# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 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_exp_12797-5
_database_code_depnum_ccdc_archive 'CCDC 2284064'
loop_
_audit_author_name
_audit_author_address
'Jing Lu'
;Liaocheng University
China
;
_audit_update_record             
;
2023-07-23 deposited with the CCDC.	2023-10-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H4 O8 Pb2 S'
_chemical_formula_weight         674.55

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -4.0753 8.5060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   7.31490(13)
_cell_length_b                   22.3592(3)
_cell_length_c                   7.59111(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.942(2)
_cell_angle_gamma                90.00
_cell_volume                     1151.63(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5515
_cell_measurement_theta_min      6.5850
_cell_measurement_theta_max      70.9830

_exptl_crystal_description       needle
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.891
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1184
_exptl_absorpt_coefficient_mu    58.256
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0542
_exptl_absorpt_correction_T_max  0.0603
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6983
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_sigmaI/netI    0.0357
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         3.95
_diffrn_reflns_theta_max         67.02
_reflns_number_total             2048
_reflns_number_gt                1971
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0785P)²+9.2152P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00071(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2048
_refine_ls_number_parameters     173
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0467
_refine_ls_wR_factor_ref         0.1204
_refine_ls_wR_factor_gt          0.1189
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_restrained_S_all      1.113
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.47238(6) 0.54927(2) -0.21308(7) 0.0259(2) Uani 1 1 d . . .
Pb2 Pb 0.96252(6) 0.56055(2) 0.23859(7) 0.0268(2) Uani 1 1 d . . .
S1 S 0.9792(4) 0.60093(13) 0.7299(4) 0.0266(6) Uani 1 1 d . . .
O3 O 0.6902(14) 0.8665(4) 0.5364(14) 0.041(2) Uani 1 1 d . . .
O4 O 0.9590(15) 0.8316(5) 0.7501(15) 0.046(2) Uani 1 1 d . . .
O7 O 1.0699(12) 0.5742(4) 0.6037(13) 0.036(2) Uani 1 1 d . . .
O8 O 0.6899(11) 0.4904(4) 0.0243(11) 0.0267(17) Uani 1 1 d . . .
H8 H 0.7380 0.4628 -0.0222 0.032 Uiso 1 1 d R . .
O5 O 0.8630(16) 0.5560(4) 0.7834(17) 0.046(3) Uani 1 1 d . . .
O6 O 1.1229(17) 0.6302(4) 0.8897(15) 0.056(3) Uani 1 1 d . . .
O1 O 0.6805(11) 0.5488(4) 0.3427(13) 0.0290(19) Uani 1 1 d . . .
O2 O 0.3952(14) 0.5625(4) 0.3682(16) 0.039(2) Uani 1 1 d . . .
C1 C 0.5595(16) 0.5796(6) 0.3867(17) 0.028(2) Uani 1 1 d . . .
C2 C 0.6220(17) 0.6425(5) 0.4589(18) 0.027(2) Uani 1 1 d . . .
C3 C 0.4928(17) 0.6888(6) 0.3756(19) 0.033(3) Uani 1 1 d . . .
H3 H 0.3694 0.6803 0.2841 0.040 Uiso 1 1 calc R . .
C4 C 0.5446(18) 0.7472(5) 0.426(2) 0.034(3) Uani 1 1 d . . .
H4A H 0.4552 0.7777 0.3708 0.041 Uiso 1 1 calc R . .
C5 C 0.7281(17) 0.7610(5) 0.5595(18) 0.028(2) Uani 1 1 d . . .
C6 C 0.8593(16) 0.7141(5) 0.6509(17) 0.027(2) Uani 1 1 d . . .
H6 H 0.9808 0.7225 0.7456 0.032 Uiso 1 1 calc R . .
C7 C 0.8058(16) 0.6571(5) 0.5986(18) 0.026(2) Uani 1 1 d . . .
C8 C 0.7977(18) 0.8239(5) 0.6175(19) 0.030(3) 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
Pb1 0.0256(3) 0.0302(3) 0.0206(3) 0.00310(17) 0.0073(2) -0.00308(15)
Pb2 0.0239(3) 0.0270(3) 0.0297(4) -0.00050(17) 0.0100(2) 0.00072(15)
S1 0.0291(12) 0.0242(14) 0.0262(15) 0.0015(11) 0.0101(11) 0.0047(10)
O3 0.056(5) 0.019(4) 0.043(6) 0.008(4) 0.013(5) 0.005(4)
O4 0.053(6) 0.039(6) 0.038(6) -0.010(4) 0.008(5) -0.002(4)
O7 0.032(4) 0.048(5) 0.024(5) -0.001(4) 0.008(4) 0.014(4)
O8 0.026(3) 0.034(4) 0.021(4) -0.004(3) 0.009(3) 0.000(3)
O5 0.050(6) 0.041(6) 0.059(7) 0.024(5) 0.034(6) 0.018(4)
O6 0.069(7) 0.033(5) 0.036(6) -0.001(4) -0.014(5) 0.011(5)
O1 0.027(4) 0.033(4) 0.030(5) -0.007(3) 0.014(4) -0.002(3)
O2 0.030(5) 0.043(5) 0.047(6) -0.004(4) 0.017(4) -0.004(4)
C1 0.024(5) 0.037(7) 0.021(6) 0.010(5) 0.005(4) -0.003(5)
C2 0.031(5) 0.024(6) 0.031(7) -0.002(5) 0.018(5) -0.001(4)
C3 0.026(5) 0.035(7) 0.033(7) 0.003(5) 0.005(5) 0.003(5)
C4 0.038(6) 0.023(6) 0.042(8) 0.002(5) 0.017(6) 0.008(5)
C5 0.033(6) 0.031(6) 0.025(6) 0.000(5) 0.017(5) 0.006(5)
C6 0.028(5) 0.033(6) 0.021(6) 0.000(5) 0.010(5) 0.003(5)
C7 0.029(5) 0.022(6) 0.030(6) 0.012(5) 0.014(5) 0.007(4)
C8 0.041(6) 0.019(6) 0.038(7) -0.005(5) 0.023(6) -0.006(5)

_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 O8 2.317(8) . ?
Pb1 O8 2.349(8) 3_665 ?
Pb1 O1 2.490(8) 3_665 ?
Pb1 O3 2.724(8) 4_575 ?
Pb2 O4 2.413(11) 4_575 ?
Pb2 O1 2.484(8) . ?
Pb2 O8 2.581(8) . ?
Pb2 O3 2.589(9) 4_575 ?
Pb2 O7 2.601(9) . ?
Pb2 C8 2.854(11) 4_575 ?
S1 O6 1.433(10) . ?
S1 O5 1.468(10) . ?
S1 O7 1.480(9) . ?
S1 C7 1.799(11) . ?
O3 C8 1.242(15) . ?
O3 Pb2 2.589(9) 4_576 ?
O3 Pb1 2.724(8) 4_576 ?
O4 C8 1.244(16) . ?
O4 Pb2 2.413(11) 4_576 ?
O8 Pb1 2.349(8) 3_665 ?
O1 C1 1.261(15) . ?
O1 Pb1 2.490(8) 3_665 ?
O2 C1 1.218(15) . ?
C1 C2 1.517(17) . ?
C2 C3 1.386(17) . ?
C2 C7 1.405(18) . ?
C3 C4 1.374(18) . ?
C4 C5 1.380(18) . ?
C5 C6 1.415(16) . ?
C5 C8 1.505(16) . ?
C6 C7 1.348(17) . ?
C8 Pb2 2.854(11) 4_576 ?

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
O8 Pb1 O8 70.6(3) . 3_665 ?
O8 Pb1 O1 83.3(3) . 3_665 ?
O8 Pb1 O1 69.8(3) 3_665 3_665 ?
O8 Pb1 O3 78.4(3) . 4_575 ?
O8 Pb1 O3 97.7(3) 3_665 4_575 ?
O1 Pb1 O3 160.6(3) 3_665 4_575 ?
O4 Pb2 O1 94.2(3) 4_575 . ?
O4 Pb2 O8 127.9(3) 4_575 . ?
O1 Pb2 O8 66.3(3) . . ?
O4 Pb2 O3 51.3(3) 4_575 4_575 ?
O1 Pb2 O3 73.1(3) . 4_575 ?
O8 Pb2 O3 76.5(3) . 4_575 ?
O4 Pb2 O7 81.2(3) 4_575 . ?
O1 Pb2 O7 68.2(3) . . ?
O8 Pb2 O7 126.7(3) . . ?
O3 Pb2 O7 114.6(3) 4_575 . ?
O4 Pb2 C8 25.6(3) 4_575 4_575 ?
O1 Pb2 C8 84.1(3) . 4_575 ?
O8 Pb2 C8 102.3(3) . 4_575 ?
O3 Pb2 C8 25.8(3) 4_575 4_575 ?
O7 Pb2 C8 99.2(3) . 4_575 ?
O6 S1 O5 113.3(8) . . ?
O6 S1 O7 111.6(7) . . ?
O5 S1 O7 110.4(6) . . ?
O6 S1 C7 107.0(6) . . ?
O5 S1 C7 105.7(5) . . ?
O7 S1 C7 108.5(6) . . ?
C8 O3 Pb2 89.1(7) . 4_576 ?
C8 O3 Pb1 166.5(9) . 4_576 ?
Pb2 O3 Pb1 95.6(3) 4_576 4_576 ?
C8 O4 Pb2 97.4(8) . 4_576 ?
S1 O7 Pb2 135.0(5) . . ?
Pb1 O8 Pb1 109.4(3) . 3_665 ?
Pb1 O8 Pb2 106.8(3) . . ?
Pb1 O8 Pb2 107.0(3) 3_665 . ?
C1 O1 Pb2 140.8(7) . . ?
C1 O1 Pb1 109.2(7) . 3_665 ?
Pb2 O1 Pb1 105.8(3) . 3_665 ?
O2 C1 O1 124.0(12) . . ?
O2 C1 C2 118.9(11) . . ?
O1 C1 C2 117.1(10) . . ?
C3 C2 C7 117.9(11) . . ?
C3 C2 C1 117.8(11) . . ?
C7 C2 C1 124.3(10) . . ?
C4 C3 C2 120.8(11) . . ?
C3 C4 C5 120.6(11) . . ?
C4 C5 C6 119.3(11) . . ?
C4 C5 C8 123.6(11) . . ?
C6 C5 C8 117.1(11) . . ?
C7 C6 C5 119.1(11) . . ?
C6 C7 C2 122.2(10) . . ?
C6 C7 S1 115.5(9) . . ?
C2 C7 S1 122.2(9) . . ?
O3 C8 O4 121.9(11) . . ?
O3 C8 C5 119.3(11) . . ?
O4 C8 C5 118.8(11) . . ?
O3 C8 Pb2 65.1(6) . 4_576 ?
O4 C8 Pb2 57.0(7) . 4_576 ?
C5 C8 Pb2 175.2(8) . 4_576 ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        67.02
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         3.153
_refine_diff_density_min         -2.010
_refine_diff_density_rms         0.436
