 K 0.148(10) 0.7500 0.964(4) 0.129(9) Uani 0.183(14) 2 d S TU P 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 W 0.0200(3) 0.0262(3) 0.0314(3) 0.000 0.0046(2) 0.000 S1 0.0246(13) 0.0246(12) 0.0343(13) 0.000 0.0044(11) 0.000 S2 0.0230(12) 0.0244(12) 0.0329(13) 0.000 0.0056(10) 0.000 K1 0.115(18) 0.22(2) 0.046(7) 0.000 0.010(16) 0.000 K2 0.115(18) 0.22(2) 0.046(7) 0.000 0.009(16) 0.000 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 '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 S1 W S1 85.15(11) 3_666 3_676 S1 W S1 109.78(8) 3_666 . S1 W S1 109.78(8) 3_676 . S1 W S2 163.37(11) 3_666 1_565 S1 W S2 93.82(7) 3_676 1_565 S1 W S2 86.22(10) . 1_565 S1 W S2 93.82(7) 3_666 . S1 W S2 163.37(11) 3_676 . S1 W S2 86.22(10) . . S2 W S2 82.44(10) 1_565 . S1 W S2 83.17(10) 3_666 3_566 S1 W S2 83.17(9) 3_676 3_566 S1 W S2 161.93(12) . 3_566 S2 W S2 80.23(9) 1_565 3_566 S2 W S2 80.23(9) . 3_566 S1 W W 102.77(7) 3_666 3_676 S1 W W 54.94(7) 3_676 3_676 S1 W W 54.85(6) . 3_676 S2 W W 90.02(6) 1_565 3_676 S2 W W 140.82(7) . 3_676 S2 W W 136.35(4) 3_566 3_676 S1 W W 54.94(7) 3_666 3_666 S1 W W 102.77(7) 3_676 3_666 S1 W W 54.85(6) . 3_666 S2 W W 140.82(7) 1_565 3_666 S2 W W 90.02(6) . 3_666 S2 W W 136.35(4) 3_566 3_666 W W W 72.01(3) 3_676 3_666 W S1 W 85.15(11) 3_666 3_676 W S1 W 70.22(8) 3_666 . W S1 W 70.22(8) 3_676 . W S1 K1 132.9(3) 3_666 . W S1 K1 132.9(3) 3_676 . W S1 K1 95.0(7) . . W S1 K2 109.3(6) 3_666 1_655 W S1 K2 109.3(6) 3_676 1_655 W S1 K2 179.4(8) . 1_655 W S1 K2 150.1(7) 3_666 3_677 W S1 K2 105.7(4) 3_676 3_677 W S1 K2 139.5(8) . 3_677 K2 S1 K2 40.9(13) 1_655 3_677 W S1 K2 105.7(4) 3_666 3_667 W S1 K2 150.1(7) 3_676 3_667 W S1 K2 139.5(8) . 3_667 K2 S1 K2 40.9(13) 1_655 3_667 K2 S1 K2 52.4(5) 3_677 3_667 W S1 K1 160.0(4) 3_666 3_677 W S1 K1 110.2(4) 3_676 3_677 W S1 K1 126.3(8) . 3_677 K1 S1 K1 43.6(13) . 3_677 W S1 K1 110.2(4) 3_666 3_667 W S1 K1 160.0(4) 3_676 3_667 W S1 K1 126.3(8) . 3_667 K1 S1 K1 43.6(13) . 3_667 K1 S1 K1 52.2(6) 3_677 3_667 W S2 W 82.44(10) 1_545 . W S2 W 99.77(9) 1_545 3_566 W S2 W 99.77(9) . 3_566 W S2 K1 94.6(7) 1_545 1_545 W S2 K1 135.3(9) . 1_545 W S2 K1 124.5(9) 3_566 1_545 W S2 K1 135.3(9) 1_545 . W S2 K1 94.6(7) . . W S2 K1 124.5(9) 3_566 . K1 S2 K1 57.1(6) 1_545 . W S2 K2 103.4(5) 1_545 1_545 W S2 K2 149.0(8) . 1_545 W S2 K2 108.9(10) 3_566 1_545 W S2 K2 149.0(8) 1_545 . W S2 K2 103.4(5) . . W S2 K2 108.9(9) 3_566 . K2 S2 K2 56.7(6) 1_545 . K1 K1 K1 75(3) 3_677 3_667 K1 K1 K1 52.3(14) 3_677 1_565 K1 K1 K1 127.7(13) 3_667 1_565 K1 K1 K1 127.7(13) 3_677 1_545 K1 K1 K1 52.3(14) 3_667 1_545 K1 K1 K1 180.0 1_565 1_545 K1 K1 S2 132(3) 3_677 . K1 K1 S2 94.5(14) 3_667 . K1 K1 S2 118.5(3) 1_565 . K1 K1 S2 61.4(3) 1_545 . K1 K1 S2 94.5(14) 3_677 1_565 K1 K1 S2 132(3) 3_667 1_565 K1 K1 S2 61.5(3) 1_565 1_565 K1 K1 S2 118.5(3) 1_545 1_565 S2 K1 S2 57.1(6) . 1_565 K1 K1 S1 74(2) 3_677 . K1 K1 S1 74(2) 3_667 . K1 K1 S1 90.000(6) 1_565 . K1 K1 S1 90.000(3) 1_545 . S2 K1 S1 58.3(7) . . S2 K1 S1 58.3(7) 1_565 . K1 K1 S1 62.9(15) 3_677 3_677 K1 K1 S1 94.8(17) 3_667 3_677 K1 K1 S1 63.9(3) 1_565 3_677 K1 K1 S1 116.1(3) 1_545 3_677 S2 K1 S1 164.6(19) . 3_677 S2 K1 S1 123.0(5) 1_565 3_677 S1 K1 S1 136.4(13) . 3_677 K1 K1 S1 94.8(17) 3_677 3_667 K1 K1 S1 62.9(15) 3_667 3_667 K1 K1 S1 116.1(3) 1_565 3_667 K1 K1 S1 63.9(3) 1_545 3_667 S2 K1 S1 123.0(5) . 3_667 S2 K1 S1 164.6(19) 1_565 3_667 S1 K1 S1 136.4(13) . 3_667 S1 K1 S1 52.2(6) 3_677 3_667 K1 K1 K1 148(3) 3_677 3_567 K1 K1 K1 111.6(15) 3_667 3_567 K1 K1 K1 113.0(6) 1_565 3_567 K1 K1 K1 67.0(7) 1_545 3_567 S2 K1 K1 80.1(10) . 3_567 S2 K1 K1 101.6(15) 1_565 3_567 S1 K1 K1 138.4(13) . 3_567 S1 K1 K1 85.2(15) 3_677 3_567 S1 K1 K1 64.6(10) 3_667 3_567 K1 K1 K1 111.6(15) 3_677 3_577 K1 K1 K1 148(3) 3_667 3_577 K1 K1 K1 67.0(6) 1_565 3_577 K1 K1 K1 113.0(6) 1_545 3_577 S2 K1 K1 101.6(15) . 3_577 S2 K1 K1 80.1(10) 1_565 3_577 S1 K1 K1 138.4(13) . 3_577 S1 K1 K1 64.6(10) 3_677 3_577 S1 K1 K1 85.2(15) 3_667 3_577 K1 K1 K1 46.1(13) 3_567 3_577 K2 K2 K2 80(3) 3_567 3_577 K2 K2 K2 130.1(16) 3_567 1_565 K2 K2 K2 49.9(16) 3_577 1_565 K2 K2 K2 49.9(16) 3_567 1_545 K2 K2 K2 130.1(16) 3_577 1_545 K2 K2 K2 179.999(19) 1_565 1_545 K2 K2 S2 90.8(13) 3_567 . K2 K2 S2 129(3) 3_577 . K2 K2 S2 118.3(3) 1_565 . K2 K2 S2 61.7(3) 1_545 . K2 K2 S2 129(3) 3_567 1_565 K2 K2 S2 90.8(13) 3_577 1_565 K2 K2 S2 61.7(3) 1_565 1_565 K2 K2 S2 118.3(3) 1_545 1_565 S2 K2 S2 56.7(6) . 1_565 K2 K2 S1 73(2) 3_567 1_455 K2 K2 S1 73(2) 3_577 1_455 K2 K2 S1 90.000(6) 1_565 1_455 K2 K2 S1 90.000(8) 1_545 1_455 S2 K2 S1 56.3(6) . 1_455 S2 K2 S1 56.3(6) 1_565 1_455 K2 K2 S1 99.4(18) 3_567 3_677 K2 K2 S1 66.1(14) 3_577 3_677 K2 K2 S1 63.8(2) 1_565 3_677 K2 K2 S1 116.2(2) 1_545 3_677 S2 K2 S1 163.6(18) . 3_677 S2 K2 S1 122.7(5) 1_565 3_677 S1 K2 S1 139.1(13) 1_455 3_677 K2 K2 S1 66.1(14) 3_567 3_667 K2 K2 S1 99.4(18) 3_577 3_667 K2 K2 S1 116.2(2) 1_565 3_667 K2 K2 S1 63.8(2) 1_545 3_667 S2 K2 S1 122.7(5) . 3_667 S2 K2 S1 163.6(18) 1_565 3_667 S1 K2 S1 139.1(13) 1_455 3_667 S1 K2 S1 52.4(5) 3_677 3_667 K2 K2 K2 149(3) 3_567 3_677 K2 K2 K2 111.4(14) 3_577 3_677 K2 K2 K2 67.6(6) 1_565 3_677 K2 K2 K2 112.4(6) 1_545 3_677 S2 K2 K2 102.0(16) . 3_677 S2 K2 K2 81.2(11) 1_565 3_677 S1 K2 K2 137.5(13) 1_455 3_677 S1 K2 K2 62.9(8) 3_677 3_677 S1 K2 K2 83.2(12) 3_667 3_677 K2 K2 K2 111.4(14) 3_567 3_667 K2 K2 K2 149(3) 3_577 3_667 K2 K2 K2 112.4(6) 1_565 3_667 K2 K2 K2 67.6(6) 1_545 3_667 S2 K2 K2 81.2(11) . 3_667 S2 K2 K2 102.0(16) 1_565 3_667 S1 K2 K2 137.5(13) 1_455 3_667 S1 K2 K2 83.2(12) 3_677 3_667 S1 K2 K2 62.9(8) 3_667 3_667 K2 K2 K2 44.8(12) 3_677 3_667 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 W S1 2.402(2) 3_666 W S1 2.402(2) 3_676 W S1 2.404(3) . W S2 2.466(2) 1_565 W S2 2.466(2) . W S2 2.534(3) 3_566 W W 2.7641(9) 3_676 W W 2.7641(9) 3_666 S1 W 2.402(2) 3_666 S1 W 2.402(2) 3_676 S1 K1 3.43(5) . S1 K2 3.52(5) 1_655 S1 K2 3.68(3) 3_677 S1 K2 3.68(3) 3_667 S1 K1 3.70(4) 3_677 S1 K1 3.70(4) 3_667 S2 W 2.466(2) 1_545 S2 W 2.534(3) 3_566 S2 K1 3.40(3) 1_545 S2 K1 3.40(3) . S2 K2 3.42(3) 1_545 S2 K2 3.42(3) . K1 K1 2.66(8) 3_677 K1 K1 2.66(8) 3_667 K1 K1 3.2498(12) 1_565 K1 K1 3.2498(11) 1_545 K1 S2 3.40(3) 1_565 K1 S1 3.70(4) 3_677 K1 S1 3.70(4) 3_667 K1 K1 4.15(11) 3_567 K1 K1 4.15(11) 3_577 K2 K2 2.52(8) 3_567 K2 K2 2.52(8) 3_577 K2 K2 3.2498(12) 1_565 K2 K2 3.2498(12) 1_545 K2 S2 3.42(3) 1_565 K2 S1 3.52(5) 1_455 K2 S1 3.68(3) 3_677 K2 S1 3.68(3) 3_667 K2 K2 4.26(11) 3_677 K2 K2 4.26(11) 3_667