# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_Na4Sn2S6_5H2O
_database_code_depnum_ccdc_archive 'CCDC 1974020'
loop_
_audit_author_name
_audit_author_address
'Hongil Jo'
;Sogang University
South Korea
;
_audit_update_record             
;
2019-12-25 deposited with the CCDC.	2020-01-21 downloaded from the CCDC.
;

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'S6 Sn2, 5(H2 O), 4(Na)'
_chemical_formula_sum            'H10 Na4 O5 S6 Sn2'
_chemical_formula_weight         611.78
_chemical_absolute_configuration unk

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'P 41 21 2'
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_Int_Tables_number      92
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y+1/2, x+1/2, z+1/4'
'y+1/2, -x+1/2, z+3/4'
'-x+1/2, y+1/2, -z+1/4'
'x+1/2, -y+1/2, -z+3/4'
'y, x, -z'
'-y, -x, -z+1/2'

_cell_length_a                   8.44260(10)
_cell_length_b                   8.44260(10)
_cell_length_c                   23.3145(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1661.80(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    9960
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      28.33
_cell_measurement_wavelength     0.71076

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       octahedron
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.464
_exptl_crystal_size_mid          0.443
_exptl_crystal_size_min          0.376
_exptl_crystal_density_diffrn    2.445
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1160

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    3.862
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        SADABS-2016/2 - Bruker AXS area detector scaling and absorption correcti
;
_exptl_absorpt_correction_T_min  0.5611
_exptl_absorpt_correction_T_max  0.7457
_shelx_estimated_absorpt_T_min   0.267
_shelx_estimated_absorpt_T_max   0.325

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'sealed x-ray tube'
_diffrn_ambient_temperature      300(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_detector                 'PHOTON II CPAD'
_diffrn_orient_matrix_type       'x-axis to radiation source'
_diffrn_orient_matrix_ub_11      -0.063614
_diffrn_orient_matrix_ub_12      -0.079974
_diffrn_orient_matrix_ub_13      0.021709
_diffrn_orient_matrix_ub_21      0.046833
_diffrn_orient_matrix_ub_22      -0.086633
_diffrn_orient_matrix_ub_23      -0.023849
_diffrn_orient_matrix_ub_31      0.088251
_diffrn_orient_matrix_ub_32      -0.011655
_diffrn_orient_matrix_ub_33      0.028273
_diffrn_measurement_device       '\three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 QEUST'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_unetI/netI     0.0089
_diffrn_reflns_number            45537
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         2.566
_diffrn_reflns_theta_max         28.329
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_reflns_Friedel_fraction_full    1
_reflns_Friedel_fraction_max     1
_reflns_Friedel_coverage         0.62
_reflns_number_total             2069
_reflns_number_gt                2066
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX3 software'
_computing_cell_refinement       'SAINT V8.38A integration software'
_computing_data_reduction        'SAINT V8.38A integration software'
_computing_structure_solution    'SHELXS 2013/2 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_shelx_SHELXL_version_number     2018/3
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0039P)²+1.1066P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_coef       0.0157(3)
_refine_ls_number_reflns         2069
_refine_ls_number_parameters     100
_refine_ls_number_restraints     8
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.0113
_refine_ls_R_factor_gt           0.0113
_refine_ls_wR_factor_ref         0.0279
_refine_ls_wR_factor_gt          0.0279
_refine_ls_goodness_of_fit_ref   1.351
_refine_ls_restrained_S_all      1.356
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_abs_structure_details 
;
 Flack x determined using 782 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.02(10)
_refine_diff_density_max         0.463
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.073

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
Sn1 Sn 0.47033(2) 0.48055(2) 0.32083(2) 0.01618(6) Uani 1 1 d . . . . .
Na1 Na 0.86294(18) 0.4831(2) 0.45336(6) 0.0411(4) Uani 1 1 d . . . . .
Na2 Na 1.18906(16) 0.49453(18) 0.54215(6) 0.0345(3) Uani 1 1 d . . . . .
S1 S 0.62450(8) 0.63193(8) 0.38440(3) 0.02146(13) Uani 1 1 d . . . . .
S2 S 0.64372(7) 0.35628(7) 0.25 0.01913(18) Uani 1 2 d S T P . .
S3 S 0.29524(9) 0.29583(9) 0.36008(3) 0.02284(13) Uani 1 1 d . . . . .
S4 S 0.34461(7) 0.65539(7) 0.25 0.02024(18) Uani 1 2 d S T P . .
O1 O 1.1272(3) 0.5474(3) 0.44450(10) 0.0339(5) Uani 1 1 d D . . . .
H1A H 1.133(5) 0.642(3) 0.4273(15) 0.038(11) Uiso 1 1 d D . . . .
H1B H 1.177(5) 0.482(5) 0.4187(17) 0.066(15) Uiso 1 1 d D . . . .
O2 O 0.9095(3) 0.4403(3) 0.55118(11) 0.0350(6) Uani 1 1 d D . . . .
H2A H 0.895(7) 0.340(4) 0.567(2) 0.09(2) Uiso 1 1 d D . . . .
H2B H 0.833(5) 0.500(5) 0.5696(18) 0.064(15) Uiso 1 1 d D . . . .
O3 O 1.4652(3) 0.4652(3) 0.5 0.0495(9) Uani 1 2 d DS T P . .
H3 H 1.530(5) 0.500(5) 0.5303(10) 0.072(15) Uiso 1 1 d D . . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
Sn1 S3 2.3355(6) . ?
Sn1 S1 2.3504(6) . ?
Sn1 S2 2.4435(6) . ?
Sn1 S4 2.4560(6) . ?
Na1 O1 2.306(3) . ?
Na1 O2 2.342(3) . ?
Na1 S3 2.8392(17) 6 ?
Na1 S1 2.8663(16) . ?
Na1 S4 3.2434(17) 3_655 ?
Na1 Na2 3.4461(19) . ?
Na1 Na2 3.981(2) 7_546 ?
Na1 Na2 4.180(2) 4_564 ?
Na2 O1 2.378(3) . ?
Na2 O2 2.414(3) . ?
Na2 O3 2.542(2) . ?
Na2 S3 2.9731(15) 7_656 ?
Na2 S3 2.9949(16) 3_655 ?
Na2 S2 3.1439(16) 3_645 ?
Na2 Na2 4.143(3) 7_646 ?
O1 H1A 0.89(2) . ?
O1 H1B 0.92(2) . ?
O2 H2A 0.93(2) . ?
O2 H2B 0.93(2) . ?
O3 H3 0.94(2) . ?
O3 H3 0.94(2) 7_646 ?

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
S3 Sn1 S1 117.81(2) . . ?
S3 Sn1 S2 110.93(2) . . ?
S1 Sn1 S2 109.137(19) . . ?
S3 Sn1 S4 113.03(2) . . ?
S1 Sn1 S4 109.66(2) . . ?
S2 Sn1 S4 93.591(19) . . ?
O1 Na1 O2 87.78(10) . . ?
O1 Na1 S3 110.08(9) . 6 ?
O2 Na1 S3 114.38(10) . 6 ?
O1 Na1 S1 121.76(8) . . ?
O2 Na1 S1 137.03(9) . . ?
S3 Na1 S1 85.98(4) 6 . ?
O1 Na1 S4 81.65(8) . 3_655 ?
O2 Na1 S4 80.04(8) . 3_655 ?
S3 Na1 S4 161.00(6) 6 3_655 ?
S1 Na1 S4 75.06(4) . 3_655 ?
O1 Na1 Na2 43.45(7) . . ?
O2 Na1 Na2 44.39(8) . . ?
S3 Na1 Na2 119.80(6) 6 . ?
S1 Na1 Na2 152.36(7) . . ?
S4 Na1 Na2 79.07(4) 3_655 . ?
O1 Na1 Na2 154.85(9) . 7_546 ?
O2 Na1 Na2 90.52(9) . 7_546 ?
S3 Na1 Na2 48.63(4) 6 7_546 ?
S1 Na1 Na2 74.89(4) . 7_546 ?
S4 Na1 Na2 122.73(5) 3_655 7_546 ?
Na2 Na1 Na2 128.75(5) . 7_546 ?
O1 Na1 Na2 75.17(8) . 4_564 ?
O2 Na1 Na2 141.00(8) . 4_564 ?
S3 Na1 Na2 45.30(3) 6 4_564 ?
S1 Na1 Na2 80.48(4) . 4_564 ?
S4 Na1 Na2 129.89(5) 3_655 4_564 ?
Na2 Na1 Na2 109.72(4) . 4_564 ?
Na2 Na1 Na2 90.82(4) 7_546 4_564 ?
O1 Na2 O2 84.51(10) . . ?
O1 Na2 O3 81.34(8) . . ?
O2 Na2 O3 155.80(11) . . ?
O1 Na2 S3 155.06(10) . 7_656 ?
O2 Na2 S3 97.02(7) . 7_656 ?
O3 Na2 S3 87.90(5) . 7_656 ?
O1 Na2 S3 110.88(9) . 3_655 ?
O2 Na2 S3 99.00(8) . 3_655 ?
O3 Na2 S3 104.35(8) . 3_655 ?
S3 Na2 S3 93.52(4) 7_656 3_655 ?
O1 Na2 S2 81.42(8) . 3_645 ?
O2 Na2 S2 74.30(7) . 3_645 ?
O3 Na2 S2 84.21(8) . 3_645 ?
S3 Na2 S2 75.13(4) 7_656 3_645 ?
S3 Na2 S2 165.71(5) 3_655 3_645 ?
O1 Na2 Na1 41.82(8) . . ?
O2 Na2 Na1 42.75(7) . . ?
O3 Na2 Na1 119.86(6) . . ?
S3 Na2 Na1 133.39(5) 7_656 . ?
S3 Na2 Na1 112.04(5) 3_655 . ?
S2 Na2 Na1 71.86(4) 3_645 . ?
O1 Na2 Na1 90.88(8) . 7_656 ?
O2 Na2 Na1 139.10(8) . 7_656 ?
O3 Na2 Na1 60.94(7) . 7_656 ?
S3 Na2 Na1 103.47(4) 7_656 7_656 ?
S3 Na2 Na1 45.35(3) 3_655 7_656 ?
S2 Na2 Na1 145.10(5) 3_645 7_656 ?
Na1 Na2 Na1 122.40(4) . 7_656 ?
O1 Na2 Na2 78.42(8) . 7_646 ?
O2 Na2 Na2 122.14(7) . 7_646 ?
O3 Na2 Na2 35.43(7) . 7_646 ?
S3 Na2 Na2 79.79(5) 7_656 7_646 ?
S3 Na2 Na2 138.76(3) 3_655 7_646 ?
S2 Na2 Na2 48.78(3) 3_645 7_646 ?
Na1 Na2 Na2 101.24(5) . 7_646 ?
Na1 Na2 Na2 96.35(3) 7_656 7_646 ?
O1 Na2 Na1 146.55(9) . 3_645 ?
O2 Na2 Na1 62.04(7) . 3_645 ?
O3 Na2 Na1 129.84(5) . 3_645 ?
S3 Na2 Na1 42.75(3) 7_656 3_645 ?
S3 Na2 Na1 76.39(4) 3_655 3_645 ?
S2 Na2 Na1 89.33(4) 3_645 3_645 ?
Na1 Na2 Na1 104.76(4) . 3_645 ?
Na1 Na2 Na1 113.64(4) 7_656 3_645 ?
Na2 Na2 Na1 118.53(5) 7_646 3_645 ?
Sn1 S1 Na1 120.29(4) . . ?
Sn1 S2 Sn1 86.68(3) 8_665 . ?
Sn1 S2 Na2 133.53(2) 8_665 4_564 ?
Sn1 S2 Na2 113.92(2) . 4_564 ?
Sn1 S2 Na2 113.92(2) 8_665 6_455 ?
Sn1 S2 Na2 133.53(2) . 6_455 ?
Na2 S2 Na2 82.43(5) 4_564 6_455 ?
Sn1 S3 Na1 102.85(4) . 6_455 ?
Sn1 S3 Na2 98.32(4) . 7_546 ?
Na1 S3 Na2 91.95(5) 6_455 7_546 ?
Sn1 S3 Na2 107.51(4) . 4_464 ?
Na1 S3 Na2 86.02(5) 6_455 4_464 ?
Na2 S3 Na2 153.90(4) 7_546 4_464 ?
Sn1 S4 Sn1 86.13(3) 8_665 . ?
Sn1 S4 Na1 127.11(3) 8_665 6_465 ?
Sn1 S4 Na1 108.63(3) . 6_465 ?
Sn1 S4 Na1 108.63(3) 8_665 4_464 ?
Sn1 S4 Na1 127.11(3) . 4_464 ?
Na1 S4 Na1 101.66(6) 6_465 4_464 ?
Na1 O1 Na2 94.73(10) . . ?
Na1 O1 H1A 108(3) . . ?
Na2 O1 H1A 126(3) . . ?
Na1 O1 H1B 111(3) . . ?
Na2 O1 H1B 114(3) . . ?
H1A O1 H1B 103(3) . . ?
Na1 O2 Na2 92.85(10) . . ?
Na1 O2 H2A 120(3) . . ?
Na2 O2 H2A 110(4) . . ?
Na1 O2 H2B 105(3) . . ?
Na2 O2 H2B 128(3) . . ?
H2A O2 H2B 103(3) . . ?
Na2 O3 Na2 109.14(15) 7_646 . ?
Na2 O3 H3 121(3) 7_646 . ?
Na2 O3 H3 102(3) . . ?
Na2 O3 H3 102(3) 7_646 7_646 ?
Na2 O3 H3 121(3) . 7_646 ?
H3 O3 H3 101(4) . 7_646 ?


# END of CIF
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Water/Methanol'
