# Supplementary Information (SI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2025

####################################################################### 
# 
# 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_i-4_a
_database_code_depnum_ccdc_archive 'CCDC 2384809'
loop_
_audit_author_name
_audit_author_address
'Jingyu GUO'
;Beijing Normal University at Zhuhai
China
;
_audit_update_record             
;
2024-09-18 deposited with the CCDC.	2025-01-06 downloaded from the CCDC.
;
_audit_creation_date             2024-07-05
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'I8 P4 S16 Sn11, 2(I)'
_chemical_formula_sum            'I10 P4 S16 Sn11'
_chemical_formula_weight         3211.43
_chemical_absolute_configuration ad
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'

_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      tetragonal
_space_group_IT_number           121
_space_group_name_H-M_alt        'I -4 2 m'
_space_group_name_Hall           'I -4 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x, y, -z'
'x, -y, -z'
'-y, -x, z'
'y, x, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'

_cell_length_a                   9.3157(4)
_cell_length_b                   9.3157(4)
_cell_length_c                   13.8689(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1203.57(15)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    3613
_cell_measurement_temperature    302.0
_cell_measurement_theta_max      24.425
_cell_measurement_theta_min      2.633
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    13.358
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5487
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    4.431
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1396
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0666
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13224
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.807
_diffrn_reflns_theta_min         2.634
_diffrn_ambient_temperature      302.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.722
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.982
_reflns_number_gt                742
_reflns_number_total             780
_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       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         1.951
_refine_diff_density_min         -2.471
_refine_diff_density_rms         0.251
_refine_ls_abs_structure_details 
;
 Flack x determined using 301 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.193
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     29
_refine_ls_number_reflns         780
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0520
_refine_ls_restrained_S_all      1.193
_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/[σ²(Fo²)+(0.0067P)²+47.8273P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1069
_refine_special_details          ?
_olex2_refinement_description    
;
1. Others
 Fixed Sof: Sn2(0.1875)
;
_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
I1 I 0.18753(14) 0.18753(14) 0.57770(11) 0.0503(5) Uani 1 2 d S T P . .
I2 I 0.500000 0.500000 0.500000 0.0549(9) Uani 1 8 d S T P . .
Sn1 Sn 0.3501(2) 0.3501(2) 0.7191(2) 0.0922(10) Uani 1 2 d S T P . .
Sn2 Sn 0.000000 0.500000 0.500000 0.0939(18) Uani 0.75 4 d S T P . .
P1 P 0.000000 0.500000 0.750000 0.0398(18) Uani 1 4 d S T P . .
S1 S 0.0930(5) 0.3460(5) 0.8338(3) 0.0442(10) Uani 1 1 d . . . . .

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
I1 0.0586(6) 0.0586(6) 0.0338(7) -0.0072(5) -0.0072(5) -0.0023(8)
I2 0.0629(15) 0.0629(15) 0.0389(18) 0.000 0.000 0.000
Sn1 0.0781(12) 0.0781(12) 0.120(2) -0.0373(12) -0.0373(12) -0.0051(14)
Sn2 0.075(3) 0.160(6) 0.047(2) 0.000 0.000 0.000
P1 0.037(3) 0.037(3) 0.044(4) 0.000 0.000 0.000
S1 0.044(2) 0.043(2) 0.046(2) 0.0030(19) 0.0009(18) 0.0057(18)

_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
I1 Sn1 2.904(3) . ?
Sn1 S1 2.876(5) 8 ?
Sn1 S1 2.876(5) . ?
Sn2 S1 2.850(4) 12_556 ?
Sn2 S1 2.850(4) 15_554 ?
Sn2 S1 2.850(4) 11_456 ?
Sn2 S1 2.850(4) 16_454 ?
P1 S1 2.040(4) . ?
P1 S1 2.040(4) 12_556 ?
P1 S1 2.040(4) 11_456 ?
P1 S1 2.040(4) 2_565 ?

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 Sn1 I1 86.11(11) 8 . ?
S1 Sn1 I1 86.11(11) . . ?
S1 Sn1 S1 70.82(19) 8 . ?
S1 Sn2 S1 119.54(17) 16_454 11_456 ?
S1 Sn2 S1 72.05(17) 12_556 11_456 ?
S1 Sn2 S1 72.05(17) 16_454 15_554 ?
S1 Sn2 S1 144.59(17) 12_556 16_454 ?
S1 Sn2 S1 119.54(17) 12_556 15_554 ?
S1 Sn2 S1 144.59(17) 15_554 11_456 ?
S1 P1 S1 108.95(12) . 11_456 ?
S1 P1 S1 110.5(2) 11_456 12_556 ?
S1 P1 S1 110.5(2) . 2_565 ?
S1 P1 S1 108.95(12) 2_565 12_556 ?
S1 P1 S1 108.95(12) . 12_556 ?
S1 P1 S1 108.95(12) 11_456 2_565 ?
Sn2 S1 Sn1 133.94(16) 11_456 . ?
P1 S1 Sn1 91.67(16) . . ?
P1 S1 Sn2 88.71(15) . 11_456 ?

_shelx_res_file                  
;
TITL bbb_a.res in I-42m
    i-4_a.res
    created by SHELXL-2018/3 at 10:08:07 on 05-Jul-2024
REM Old TITL BBB in I-42m
REM SHELXT solution in I-42m: R1 0.181, Rweak 0.049, Alpha 0.001
REM <I/s> 0.000 for 0 systematic absences, Orientation as input
REM Flack x = 0.130 ( 0.027 ) from 263 Parsons' quotients
REM Formula found by SHELXT: P2 S10 Sn4 I5
CELL 0.71073 9.3157 9.3157 13.8689 90 90 90
ZERR 1 0.0004 0.0004 0.0013 0 0 0
LATT -2
SYMM -X,-Y,+Z
SYMM +Y,-X,-Z
SYMM -Y,+X,-Z
SYMM -X,+Y,-Z
SYMM +X,-Y,-Z
SYMM -Y,-X,+Z
SYMM +Y,+X,+Z
SFAC I P S Sn
UNIT 10 4 16 11

L.S. 20
PLAN  2
TEMP 28.85
CONF
list 4
MORE -1
fmap 2 53
acta
REM <olex2.extras>
REM <HklSrc "%.\\I-4_a.hkl">
REM </olex2.extras>

WGHT    0.006700   47.827301
FVAR       0.21176
I1    1    0.187531    0.187531    0.577699    10.50000    0.05861    0.05861 =
         0.03382   -0.00720   -0.00720   -0.00228
I2    1    0.500000    0.500000    0.500000    10.12500    0.06290    0.06290 =
         0.03889    0.00000    0.00000    0.00000
SN1   4    0.350136    0.350136    0.719081    10.50000    0.07810    0.07810 =
         0.12050   -0.03734   -0.03734   -0.00510
SN2   4    0.000000    0.500000    0.500000    10.18750    0.07531    0.15987 =
         0.04655    0.00000    0.00000    0.00000
P1    2    0.000000    0.500000    0.750000    10.25000    0.03749    0.03749 =
         0.04439    0.00000    0.00000    0.00000
S1    3    0.093031    0.345981    0.833805    11.00000    0.04368    0.04312 =
         0.04585    0.00300    0.00092    0.00570
HKLF 4




REM  bbb_a.res in I-42m
REM wR2 = 0.1069, GooF = S = 1.193, Restrained GooF = 1.193 for all data
REM R1 = 0.0520 for 742 Fo > 4sig(Fo) and 0.0548 for all 780 data
REM 29 parameters refined using 0 restraints

END

WGHT      0.0065     47.8339

REM Highest difference peak  1.951,  deepest hole -2.471,  1-sigma level  0.251
Q1    1   0.3384  0.3384  0.7389  10.50000  0.05    1.95
Q2    1   0.3006  0.3006  0.7209  10.50000  0.05    1.60
;
_shelx_res_checksum              72469
_olex2_submission_special_instructions 'No special instructions were received'
