# Supplementary Information (SI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_mo_zjz20210406002_0m
_database_code_depnum_ccdc_archive 'CCDC 2369466'
loop_
_audit_author_name
_audit_author_address
'Wang Zhao'
;Xinjiang Technical Institute of Physics and Chemistry, Chinese Academy of Sciences
China
;
_audit_update_record             
;
2024-07-10 deposited with the CCDC.	2024-10-08 downloaded from the CCDC.
;
_audit_creation_date             2024-06-24
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Ba3 I10 Pb6 S8 Si2'
_chemical_formula_sum            'Ba3 I10 Pb6 S8 Si2'
_chemical_formula_weight         3236.76
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 '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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c'
_space_group_name_Hall           '-R 3 2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   9.7925(2)
_cell_length_b                   9.7925(2)
_cell_length_c                   70.628(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     5865.4(3)
_cell_formula_units_Z            6.00012
_cell_measurement_reflns_used    4806
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      28.151
_cell_measurement_theta_min      2.470
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    37.085
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.5625
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1002 before and 0.0642 after correction. The Ratio of minimum to maximum transmission is 0.7540. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    5.498
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             8076
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       98
_diffrn_reflns_limit_l_min       -89
_diffrn_reflns_number            8103
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.034
_diffrn_reflns_theta_min         2.470
_diffrn_ambient_temperature      273.15
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 6000 area detector'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1507
_reflns_number_total             1870
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_refine_diff_density_max         2.111
_refine_diff_density_min         -2.194
_refine_diff_density_rms         0.326
_refine_ls_extinction_coef       0.000019(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     47
_refine_ls_number_reflns         1870
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0434
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0285P)²+247.8492P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0869
_refine_ls_wR_factor_ref         0.0911
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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
I2 I 0.000000 0.000000 0.500000 0.0191(3) Uani 1 6 d S T P . .
I1 I 0.32670(8) 0.41122(9) 0.47493(2) 0.0338(2) Uani 1 1 d . . . . .
Ba1 Ba 0.333333 0.32210(10) 0.416667 0.0458(3) Uani 1 2 d S T P A .
S1 S 0.666667 0.333333 0.47794(5) 0.0164(7) Uani 1 3 d S T P . .
S2 S 0.4603(3) 0.1297(3) 0.43819(3) 0.0203(5) Uani 1 1 d . . . . .
Si1 Si 0.666667 0.333333 0.44747(6) 0.0158(8) Uani 1 3 d S T P B .
I4 I 0.000000 0.000000 0.44368(2) 0.0379(3) Uani 1 3 d S T P A 2
Pb1 Pb 0.34477(6) 0.07913(6) 0.47562(2) 0.04302(17) Uani 1 1 d . . . B 6
I3 I 0.333333 0.666667 0.416667 0.0780(10) Uani 1 6 d S T P A .

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
I2 0.0187(4) 0.0187(4) 0.0199(6) 0.000 0.000 0.0093(2)
I1 0.0228(4) 0.0248(4) 0.0533(5) 0.0052(3) 0.0090(3) 0.0114(3)
Ba1 0.0403(6) 0.0271(4) 0.0743(8) -0.0191(3) -0.0381(6) 0.0202(3)
S1 0.0185(11) 0.0185(11) 0.0124(15) 0.000 0.000 0.0092(5)
S2 0.0188(11) 0.0187(11) 0.0228(11) -0.0041(8) -0.0032(8) 0.0090(9)
Si1 0.0151(12) 0.0151(12) 0.0171(19) 0.000 0.000 0.0076(6)
I4 0.0453(5) 0.0453(5) 0.0233(6) 0.000 0.000 0.0226(2)
Pb1 0.0436(3) 0.0369(3) 0.0366(3) 0.00146(19) 0.0131(2) 0.0111(2)
I3 0.0225(6) 0.0225(6) 0.189(3) 0.000 0.000 0.0112(3)

_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
I2 Pb1 3.5138(5) . ?
I1 Pb1 3.3443(9) . ?
Ba1 S2 3.122(2) . ?
Ba1 S2 3.122(3) 12 ?
Ba1 S2 3.266(2) 11_455 ?
Ba1 S2 3.266(2) 3_665 ?
Ba1 I4 3.7345(7) 10 ?
Ba1 I4 3.7346(7) . ?
Ba1 I3 3.3742(10) . ?
S1 Si1 2.152(5) . ?
S1 Pb1 2.8832(6) 2_655 ?
S1 Pb1 2.8832(6) . ?
S1 Pb1 2.8832(6) 3_665 ?
S2 Si1 2.112(3) . ?
S2 Pb1 2.821(2) . ?

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
S2 Ba1 S2 73.24(9) 12 . ?
S2 Ba1 S2 65.92(8) . 3_665 ?
S2 Ba1 S2 130.29(3) 12 3_665 ?
S2 Ba1 S2 130.29(3) . 11_455 ?
S2 Ba1 S2 65.92(8) 12 11_455 ?
S2 Ba1 S2 162.89(9) 3_665 11_455 ?
S2 Ba1 I4 118.91(4) 3_665 . ?
S2 Ba1 I4 68.76(4) 3_665 10 ?
S2 Ba1 I4 71.65(5) . . ?
S2 Ba1 I4 70.16(5) . 10 ?
S2 Ba1 I4 68.76(4) 11_455 . ?
S2 Ba1 I4 71.66(5) 12 10 ?
S2 Ba1 I4 118.91(4) 11_455 10 ?
S2 Ba1 I4 70.15(5) 12 . ?
S2 Ba1 I3 81.45(4) 11_455 . ?
S2 Ba1 I3 143.38(4) 12 . ?
S2 Ba1 I3 143.38(4) . . ?
S2 Ba1 I3 81.45(4) 3_665 . ?
I3 Ba1 I4 114.051(15) . . ?
I3 Ba1 I4 114.051(15) . 10 ?
Si1 S1 Pb1 86.75(7) . 2_655 ?
Si1 S1 Pb1 86.75(7) . 3_665 ?
Si1 S1 Pb1 86.75(7) . . ?
Pb1 S1 Pb1 119.682(14) . 3_665 ?
Pb1 S1 Pb1 119.681(14) 2_655 3_665 ?
Pb1 S1 Pb1 119.682(14) 2_655 . ?
Ba1 S2 Ba1 121.00(7) . 2_655 ?
Si1 S2 Ba1 89.63(9) . 2_655 ?
Si1 S2 Ba1 93.61(10) . . ?
Si1 S2 Pb1 89.15(13) . . ?
Pb1 S2 Ba1 108.45(7) . . ?
S2 Si1 S1 108.09(12) 2_655 . ?
S2 Si1 S1 108.09(12) 3_665 . ?
S2 Si1 S1 108.08(12) . . ?
S2 Si1 S2 110.82(12) . 2_655 ?
S2 Si1 S2 110.82(12) 2_655 3_665 ?
S2 Si1 S2 110.82(12) . 3_665 ?
Ba1 I4 Ba1 96.23(2) 2 . ?
Ba1 I4 Ba1 96.24(2) 3 2 ?
Ba1 I4 Ba1 96.23(2) 3 . ?
I1 Pb1 I2 73.110(16) . . ?
S1 Pb1 I2 132.67(5) . . ?
S1 Pb1 I1 74.207(17) . . ?
S2 Pb1 I2 139.01(5) . . ?
S2 Pb1 I1 91.56(5) . . ?
S2 Pb1 S1 74.47(8) . . ?
Ba1 I3 Ba1 120.0 2_665 . ?
Ba1 I3 Ba1 120.000(1) 3_565 . ?
Ba1 I3 Ba1 120.0 3_565 2_665 ?

_shelx_res_file                  
;
TITL mo_zjz20210406002_0m_a.res in R-3c
    mo_zjz20210406002_0m.res
    created by SHELXL-2016/6 at 19:21:40 on 24-Jun-2024
REM Old TITL mo_ZJZ20210406002_0m in R-3c
REM SHELXT solution in R-3c
REM R1 0.263, Rweak 0.008, Alpha 0.028, Orientation as input
REM Formula found by SHELXT: Ba6 I13 S8 Si2
CELL 0.71073 9.7925 9.7925 70.6282 90 90 120
ZERR 6.00012 0.0002 0.0002 0.0028 0 0 0
LATT 3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SYMM +Y,+X,0.5-Z
SYMM -Y+X,-Y,0.5-Z
SYMM -X,-X+Y,0.5-Z
SFAC Ba I Pb S Si
UNIT 18 60 36 48 12

L.S. 40
PLAN  6
TEMP 0
CONF
BIND Pb1 I2
list 4
fmap 2 53
acta
MORE -1
OMIT 0 0 6
REM <olex2.extras>
REM <HklSrc "%.\\mo_zjz20210406002_0m.hkl">
REM </olex2.extras>

WGHT    0.028500  247.849197
EXTI    0.000019
FVAR       0.02854
I2    2    0.000000    0.000000    0.500000    10.16667    0.01869    0.01869 =
         0.01993    0.00000    0.00000    0.00934
I1    2    0.326701    0.411219    0.474930    11.00000    0.02282    0.02480 =
         0.05325    0.00519    0.00896    0.01140
BA1   1    0.333333    0.322095    0.416667    10.50000    0.04031    0.02712 =
         0.07426   -0.01907   -0.03815    0.02016
S1    4    0.666667    0.333333    0.477936    10.33333    0.01847    0.01847 =
         0.01237    0.00000    0.00000    0.00923
S2    4    0.460276    0.129659    0.438188    11.00000    0.01885    0.01865 =
         0.02275   -0.00407   -0.00324    0.00897
SI1   5    0.666667    0.333333    0.447469    10.33333    0.01511    0.01511 =
         0.01715    0.00000    0.00000    0.00755
PART 2
I4    2    0.000000    0.000000    0.443678    10.33333    0.04527    0.04527 =
         0.02330    0.00000    0.00000    0.02264
PART 6
PB1   3    0.344767    0.079129    0.475624    11.00000    0.04357    0.03685 =
         0.03661    0.00146    0.01312    0.01110
PART 0
I3    2    0.333333    0.666667    0.416667    10.16667    0.02247    0.02247 =
         0.18919    0.00000    0.00000    0.01123
HKLF 4




REM  mo_zjz20210406002_0m_a.res in R-3c
REM R1 =  0.0434 for    1507 Fo > 4sig(Fo)  and  0.0540 for all    1870 data
REM     47 parameters refined using      0 restraints

END

WGHT      0.0285    247.9035

REM Highest difference peak  2.111,  deepest hole -2.194,  1-sigma level  0.326
Q1    1   0.0471  0.0713  0.4399  11.00000  0.05    2.11
Q2    1   0.3593  0.2782  0.4207  11.00000  0.05    1.62
Q3    1   0.0454  0.0758  0.4496  11.00000  0.05    1.50
Q4    1   0.3446  0.1492  0.4685  11.00000  0.05    1.24
Q5    1   0.3551  0.4753  0.4665  11.00000  0.05    1.15
Q6    1   0.3790  0.0292  0.4718  11.00000  0.05    1.10
;
_shelx_res_checksum              40531
_olex2_submission_special_instructions 'No special instructions were received'
