# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2023

####################################################################### 
# 
# 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_1
_audit_block_doi                 10.5517/ccdc.csd.cc2d0qz4
_database_code_depnum_ccdc_archive 'CCDC 2205246'
loop_
_audit_author_name
_audit_author_address
'Wei-Ming Liao'
;Guangdong University of Technology
China
;
_audit_update_record             
;
2022-09-05 deposited with the CCDC.	2023-03-22 downloaded from the CCDC.
;
_audit_creation_date             2022-03-22
_audit_creation_method           
;
Olex2 1.5-alpha
(compiled 2022.03.08 svn.r54f81f84 for OlexSys, GUI svn.r6487)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 H6 I O2 Pb S2'
_chemical_formula_sum            'C6 H6 I O2 Pb S2'
_chemical_formula_weight         508.32
_chemical_melting_point          ?
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'
I I -0.4742 1.8119 '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'

_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      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
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                   8.5418(7)
_cell_length_b                   22.790(2)
_cell_length_c                   10.2937(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2003.9(3)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9992
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      27.468
_cell_measurement_theta_min      3.099
_shelx_estimated_absorpt_T_max   0.113
_shelx_estimated_absorpt_T_min   0.095
_exptl_absorpt_coefficient_mu    20.293
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4487
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1410 before and 0.0576 after correction.
The Ratio of minimum to maximum transmission is 0.6018.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.370
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plank
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.19
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            18212
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         3.099
_diffrn_ambient_temperature      150.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2138
_reflns_number_total             2334
_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-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.891
_refine_diff_density_min         -1.899
_refine_diff_density_rms         0.184
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         2334
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0271
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0254P)²+15.4699P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0648
_refine_ls_wR_factor_ref         0.0667
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C4-H6C
 3.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
4.a Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
Pb1 Pb 0.46283(3) 0.34845(2) 0.36809(2) 0.03191(9) Uani 1 1 d . . . . .
I1 I 0.72686(6) 0.250000 0.29612(6) 0.02774(13) Uani 1 2 d S T P . .
I2 I 0.42236(8) 0.250000 0.59152(6) 0.04439(17) Uani 1 2 d S T P . .
S1 S 0.65022(15) 0.54395(6) 0.47607(17) 0.0317(3) Uani 1 1 d . . . . .
S2 S 0.92596(16) 0.63405(6) 0.56225(15) 0.0255(3) Uani 1 1 d . . . . .
O1 O 0.7297(6) 0.4173(2) 0.3005(6) 0.0487(13) Uani 1 1 d . . . . .
O2 O 0.6711(5) 0.39548(19) 0.5021(5) 0.0376(10) Uani 1 1 d . . . . .
C1 C 0.7509(6) 0.4216(2) 0.4103(6) 0.0239(11) Uani 1 1 d . U . . .
C2 C 0.8806(6) 0.4620(2) 0.4610(5) 0.0206(10) Uani 1 1 d . . . . .
C3 C 0.8481(6) 0.5211(2) 0.4868(5) 0.0193(10) Uani 1 1 d . . . . .
C4 C 0.9674(6) 0.5595(2) 0.5261(5) 0.0200(10) Uani 1 1 d D . . . .
C5 C 0.6329(13) 0.5620(5) 0.3096(10) 0.078(3) Uani 1 1 d . U . . .
H5A H 0.525983 0.575279 0.291528 0.118 Uiso 1 1 calc R U . . .
H5B H 0.656113 0.527267 0.256735 0.118 Uiso 1 1 calc R U . . .
H5C H 0.706985 0.593343 0.288145 0.118 Uiso 1 1 calc R U . . .
C6 C 1.0034(11) 0.6707(3) 0.4207(10) 0.056(2) Uani 1 1 d . U . . .
H6A H 1.050504 0.641678 0.362305 0.084 Uiso 1 1 calc R U . . .
H6B H 1.083278 0.699104 0.447541 0.084 Uiso 1 1 calc R U . . .
H6C H 0.918633 0.691203 0.375443 0.084 Uiso 1 1 calc DR U . . .

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
Pb1 0.03084(14) 0.02707(13) 0.03781(15) -0.00701(9) 0.00087(9) -0.00570(9)
I1 0.0238(2) 0.0161(2) 0.0433(3) 0.000 0.0118(2) 0.000
I2 0.0487(4) 0.0561(4) 0.0284(3) 0.000 0.0035(3) 0.000
S1 0.0175(6) 0.0253(7) 0.0523(10) -0.0107(6) -0.0042(6) 0.0029(5)
S2 0.0239(6) 0.0154(6) 0.0372(8) -0.0060(5) -0.0014(6) 0.0010(5)
O1 0.048(3) 0.035(3) 0.062(4) 0.005(2) -0.017(3) -0.006(2)
O2 0.026(2) 0.030(2) 0.057(3) -0.006(2) 0.004(2) -0.0098(17)
C1 0.015(2) 0.013(2) 0.044(3) -0.012(2) -0.011(2) -0.0016(17)
C2 0.019(2) 0.017(2) 0.026(3) -0.0055(19) 0.002(2) -0.0040(19)
C3 0.017(2) 0.018(2) 0.023(3) -0.0010(19) -0.0004(19) -0.0021(18)
C4 0.024(2) 0.012(2) 0.023(3) -0.0023(19) 0.0005(19) -0.0008(18)
C5 0.073(5) 0.102(7) 0.060(5) -0.001(5) -0.019(4) 0.038(5)
C6 0.065(4) 0.033(3) 0.070(5) 0.018(4) 0.019(4) 0.006(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
Pb1 I1 3.2664(5) . ?
Pb1 I2 3.2316(6) . ?
Pb1 S1 3.0854(14) 5_666 ?
Pb1 O2 2.493(4) . ?
S1 C3 1.772(5) . ?
S1 C5 1.769(10) . ?
S2 C4 1.775(5) . ?
S2 C6 1.805(8) . ?
O1 C1 1.149(8) . ?
O2 C1 1.308(8) . ?
C1 C2 1.533(6) . ?
C2 C3 1.400(7) . ?
C2 C4 1.395(7) 5_766 ?
C3 C4 1.403(7) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 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
I2 Pb1 I1 76.017(15) . . ?
S1 Pb1 I1 151.64(3) 5_666 . ?
S1 Pb1 I2 98.53(3) 5_666 . ?
O2 Pb1 I1 85.88(10) . . ?
O2 Pb1 I2 88.91(11) . . ?
O2 Pb1 S1 66.04(10) . 5_666 ?
Pb1 I1 Pb1 86.771(16) 7_565 . ?
Pb1 I2 Pb1 87.941(19) . 7_565 ?
C3 S1 Pb1 119.99(17) . 5_666 ?
C5 S1 Pb1 107.0(4) . 5_666 ?
C5 S1 C3 102.0(4) . . ?
C4 S2 C6 101.6(3) . . ?
C1 O2 Pb1 99.6(3) . . ?
O1 C1 O2 126.2(5) . . ?
O1 C1 C2 120.0(6) . . ?
O2 C1 C2 113.8(5) . . ?
C3 C2 C1 120.0(4) . . ?
C4 C2 C1 119.6(4) 5_766 . ?
C4 C2 C3 120.3(4) 5_766 . ?
C2 C3 S1 117.4(4) . . ?
C2 C3 C4 120.7(5) . . ?
C4 C3 S1 121.8(4) . . ?
C2 C4 S2 120.1(4) 5_766 . ?
C2 C4 C3 119.0(4) 5_766 . ?
C3 C4 S2 120.9(4) . . ?
S1 C5 H5A 109.5 . . ?
S1 C5 H5B 109.5 . . ?
S1 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
S2 C6 H6A 109.5 . . ?
S2 C6 H6B 109.5 . . ?
S2 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 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 S1 C3 C2 154.7(4) 5_666 . . . ?
Pb1 S1 C3 C4 -22.1(5) 5_666 . . . ?
Pb1 O2 C1 O1 -5.6(7) . . . . ?
Pb1 O2 C1 C2 172.9(3) . . . . ?
S1 C3 C4 S2 -2.0(7) . . . . ?
S1 C3 C4 C2 176.7(4) . . . 5_766 ?
O1 C1 C2 C3 89.0(7) . . . . ?
O1 C1 C2 C4 -87.3(7) . . . 5_766 ?
O2 C1 C2 C3 -89.6(6) . . . . ?
O2 C1 C2 C4 94.1(6) . . . 5_766 ?
C1 C2 C3 S1 6.9(7) . . . . ?
C1 C2 C3 C4 -176.3(5) . . . . ?
C2 C3 C4 S2 -178.7(4) . . . . ?
C2 C3 C4 C2 0.0(9) . . . 5_766 ?
C4 C2 C3 S1 -176.8(4) 5_766 . . . ?
C4 C2 C3 C4 0.0(9) 5_766 . . . ?
C5 S1 C3 C2 -87.4(6) . . . . ?
C5 S1 C3 C4 95.9(6) . . . . ?
C6 S2 C4 C2 76.2(6) . . . 5_766 ?
C6 S2 C4 C3 -105.1(5) . . . . ?

_shelx_res_file                  
;
TITL 1_a.res in Pnma
    1.res
    created by SHELXL-2016/6 at 14:48:19 on 22-Mar-2022
REM Old TITL 1_a.res in Pnma
REM SHELXT solution in Pnma
REM R1 0.158, Rweak 0.005, Alpha 0.018, Orientation as input
REM Formula found by SHELXT: C6 O S2 I2
CELL 0.71073 8.5418 22.7903 10.2937 90 90 90
ZERR 8 0.0007 0.0022 0.001 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,-Z
SYMM 0.5+X,0.5-Y,0.5-Z
SFAC C H I O Pb S
UNIT 48 48 8 16 8 16
ISOR 0.005 0.01 C1 C5 C6
DFIX 3.4 C4 H6c

L.S. 10 0 0
PLAN  22
SIZE 0.19 0.2 0.22
TEMP -123.15
CONF
list 4
MORE -1
BOND $H
fmap 2 53
acta
REM <olex2.extras>
REM <HklSrc "%.\\1.hkl">
REM </olex2.extras>

WGHT    0.025400   15.469900
FVAR       0.12674
PB1   5    0.462834    0.348450    0.368086    11.00000    0.03084    0.02707 =
         0.03781   -0.00701    0.00087   -0.00570
I1    3    0.726865    0.250000    0.296122    10.50000    0.02379    0.01614 =
         0.04329    0.00000    0.01179    0.00000
I2    3    0.422359    0.250000    0.591520    10.50000    0.04866    0.05613 =
         0.02839    0.00000    0.00348    0.00000
S1    6    0.650216    0.543946    0.476071    11.00000    0.01750    0.02529 =
         0.05226   -0.01068   -0.00422    0.00292
S2    6    0.925959    0.634053    0.562245    11.00000    0.02391    0.01541 =
         0.03722   -0.00598   -0.00143    0.00096
O1    4    0.729673    0.417283    0.300496    11.00000    0.04811    0.03546 =
         0.06246    0.00519   -0.01749   -0.00614
O2    4    0.671104    0.395476    0.502126    11.00000    0.02571    0.02984 =
         0.05735   -0.00606    0.00431   -0.00981
C1    1    0.750883    0.421559    0.410304    11.00000    0.01465    0.01333 =
         0.04371   -0.01151   -0.01145   -0.00159
C2    1    0.880569    0.462004    0.460953    11.00000    0.01857    0.01696 =
         0.02638   -0.00553    0.00173   -0.00401
C3    1    0.848098    0.521081    0.486797    11.00000    0.01678    0.01774 =
         0.02329   -0.00101   -0.00043   -0.00214
C4    1    0.967395    0.559506    0.526084    11.00000    0.02428    0.01227 =
         0.02338   -0.00232    0.00047   -0.00075
C5    1    0.632893    0.561968    0.309556    11.00000    0.07331    0.10211 =
         0.06002   -0.00135   -0.01943    0.03850
AFIX 137
H5A   2    0.525983    0.575279    0.291528    11.00000   -1.50000
H5B   2    0.656113    0.527267    0.256735    11.00000   -1.50000
H5C   2    0.706985    0.593343    0.288145    11.00000   -1.50000
AFIX   0
C6    1    1.003448    0.670697    0.420710    11.00000    0.06514    0.03324 =
         0.07032    0.01785    0.01944    0.00572
AFIX 137
H6A   2    1.050504    0.641678    0.362305    11.00000   -1.50000
H6B   2    1.083278    0.699104    0.447541    11.00000   -1.50000
H6C   2    0.918633    0.691203    0.375443    11.00000   -1.50000
AFIX   0
HKLF 4




REM  1_a.res in Pnma
REM R1 =  0.0271 for    2138 Fo > 4sig(Fo)  and  0.0303 for all    2334 data
REM    114 parameters refined using     19 restraints

END

WGHT      0.0254     15.4872

REM Highest difference peak  1.891,  deepest hole -1.899,  1-sigma level  0.184
Q1    1   0.3817  0.3409  0.3593  11.00000  0.05    1.89
Q2    1   0.4862  0.3590  0.2922  11.00000  0.05    1.84
Q3    1   0.7475  0.4396  0.3583  11.00000  0.05    1.24
Q4    1   0.4604  0.2821  0.6175  11.00000  0.05    0.90
Q5    1   0.6948  0.2500  0.2343  10.50000  0.05    0.77
Q6    1   0.7527  0.4215  0.4546  11.00000  0.05    0.74
Q7    1   1.1942  0.6984  0.4230  11.00000  0.05    0.72
Q8    1   0.7658  0.4211  0.2555  11.00000  0.05    0.68
Q9    1   0.7084  0.2500  0.3424  10.50000  0.05    0.63
Q10   1   0.6664  0.4195  0.3000  11.00000  0.05    0.61
Q11   1   0.7200  0.3983  0.3075  11.00000  0.05    0.61
Q12   1   0.5094  0.3182  0.3798  11.00000  0.05    0.61
Q13   1   1.2153  0.6833  0.3814  11.00000  0.05    0.60
Q14   1   0.7654  0.2500  0.3043  10.50000  0.05    0.58
Q15   1   0.4127  0.1976  0.5372  11.00000  0.05    0.54
Q16   1   0.4611  0.2985  0.2698  11.00000  0.05    0.53
Q17   1   0.8962  0.6226  0.3033  11.00000  0.05    0.50
Q18   1   0.4370  0.2942  0.4202  11.00000  0.05    0.49
Q19   1   0.4582  0.4991  0.3480  11.00000  0.05    0.48
Q20   1   0.4443  0.2500  0.4144  10.50000  0.05    0.47
Q21   1   0.9475  0.6624  0.3592  11.00000  0.05    0.46
Q22   1   0.4930  0.2988  0.4730  11.00000  0.05    0.46
;
_shelx_res_checksum              59829
_olex2_submission_special_instructions 'No special instructions were received'
