# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_gz1412
_database_code_depnum_ccdc_archive 'CCDC 2171871'
loop_
_audit_author_name
_audit_author_address
'Michelle C. Neary'
;Hunter College, City University of New York
United States of America
;
_audit_update_record             
;
2022-05-10 deposited with the CCDC.	2022-06-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H66 Pb2 Si6'
_chemical_formula_sum            'C24 H66 Pb2 Si6'
_chemical_formula_weight         937.68

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 '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'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           143
_space_group_name_H-M_alt        'P 3'
_space_group_name_Hall           'P 3'

_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'
'-y, x-y, z'
'-x+y, -x, z'

_cell_length_a                   10.6008(2)
_cell_length_b                   10.6008(2)
_cell_length_c                   9.9986(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     973.08(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    9913
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      38.65

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.600
_exptl_crystal_F_000             458
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.430
_exptl_crystal_size_mid          0.330
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    8.836
_shelx_estimated_absorpt_T_min   0.115
_shelx_estimated_absorpt_T_max   0.443
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.2354
_exptl_absorpt_correction_T_max  0.4993
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            29256
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.012
_diffrn_reflns_theta_max         36.261
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             6315
_reflns_number_gt                6100
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    0.997

_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       'Bruker APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
; 
 Refined as a 2-component twin. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0243P)²+0.8413P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
; 
 Flack x determined using 2978 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.03(3)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         6315
_refine_ls_number_parameters     104
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0191
_refine_ls_R_factor_gt           0.0179
_refine_ls_wR_factor_ref         0.0465
_refine_ls_wR_factor_gt          0.0460
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.071
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

_vrf_PLAT094_gz1412              
;
PROBLEM: Ratio of Maximum / Minimum Residual Density ....       6.44 Report
RESPONSE: There is excess electron density due to the heavy atom Pb
;
_vrf_PLAT111_gz1412              
;
PROBLEM: ADDSYM Detects New (Pseudo) Centre of Symmetry .        100 %Fit  
RESPONSE: Disorder in the SiMe3 group orientation breaks the symmetry. The
model is much better with this space group and a twin law than with the 
higher symmetry space group with disorder.
;
_vrf_PLAT113_gz1412              
;
PROBLEM: ADDSYM Suggests Possible Pseudo/New  Space Group        P-3 Check 
RESPONSE: Disorder in the SiMe3 group orientation breaks the symmetry. The
model is much better with this space group and a twin law than with the 
higher symmetry space group with disorder.
;

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
Pb1 Pb 0.333333 0.666667 0.38851(2) 0.01073(12) Uani 1 3 d S T P . .
C11 C 0.1995(9) 0.4451(9) 0.2931(9) 0.0170(12) Uani 1 1 d . . . . .
H11A H 0.234746 0.452579 0.200173 0.020 Uiso 1 1 calc R U . . .
H11B H 0.222364 0.377203 0.340863 0.020 Uiso 1 1 calc R U . . .
Si1 Si -0.0028(3) 0.3577(3) 0.2857(2) 0.0156(4) Uani 1 1 d . . . . .
C12 C -0.0816(11) 0.1584(11) 0.2595(14) 0.033(2) Uani 1 1 d . . . . .
H12A H -0.062237 0.140497 0.167648 0.049 Uiso 1 1 calc R U . . .
H12B H -0.187062 0.108651 0.274567 0.049 Uiso 1 1 calc R U . . .
H12C H -0.037140 0.121180 0.322391 0.049 Uiso 1 1 calc R U . . .
C13 C -0.0787(11) 0.3843(13) 0.4461(11) 0.030(2) Uani 1 1 d . . . . .
H13A H -0.181439 0.355123 0.433381 0.045 Uiso 1 1 calc R U . . .
H13B H -0.023901 0.487174 0.472152 0.045 Uiso 1 1 calc R U . . .
H13C H -0.070491 0.324573 0.516577 0.045 Uiso 1 1 calc R U . . .
C14 C -0.0589(10) 0.4348(10) 0.1466(10) 0.0255(16) Uani 1 1 d . . . . .
H14A H -0.033894 0.407843 0.061001 0.038 Uiso 1 1 calc R U . . .
H14B H -0.008189 0.541140 0.154564 0.038 Uiso 1 1 calc R U . . .
H14C H -0.164343 0.396062 0.150783 0.038 Uiso 1 1 calc R U . . .
Pb2 Pb 0.333333 0.666667 0.67847(2) 0.01058(11) Uani 1 3 d S T P . .
C21 C 0.4209(9) 0.5329(9) 0.7702(8) 0.0169(12) Uani 1 1 d . . . . .
H21A H 0.511432 0.556277 0.721697 0.020 Uiso 1 1 calc R U . . .
H21B H 0.449351 0.567397 0.863316 0.020 Uiso 1 1 calc R U . . .
Si2 Si 0.3060(3) 0.3305(3) 0.7763(2) 0.0152(4) Uani 1 1 d . . . . .
C22 C 0.2035(13) 0.2540(11) 0.6187(10) 0.030(2) Uani 1 1 d . . . . .
H22A H 0.270852 0.290932 0.542703 0.046 Uiso 1 1 calc R U . . .
H22B H 0.129609 0.283073 0.608819 0.046 Uiso 1 1 calc R U . . .
H22C H 0.155923 0.147456 0.621228 0.046 Uiso 1 1 calc R U . . .
C23 C 0.1727(11) 0.2750(11) 0.9185(12) 0.031(2) Uani 1 1 d . . . . .
H23A H 0.095375 0.296303 0.895329 0.046 Uiso 1 1 calc R U . . .
H23B H 0.223235 0.329488 0.999121 0.046 Uiso 1 1 calc R U . . .
H23C H 0.129862 0.170443 0.935272 0.046 Uiso 1 1 calc R U . . .
C24 C 0.4252(12) 0.2496(11) 0.8059(11) 0.0274(18) Uani 1 1 d . . . . .
H24A H 0.484203 0.262936 0.726084 0.041 Uiso 1 1 calc R U . . .
H24B H 0.364347 0.145326 0.824911 0.041 Uiso 1 1 calc R U . . .
H24C H 0.489329 0.298064 0.882301 0.041 Uiso 1 1 calc R U . . .


_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
Pb1 C11 2.260(8) . ?
Pb1 C11 2.260(8) 3_565 ?
Pb1 C11 2.260(8) 2_665 ?
Pb1 Pb2 2.89922(19) . ?
C11 Si1 1.864(8) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
Si1 C14 1.855(10) . ?
Si1 C12 1.862(10) . ?
Si1 C13 1.878(11) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
Pb2 C21 2.243(8) 2_665 ?
Pb2 C21 2.243(8) 3_565 ?
Pb2 C21 2.243(8) . ?
C21 Si2 1.865(8) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
Si2 C22 1.855(10) . ?
Si2 C24 1.872(10) . ?
Si2 C23 1.880(11) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?

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
C11 Pb1 C11 103.5(3) . 3_565 ?
C11 Pb1 C11 103.5(3) . 2_665 ?
C11 Pb1 C11 103.5(3) 3_565 2_665 ?
C11 Pb1 Pb2 115.0(2) . . ?
C11 Pb1 Pb2 115.0(2) 3_565 . ?
C11 Pb1 Pb2 115.0(2) 2_665 . ?
Si1 C11 Pb1 120.1(4) . . ?
Si1 C11 H11A 107.3 . . ?
Pb1 C11 H11A 107.3 . . ?
Si1 C11 H11B 107.3 . . ?
Pb1 C11 H11B 107.3 . . ?
H11A C11 H11B 106.9 . . ?
C14 Si1 C12 109.5(5) . . ?
C14 Si1 C11 110.7(4) . . ?
C12 Si1 C11 108.8(4) . . ?
C14 Si1 C13 108.6(5) . . ?
C12 Si1 C13 107.9(6) . . ?
C11 Si1 C13 111.4(4) . . ?
Si1 C12 H12A 109.5 . . ?
Si1 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
Si1 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Si1 C13 H13A 109.5 . . ?
Si1 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
Si1 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
Si1 C14 H14A 109.5 . . ?
Si1 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
Si1 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C21 Pb2 C21 104.4(3) 2_665 3_565 ?
C21 Pb2 C21 104.4(3) 2_665 . ?
C21 Pb2 C21 104.4(3) 3_565 . ?
C21 Pb2 Pb1 114.2(2) 2_665 . ?
C21 Pb2 Pb1 114.2(2) 3_565 . ?
C21 Pb2 Pb1 114.2(2) . . ?
Si2 C21 Pb2 120.1(4) . . ?
Si2 C21 H21A 107.3 . . ?
Pb2 C21 H21A 107.3 . . ?
Si2 C21 H21B 107.3 . . ?
Pb2 C21 H21B 107.3 . . ?
H21A C21 H21B 106.9 . . ?
C22 Si2 C21 112.2(4) . . ?
C22 Si2 C24 108.4(5) . . ?
C21 Si2 C24 109.3(5) . . ?
C22 Si2 C23 108.7(6) . . ?
C21 Si2 C23 109.9(4) . . ?
C24 Si2 C23 108.1(5) . . ?
Si2 C22 H22A 109.5 . . ?
Si2 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
Si2 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
Si2 C23 H23A 109.5 . . ?
Si2 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
Si2 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
Si2 C24 H24A 109.5 . . ?
Si2 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
Si2 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pb1 C11 Si1 C14 79.6(6) . . . . ?
Pb1 C11 Si1 C12 -160.1(6) . . . . ?
Pb1 C11 Si1 C13 -41.2(7) . . . . ?
Pb2 C21 Si2 C22 41.7(7) . . . . ?
Pb2 C21 Si2 C24 162.0(5) . . . . ?
Pb2 C21 Si2 C23 -79.5(6) . . . . ?

_refine_diff_density_max         4.607
_refine_diff_density_min         -0.715
_refine_diff_density_rms         0.086

####################################################################### 
# 
# 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_pbcl2dmso
_database_code_depnum_ccdc_archive 'CCDC 2179452'
loop_
_audit_author_name
_audit_author_address
'Michelle C. Neary'
;Hunter College, City University of New York
United States of America
;
_audit_update_record             
;
2022-06-16 deposited with the CCDC.	2022-06-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 H18 Cl4 O3 Pb2 S3'
_chemical_formula_sum            'C6 H18 Cl4 O3 Pb2 S3'
_chemical_formula_weight         790.56

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_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+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   13.9407(5)
_cell_length_b                   17.4187(6)
_cell_length_c                   7.3245(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1778.60(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    9866
_cell_measurement_theta_min      2.76
_cell_measurement_theta_max      36.32

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.952
_exptl_crystal_F_000             1432
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.130
_exptl_absorpt_coefficient_mu    19.855
_shelx_estimated_absorpt_T_min   0.087
_shelx_estimated_absorpt_T_max   0.182
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4698
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 with PHOTON III detector'
_diffrn_measurement_method       'φ and ω shutterless scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            93502
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.338
_diffrn_reflns_theta_max         36.333
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4427
_reflns_number_gt                4315
_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       'Bruker APEX4'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT-2018 (Sheldrick 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0085P)²+1.2451P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.00093(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4427
_refine_ls_number_parameters     109
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0157
_refine_ls_R_factor_gt           0.0151
_refine_ls_wR_factor_ref         0.0321
_refine_ls_wR_factor_gt          0.0319
_refine_ls_goodness_of_fit_ref   1.228
_refine_ls_restrained_S_all      1.228
_refine_ls_shift/su_max          0.001
_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
Pb1 Pb 0.02464(2) 0.750000 0.01016(2) 0.01220(2) Uani 1 2 d S T P . .
Pb2 Pb 0.18037(2) 0.750000 0.54501(2) 0.01164(2) Uani 1 2 d S T P . .
Cl1 Cl -0.12567(3) 0.64712(2) 0.02440(5) 0.01848(6) Uani 1 1 d . . . . .
Cl2 Cl 0.11756(3) 0.64494(2) 0.29711(5) 0.01658(6) Uani 1 1 d . . . . .
O1 O 0.13811(9) 0.65106(6) -0.18005(16) 0.01661(19) Uani 1 1 d . . . . .
S1 S 0.13316(3) 0.56496(2) -0.14120(5) 0.01358(6) Uani 1 1 d . . . . .
C11 C 0.03070(13) 0.53130(11) -0.2615(3) 0.0249(3) Uani 1 1 d . . . . .
H11A H -0.027318 0.553706 -0.207988 0.037 Uiso 1 1 calc R U . . .
H11B H 0.027486 0.475214 -0.252863 0.037 Uiso 1 1 calc R U . . .
H11C H 0.035458 0.546421 -0.390093 0.037 Uiso 1 1 calc R U . . .
C12 C 0.22189(12) 0.52217(9) -0.2834(3) 0.0209(3) Uani 1 1 d . . . . .
H12A H 0.285669 0.539327 -0.244668 0.031 Uiso 1 1 calc R U . . .
H12B H 0.210928 0.537464 -0.410445 0.031 Uiso 1 1 calc R U . . .
H12C H 0.217901 0.466155 -0.273317 0.031 Uiso 1 1 calc R U . . .
O2 O 0.00705(14) 0.750000 0.6182(3) 0.0149(3) Uani 0.921(2) 2 d S T P A 1
S2 S -0.06459(4) 0.750000 0.45915(7) 0.01134(12) Uani 0.921(2) 2 d S T P A 1
C21 C -0.1441(2) 0.6719(3) 0.5058(7) 0.0211(5) Uani 0.921(2) 1 d . . P A 1
H21A H -0.198725 0.674021 0.421701 0.032 Uiso 0.921(2) 1 calc R U P A 1
H21B H -0.167276 0.675695 0.631795 0.032 Uiso 0.921(2) 1 calc R U P A 1
H21C H -0.109921 0.623246 0.489447 0.032 Uiso 0.921(2) 1 calc R U P A 1
O2A O -0.0157(18) 0.750000 0.684(4) 0.025(5) Uani 0.079(2) 2 d S T P A 2
S2A S -0.1230(5) 0.750000 0.6344(10) 0.0179(16) Uani 0.079(2) 2 d S T P A 2
C21A C -0.130(4) 0.675(4) 0.499(10) 0.0211(5) Uani 0.079(2) 1 d . . P A 2
H21D H -0.177192 0.684994 0.403654 0.032 Uiso 0.079(2) 1 calc R U P A 2
H21E H -0.148761 0.630117 0.570322 0.032 Uiso 0.079(2) 1 calc R U P A 2
H21F H -0.066822 0.666026 0.443342 0.032 Uiso 0.079(2) 1 calc R U 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
Pb1 O2A 2.46(3) 1_554 ?
Pb1 O1 2.7227(12) . ?
Pb1 O1 2.7228(12) 7_575 ?
Pb1 Cl1 2.7591(4) . ?
Pb1 Cl1 2.7592(4) 7_575 ?
Pb1 Cl2 3.0731(4) . ?
Pb1 Cl2 3.0732(4) 7_575 ?
Pb2 O2 2.475(2) . ?
Pb2 O1 2.7152(12) 7_576 ?
Pb2 O1 2.7152(12) 1_556 ?
Pb2 Cl2 2.7225(4) . ?
Pb2 Cl2 2.7225(4) 7_575 ?
O1 S1 1.5282(12) . ?
S1 C11 1.7779(18) . ?
S1 C12 1.7804(17) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
O2 S2 1.5346(19) . ?
S2 C21 1.787(3) . ?
S2 C21 1.788(3) 7_575 ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
O2A S2A 1.54(3) . ?
S2A C21A 1.64(8) . ?
S2A C21A 1.64(8) 7_575 ?
C21A H21D 0.9800 . ?
C21A H21E 0.9800 . ?
C21A H21F 0.9800 . ?

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
O2A Pb1 O1 68.6(5) 1_554 . ?
O1 Pb1 O1 78.54(5) . 7_575 ?
O2A Pb1 Cl1 82.1(5) 1_554 . ?
O1 Pb1 Cl1 92.83(3) . . ?
O1 Pb1 Cl1 150.65(3) 7_575 . ?
O1 Pb1 Cl1 150.65(3) . 7_575 ?
O1 Pb1 Cl1 92.83(3) 7_575 7_575 ?
Cl1 Pb1 Cl1 81.007(18) . 7_575 ?
O2A Pb1 Cl2 139.7(3) 1_554 . ?
O1 Pb1 Cl2 74.23(3) . . ?
O1 Pb1 Cl2 118.81(3) 7_575 . ?
Cl1 Pb1 Cl2 84.694(11) . . ?
Cl1 Pb1 Cl2 132.924(11) 7_575 . ?
O1 Pb1 Cl2 118.81(3) . 7_575 ?
O1 Pb1 Cl2 74.23(3) 7_575 7_575 ?
Cl1 Pb1 Cl2 132.923(11) . 7_575 ?
Cl1 Pb1 Cl2 84.694(11) 7_575 7_575 ?
Cl2 Pb1 Cl2 73.091(13) . 7_575 ?
O2 Pb2 O1 68.13(4) . 7_576 ?
O2 Pb2 O1 68.13(4) . 1_556 ?
O1 Pb2 O1 78.80(5) 7_576 1_556 ?
O2 Pb2 Cl2 80.24(4) . . ?
O1 Pb2 Cl2 148.37(3) 7_576 . ?
O1 Pb2 Cl2 89.90(3) 1_556 . ?
O2 Pb2 Cl2 80.24(4) . 7_575 ?
O1 Pb2 Cl2 89.90(3) 7_576 7_575 ?
O1 Pb2 Cl2 148.37(3) 1_556 7_575 ?
Cl2 Pb2 Cl2 84.467(16) . 7_575 ?
Pb2 Cl2 Pb1 101.037(11) . . ?
S1 O1 Pb2 140.43(7) . 1_554 ?
S1 O1 Pb1 119.98(6) . . ?
Pb2 O1 Pb1 95.96(3) 1_554 . ?
O1 S1 C11 105.52(8) . . ?
O1 S1 C12 105.70(7) . . ?
C11 S1 C12 97.48(9) . . ?
S1 C11 H11A 109.5 . . ?
S1 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
S1 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
S1 C12 H12A 109.5 . . ?
S1 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
S1 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
S2 O2 Pb2 118.09(12) . . ?
O2 S2 C21 104.98(17) . . ?
O2 S2 C21 104.98(17) . 7_575 ?
C21 S2 C21 99.1(3) . 7_575 ?
S2 C21 H21A 109.5 . . ?
S2 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
S2 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O2A S2A C21A 101(2) . . ?
O2A S2A C21A 101(2) . 7_575 ?
C21A S2A C21A 105(5) . 7_575 ?
S2A C21A H21D 109.5 . . ?
S2A C21A H21E 109.5 . . ?
H21D C21A H21E 109.5 . . ?
S2A C21A H21F 109.5 . . ?
H21D C21A H21F 109.5 . . ?
H21E C21A H21F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pb2 O1 S1 C11 -71.94(13) 1_554 . . . ?
Pb1 O1 S1 C11 80.48(9) . . . . ?
Pb2 O1 S1 C12 30.67(13) 1_554 . . . ?
Pb1 O1 S1 C12 -176.91(8) . . . . ?
Pb2 O2 S2 C21 128.04(17) . . . . ?
Pb2 O2 S2 C21 -128.04(17) . . . 7_575 ?
Pb1 O2A S2A C21A -126(3) 1_556 . . . ?
Pb1 O2A S2A C21A 126(3) 1_556 . . 7_575 ?

_refine_diff_density_max         2.287
_refine_diff_density_min         -1.309
_refine_diff_density_rms         0.170

