# Electronic Supplementary Material (ESI) for CrystEngComm.
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 2175218'
loop_
_audit_author_name
_audit_author_address
'Yoshitaka Mastushita'
;National Institute for Materials Science
Japan
;
_audit_update_record             
;
2022-05-27 deposited with the CCDC.	2022-10-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C3 H11 Cl3 N2 O Pb S'
_chemical_formula_weight         436.74

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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'
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   9.7289(2)
_cell_length_b                   13.9219(2)
_cell_length_c                   8.9307(2)
_cell_angle_alpha                90
_cell_angle_beta                 113.7730(10)
_cell_angle_gamma                90
_cell_volume                     1106.98(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    113(2)
_cell_measurement_reflns_used    9875
_cell_measurement_theta_min      2.49
_cell_measurement_theta_max      46.19

_exptl_crystal_description       Chunk
_exptl_crystal_colour            'Clear white'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.621
_exptl_crystal_F_000             800
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.093
_exptl_crystal_size_mid          0.037
_exptl_crystal_size_min          0.029
_exptl_absorpt_coefficient_mu    16.108
_shelx_estimated_absorpt_T_min   0.316
_shelx_estimated_absorpt_T_max   0.652
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6472
_exptl_absorpt_correction_T_max  0.8631
_exptl_absorpt_process_details   
;
CrystalClear (Rigaku, 1997--2002)
;
_diffrn_ambient_temperature      113(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_detector       CCD
_diffrn_measurement_device       
;
Rigaku AFC11 Saturn724+ (4x4 bin mode)
;
_diffrn_measurement_method       dtprofit.ref
_diffrn_reflns_number            14383
_diffrn_reflns_av_unetI/netI     0.0140
_diffrn_reflns_av_R_equivalents  0.0229
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.890
_diffrn_reflns_theta_max         26.367
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             2259
_reflns_number_gt                2180
_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       'CrystalClear (Rigaku, 1997--2002)'
_computing_cell_refinement       'CrystalClear (Rigaku, 1997--2002)'
_computing_data_reduction        'CrystalClear (Rigaku, 1997--2002)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_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)+(0.0111P)²+0.7379P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_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_number_reflns         2259
_refine_ls_number_parameters     102
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0118
_refine_ls_R_factor_gt           0.0111
_refine_ls_wR_factor_ref         0.0267
_refine_ls_wR_factor_gt          0.0264
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_restrained_S_all      1.106
_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
Pb Pb 0.15539(2) 0.38723(2) 0.11327(2) 0.00948(4) Uani 1 1 d . . . . .
Cl1 Cl 0.45511(6) 0.36173(4) 0.24509(6) 0.01422(10) Uani 1 1 d . . . . .
Cl2 Cl 0.15240(6) 0.27080(4) 0.38364(6) 0.01555(11) Uani 1 1 d . . . . .
Cl3 Cl 0.14982(6) 0.53365(4) -0.10930(6) 0.01553(11) Uani 1 1 d . . . . .
S S 0.15094(6) 0.61354(3) 0.27783(7) 0.01135(11) Uani 1 1 d . . . . .
O O 0.25534(17) 0.52651(11) 0.30180(19) 0.0154(3) Uani 1 1 d . . . . .
N1 N 0.4999(2) 0.39751(14) 0.9096(2) 0.0171(4) Uani 1 1 d . . . . .
H1AN H 0.582943 0.430025 0.928868 0.021 Uiso 1 1 calc R U . . .
H1BN H 0.481237 0.375198 0.991640 0.021 Uiso 1 1 calc R U . . .
N2 N 0.4219(2) 0.41214(16) 0.6309(2) 0.0216(4) Uani 1 1 d . . . . .
H2AN H 0.502423 0.445122 0.641274 0.026 Uiso 1 1 calc R U . . .
H2BN H 0.352928 0.399323 0.532978 0.026 Uiso 1 1 calc R U . . .
C1 C 0.4050(3) 0.38246(14) 0.7599(3) 0.0141(5) Uani 1 1 d . . . . .
H1 H 0.316684 0.347082 0.743890 0.017 Uiso 1 1 calc R U . . .
C2 C 0.2714(3) 0.71553(17) 0.3279(3) 0.0199(5) Uani 1 1 d . . . . .
H2A H 0.213991 0.772986 0.329920 0.030 Uiso 1 1 calc R U . . .
H2B H 0.313283 0.723550 0.245567 0.030 Uiso 1 1 calc R U . . .
H2C H 0.353279 0.706213 0.435730 0.030 Uiso 1 1 calc R U . . .
C3 C 0.1058(3) 0.61176(18) 0.4521(3) 0.0238(6) Uani 1 1 d . . . . .
H3A H 0.055835 0.671975 0.457453 0.036 Uiso 1 1 calc R U . . .
H3B H 0.198144 0.604705 0.551338 0.036 Uiso 1 1 calc R U . . .
H3C H 0.038635 0.557628 0.443380 0.036 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
Pb O 2.4940(15) . ?
Pb Cl1 2.6920(5) . ?
Pb Cl3 2.8324(5) . ?
Pb Cl2 2.9181(5) . ?
Pb Cl2 2.9998(5) 4_565 ?
Pb Cl3 3.1538(5) 3_565 ?
S O 1.5396(15) . ?
S C2 1.780(2) . ?
S C3 1.779(3) . ?
N1 C1 1.299(3) . ?
N1 H1AN 0.8800 . ?
N1 H1BN 0.8800 . ?
N2 C1 1.295(3) . ?
N2 H2AN 0.8800 . ?
N2 H2BN 0.8800 . ?
C1 H1 0.9500 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 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
O Pb Cl1 75.43(4) . . ?
O Pb Cl3 78.82(4) . . ?
Cl1 Pb Cl3 96.472(15) . . ?
O Pb Cl2 90.26(4) . . ?
Cl1 Pb Cl2 86.286(15) . . ?
Cl3 Pb Cl2 167.614(17) . . ?
O Pb Cl2 157.73(4) . 4_565 ?
Cl1 Pb Cl2 84.981(15) . 4_565 ?
Cl3 Pb Cl2 93.205(17) . 4_565 ?
Cl2 Pb Cl2 99.072(4) . 4_565 ?
O Pb Cl3 81.09(4) . 3_565 ?
Cl1 Pb Cl3 154.147(15) . 3_565 ?
Cl3 Pb Cl3 89.381(14) . 3_565 ?
Cl2 Pb Cl3 83.104(14) . 3_565 ?
Cl2 Pb Cl3 119.923(14) 4_565 3_565 ?
Pb Cl2 Pb 166.53(2) . 4_566 ?
Pb Cl3 Pb 90.619(14) . 3_565 ?
O S C2 105.20(11) . . ?
O S C3 104.42(11) . . ?
C2 S C3 99.27(12) . . ?
O S Pb 39.40(6) . . ?
C2 S Pb 135.11(8) . . ?
C3 S Pb 113.94(8) . . ?
O S Pb 112.22(6) . 3_565 ?
C2 S Pb 117.04(8) . 3_565 ?
C3 S Pb 116.98(10) . 3_565 ?
Pb S Pb 74.420(11) . 3_565 ?
S O Pb 117.53(8) . . ?
S O Pb 48.80(5) . 3_565 ?
Pb O Pb 70.59(3) . 3_565 ?
C1 N1 Pb 94.35(14) . 1_556 ?
C1 N1 Pb 106.88(14) . 3_666 ?
Pb N1 Pb 137.19(5) 1_556 3_666 ?
C1 N1 H1AN 120.0 . . ?
Pb N1 H1AN 136.5 1_556 . ?
Pb N1 H1AN 15.9 3_666 . ?
C1 N1 H1BN 120.0 . . ?
Pb N1 H1BN 36.8 1_556 . ?
Pb N1 H1BN 132.2 3_666 . ?
H1AN N1 H1BN 120.0 . . ?
C1 N2 Pb 133.75(15) . . ?
C1 N2 H2AN 120.0 . . ?
Pb N2 H2AN 106.2 . . ?
C1 N2 H2BN 120.0 . . ?
Pb N2 H2BN 13.8 . . ?
H2AN N2 H2BN 120.0 . . ?
N1 C1 N2 124.8(2) . . ?
N1 C1 Pb 121.66(14) . 4_566 ?
N2 C1 Pb 105.18(15) . 4_566 ?
N1 C1 Pb 69.63(13) . 1_556 ?
N2 C1 Pb 151.52(15) . 1_556 ?
Pb C1 Pb 80.69(4) 4_566 1_556 ?
N1 C1 H1 117.6 . . ?
N2 C1 H1 117.6 . . ?
Pb C1 H1 31.9 4_566 . ?
Pb C1 H1 55.0 1_556 . ?
S C2 Pb 43.03(6) . 3_565 ?
S C2 H2A 109.5 . . ?
Pb C2 H2A 86.9 3_565 . ?
S C2 H2B 109.5 . . ?
Pb C2 H2B 84.2 3_565 . ?
H2A C2 H2B 109.5 . . ?
S C2 H2C 109.5 . . ?
Pb C2 H2C 152.4 3_565 . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
S C3 Pb 101.54(10) . 2 ?
S C3 Pb 44.93(6) . . ?
Pb C3 Pb 135.25(7) 2 . ?
S C3 Pb 43.08(7) . 3_565 ?
Pb C3 Pb 79.86(4) 2 3_565 ?
Pb C3 Pb 55.44(3) . 3_565 ?
S C3 H3A 109.5 . . ?
Pb C3 H3A 9.4 2 . ?
Pb C3 H3A 144.6 . . ?
Pb C3 H3A 89.2 3_565 . ?
S C3 H3B 109.5 . . ?
Pb C3 H3B 117.8 2 . ?
Pb C3 H3B 103.3 . . ?
Pb C3 H3B 152.1 3_565 . ?
H3A C3 H3B 109.5 . . ?
S C3 H3C 109.5 . . ?
Pb C3 H3C 108.7 2 . ?
Pb C3 H3C 70.3 . . ?
Pb C3 H3C 82.0 3_565 . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 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
C2 S O Pb -145.68(10) . . . . ?
C3 S O Pb 110.30(12) . . . . ?
Pb S O Pb -17.36(10) 3_565 . . . ?
C2 S O Pb -128.31(10) . . . 3_565 ?
C3 S O Pb 127.67(11) . . . 3_565 ?
Pb S O Pb 17.36(10) . . . 3_565 ?
Pb N1 C1 N2 152.1(2) 1_556 . . . ?
Pb N1 C1 N2 9.7(3) 3_666 . . . ?
Pb N1 C1 Pb -64.43(12) 1_556 . . 4_566 ?
Pb N1 C1 Pb 153.20(8) 3_666 . . 4_566 ?
Pb N1 C1 Pb -142.37(8) 3_666 . . 1_556 ?
Pb N2 C1 N1 -179.90(15) . . . . ?
Pb N2 C1 Pb 31.8(2) . . . 4_566 ?
Pb N2 C1 Pb -66.8(4) . . . 1_556 ?
O S C2 Pb 125.36(10) . . . 3_565 ?
C3 S C2 Pb -126.83(11) . . . 3_565 ?
Pb S C2 Pb 94.89(10) . . . 3_565 ?
O S C3 Pb 174.09(7) . . . 2 ?
C2 S C3 Pb 65.65(10) . . . 2 ?
Pb S C3 Pb -145.27(3) . . . 2 ?
Pb S C3 Pb -61.22(8) 3_565 . . 2 ?
O S C3 Pb -40.64(7) . . . . ?
C2 S C3 Pb -149.08(10) . . . . ?
Pb S C3 Pb 84.04(6) 3_565 . . . ?
O S C3 Pb -124.69(9) . . . 3_565 ?
C2 S C3 Pb 126.87(10) . . . 3_565 ?
Pb S C3 Pb -84.04(6) . . . 3_565 ?

_refine_diff_density_max         1.286
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.089



_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: DMSO'
####################################################################### 
# 
# 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_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2175219'
loop_
_audit_author_name
_audit_author_address
'Yoshitaka Mastushita'
;National Institute for Materials Science
Japan
;
_audit_update_record             
;
2022-05-27 deposited with the CCDC.	2022-10-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C3 H11 Cl3 N2 O Pb S'
_chemical_formula_weight         436.74

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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'
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   9.8864(4)
_cell_length_b                   14.1043(4)
_cell_length_c                   9.0106(3)
_cell_angle_alpha                90
_cell_angle_beta                 113.211(5)
_cell_angle_gamma                90
_cell_volume                     1154.75(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7938
_cell_measurement_theta_min      2.6480
_cell_measurement_theta_max      29.3460
_exptl_crystal_colour            'Clear white'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.512
_exptl_crystal_F_000             800
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.079
_exptl_crystal_size_min          0.045
_exptl_absorpt_coefficient_mu    15.442
_shelx_estimated_absorpt_T_min   0.119
_shelx_estimated_absorpt_T_max   0.543
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.60a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.29726
_exptl_absorpt_correction_T_max  1.00000
_diffrn_ambient_temperature      293(2)
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_reflns_number            19267
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.667
_diffrn_reflns_theta_max         30.648
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             3452
_reflns_number_gt                2848
_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       'CrysAlisPro 1.171.40.60a (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.60a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.60a (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_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)+(0.0101P)²+0.7560P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.00248(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3452
_refine_ls_number_parameters     103
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0256
_refine_ls_wR_factor_ref         0.0422
_refine_ls_wR_factor_gt          0.0402
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.050
_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
Pb Pb 0.15566(2) 0.38787(2) 0.11502(2) 0.02712(5) Uani 1 1 d . . . . .
Cl1 Cl 0.45233(10) 0.36268(7) 0.24128(12) 0.0401(2) Uani 1 1 d . . . . .
Cl2 Cl 0.15249(11) 0.26919(7) 0.38170(12) 0.0452(2) Uani 1 1 d . . . . .
Cl3 Cl 0.15326(11) 0.53727(7) -0.09822(12) 0.0455(2) Uani 1 1 d . . . . .
S S 0.14824(10) 0.61059(6) 0.28385(11) 0.0332(2) Uani 1 1 d . . . . .
O O 0.2471(3) 0.52290(18) 0.3093(3) 0.0418(7) Uani 1 1 d . . . . .
N1 N 0.4950(4) 0.3959(3) 0.9036(4) 0.0573(11) Uani 1 1 d . . . . .
H1AN H 0.572810 0.429436 0.922888 0.069 Uiso 1 1 calc R U . . .
H1BN H 0.478867 0.370945 0.982123 0.069 Uiso 1 1 calc R U . . .
N2 N 0.4149(5) 0.4163(3) 0.6325(4) 0.0693(12) Uani 1 1 d . . . . .
H2AN H 0.489532 0.450625 0.641082 0.083 Uiso 1 1 calc R U . . .
H2BN H 0.347929 0.404309 0.538824 0.083 Uiso 1 1 calc R U . . .
C1 C 0.4036(5) 0.3833(3) 0.7585(6) 0.0460(10) Uani 1 1 d . . . . .
H1 H 0.321112 0.346597 0.743466 0.055 Uiso 1 1 calc R U . . .
C2 C 0.2707(5) 0.7092(3) 0.3318(6) 0.0583(13) Uani 1 1 d . . . . .
H2A H 0.217650 0.766094 0.332789 0.087 Uiso 1 1 calc R U . . .
H2B H 0.312194 0.714889 0.252199 0.087 Uiso 1 1 calc R U . . .
H2C H 0.348115 0.699866 0.436267 0.087 Uiso 1 1 calc R U . . .
C3 C 0.1041(7) 0.6141(4) 0.4562(6) 0.0728(16) Uani 1 1 d . . . . .
H3A H 0.054883 0.672617 0.457193 0.109 Uiso 1 1 calc R U . . .
H3B H 0.192805 0.609731 0.552001 0.109 Uiso 1 1 calc R U . . .
H3C H 0.040689 0.561850 0.452706 0.109 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
Pb O 2.503(2) . ?
Pb Cl1 2.7190(10) . ?
Pb Cl3 2.8455(9) . ?
Pb Cl2 2.9388(9) . ?
Pb Cl2 3.0457(9) 4_565 ?
S O 1.536(2) . ?
S C3 1.771(5) . ?
S C2 1.782(4) . ?
N1 C1 1.275(5) . ?
N2 C1 1.272(5) . ?

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
O Pb Cl1 76.94(6) . . ?
O Pb Cl3 79.25(6) . . ?
Cl1 Pb Cl3 95.73(3) . . ?
O Pb Cl2 88.78(6) . . ?
Cl1 Pb Cl2 86.61(3) . . ?
Cl3 Pb Cl2 166.90(3) . . ?
O Pb Cl2 159.90(7) . 4_565 ?
Cl1 Pb Cl2 84.82(3) . 4_565 ?
Cl3 Pb Cl2 94.44(3) . 4_565 ?
Cl2 Pb Cl2 98.605(6) . 4_565 ?
Pb Cl2 Pb 168.00(4) . 4_566 ?
O S C3 104.7(2) . . ?
O S C2 105.1(2) . . ?
C3 S C2 98.3(2) . . ?
S O Pb 118.36(13) . . ?
N2 C1 N1 126.0(4) . . ?

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
C3 S O Pb 115.6(2) . . . . ?
C2 S O Pb -141.4(2) . . . . ?

_refine_diff_density_max         0.972
_refine_diff_density_min         -0.764
_refine_diff_density_rms         0.135



_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: DMSO'
