# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_0703-1_a
_database_code_depnum_ccdc_archive 'CCDC 1946876'
loop_
_audit_author_name
_audit_author_address
'Yuanlv Mao'
;Shanghai Institute of Ceramics, Chinese Academy of Sciences
China
;
_audit_update_record             
;
2019-08-13 deposited with the CCDC.	2019-10-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'K0.36 S2 W'
_chemical_formula_weight         262.05

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_H-M_alt        'P 21/m'
_space_group_name_Hall           '-P 2yb'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'

_cell_length_a                   5.693(2)
_cell_length_b                   3.2498(11)
_cell_length_c                   9.410(3)
_cell_angle_alpha                90
_cell_angle_beta                 100.317(7)
_cell_angle_gamma                90
_cell_volume                     171.28(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    632
_cell_measurement_theta_min      7
_cell_measurement_theta_max      15

_exptl_crystal_description       plate
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    5.081
_exptl_crystal_F_000             226
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    35.079
_shelx_estimated_absorpt_T_min   0.193
_shelx_estimated_absorpt_T_max   0.419
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.140
_exptl_absorpt_correction_T_max  0.349
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            1459
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.200
_diffrn_reflns_theta_max         27.479
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measured_fraction_theta_full 0.943
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_Laue_measured_fraction_full 0.943
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_point_group_measured_fraction_full 0.943
_reflns_number_total             439
_reflns_number_gt                419
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0603P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         439
_refine_ls_number_parameters     33
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0308
_refine_ls_wR_factor_ref         0.0811
_refine_ls_wR_factor_gt          0.0807
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_restrained_S_all      1.108
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
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 ?

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
_geom_angle_publ_flag
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 ?

_refine_diff_density_max         1.295
_refine_diff_density_min         -1.587
_refine_diff_density_rms         0.491

