# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_221111_pb-o-sphome_autored
_database_code_depnum_ccdc_archive 'CCDC 2308865'
loop_
_audit_author_name
_audit_author_address
'Ryohei Akiyoshi'
;Kwansei Gakuin University
Japan
;
_audit_update_record             
;
2023-11-18 deposited with the CCDC.	2023-12-27 downloaded from the CCDC.
;
_audit_creation_date             2022-11-12
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C14 H14 O2 Pb S2'
_chemical_formula_sum            'C14 H14 O2 Pb S2'
_chemical_formula_weight         485.56
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H O Pb S'
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'
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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   9.5333(3)
_cell_length_b                   19.6388(5)
_cell_length_c                   7.7462(3)
_cell_angle_alpha                90
_cell_angle_beta                 95.886(3)
_cell_angle_gamma                90
_cell_volume                     1442.62(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    13285
_cell_measurement_temperature    150
_cell_measurement_theta_max      31.3220
_cell_measurement_theta_min      2.0610
_shelx_estimated_absorpt_T_max   0.796
_shelx_estimated_absorpt_T_min   0.166
_exptl_absorpt_coefficient_mu    11.978
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73804
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'whiteish yellow'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.236
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.234
_exptl_crystal_size_mid          0.026
_exptl_crystal_size_min          0.02
_exptl_crystal_size_rad          0.400
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0192
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.939
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            20303
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.184
_diffrn_reflns_theta_min         2.385
_diffrn_ambient_temperature      150
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00  70.00   0.50   30.00    --  -20.00  45.00   0.00  360
  2  ω   -110.00  70.00   0.50   30.00    --  -20.00  45.00  90.00  360
  3  ω   -110.00  70.00   0.50   30.00    --  -20.00  45.00 180.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0138452000
_diffrn_orient_matrix_UB_12      -0.0332847000
_diffrn_orient_matrix_UB_13      -0.0296069000
_diffrn_orient_matrix_UB_21      0.0730098000
_diffrn_orient_matrix_UB_22      0.0076184000
_diffrn_orient_matrix_UB_23      0.0053853000
_diffrn_orient_matrix_UB_31      0.0082482000
_diffrn_orient_matrix_UB_32      -0.0117920000
_diffrn_orient_matrix_UB_33      0.0870096000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3965
_reflns_number_total             4394
_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       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.698
_refine_diff_density_min         -1.088
_refine_diff_density_rms         0.129
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         4394
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0234
_refine_ls_R_factor_gt           0.0194
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0275P)²+0.6404P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0456
_refine_ls_wR_factor_ref         0.0474
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C3(H3), C4(H4), C8(H8), C9(H9), C11(H11), C10(H10)
2.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C)
;
_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 0.58910(2) 0.71954(2) 0.25227(2) 0.01887(4) Uani 1 1 d . . . . .
S2 S 0.39775(7) 0.72393(3) 0.49657(8) 0.01945(11) Uani 1 1 d . . . . .
S1 S 0.64276(6) 0.84770(3) 0.36216(8) 0.02244(12) Uani 1 1 d . . . . .
O2 O 0.43638(19) 0.59682(8) 0.3016(2) 0.0253(4) Uani 1 1 d . . . . .
O1 O 0.8215(2) 0.72731(8) 0.4827(3) 0.0302(4) Uani 1 1 d . . . . .
C5 C 1.0100(3) 0.91239(14) 0.6099(3) 0.0299(6) Uani 1 1 d . . . . .
H5 H 1.049234 0.955189 0.645870 0.036 Uiso 1 1 calc R U . . .
C1 C 0.8123(2) 0.84703(12) 0.4758(3) 0.0195(4) Uani 1 1 d . . . . .
C6 C 0.8756(3) 0.90887(12) 0.5254(3) 0.0251(5) Uani 1 1 d . . . . .
H6 H 0.824762 0.949874 0.500185 0.030 Uiso 1 1 calc R U . . .
C2 C 0.8900(3) 0.78785(11) 0.5212(3) 0.0218(5) Uani 1 1 d . . . . .
C13 C 0.8949(3) 0.66535(13) 0.5324(4) 0.0330(6) Uani 1 1 d . . . . .
H13A H 0.831284 0.626524 0.508349 0.049 Uiso 1 1 calc R U . . .
H13B H 0.926979 0.666767 0.656618 0.049 Uiso 1 1 calc R U . . .
H13C H 0.976457 0.660486 0.465989 0.049 Uiso 1 1 calc R U . . .
C3 C 1.0272(3) 0.79125(14) 0.5994(4) 0.0289(6) Uani 1 1 d . . . . .
H3 H 1.079809 0.750681 0.623473 0.035 Uiso 1 1 calc R U . . .
C4 C 1.0870(3) 0.85361(15) 0.6420(4) 0.0324(6) Uani 1 1 d . . . . .
H4 H 1.181585 0.856089 0.693725 0.039 Uiso 1 1 calc R U . . .
C8 C 0.2679(3) 0.63185(12) 0.6910(3) 0.0234(5) Uani 1 1 d . . . . .
H8 H 0.257253 0.668888 0.767470 0.028 Uiso 1 1 calc R U . . .
C9 C 0.2092(3) 0.56930(14) 0.7240(4) 0.0320(6) Uani 1 1 d . . . . .
H9 H 0.158403 0.563561 0.822261 0.038 Uiso 1 1 calc R U . . .
C11 C 0.3017(3) 0.52262(13) 0.4727(4) 0.0321(6) Uani 1 1 d . . . . .
H11 H 0.313953 0.484977 0.398681 0.039 Uiso 1 1 calc R U . . .
C12 C 0.3605(3) 0.58520(11) 0.4405(3) 0.0212(4) Uani 1 1 d . . . . .
C7 C 0.3421(2) 0.64115(11) 0.5476(3) 0.0193(4) Uani 1 1 d . . . . .
C10 C 0.2247(3) 0.51542(14) 0.6137(4) 0.0386(7) Uani 1 1 d . . . . .
H10 H 0.182178 0.472872 0.634640 0.046 Uiso 1 1 calc R U . . .
C14 C 0.4420(3) 0.54354(13) 0.1768(4) 0.0329(6) Uani 1 1 d . . . . .
H14A H 0.495840 0.559026 0.083001 0.049 Uiso 1 1 calc R U . . .
H14B H 0.346066 0.531548 0.128980 0.049 Uiso 1 1 calc R U . . .
H14C H 0.488074 0.503521 0.232980 0.049 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 S2 2.7612(6) . ?
Pb1 S2 2.7825(6) 4_575 ?
Pb1 S1 2.6893(6) . ?
Pb1 O1 2.703(2) . ?
S2 C7 1.767(2) . ?
S1 C1 1.759(2) . ?
O2 C12 1.375(3) . ?
O2 C14 1.429(3) . ?
O1 C2 1.375(3) . ?
O1 C13 1.436(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.379(4) . ?
C5 C4 1.377(4) . ?
C1 C6 1.393(3) . ?
C1 C2 1.404(3) . ?
C6 H6 0.9500 . ?
C2 C3 1.385(4) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C3 H3 0.9500 . ?
C3 C4 1.377(4) . ?
C4 H4 0.9500 . ?
C8 H8 0.9500 . ?
C8 C9 1.384(3) . ?
C8 C7 1.390(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.377(4) . ?
C11 H11 0.9500 . ?
C11 C12 1.384(3) . ?
C11 C10 1.384(4) . ?
C12 C7 1.399(3) . ?
C10 H10 0.9500 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 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
S2 Pb1 S2 92.547(19) . 4_575 ?
S1 Pb1 S2 82.611(17) . . ?
S1 Pb1 S2 86.643(17) . 4_575 ?
S1 Pb1 O1 67.77(4) . . ?
O1 Pb1 S2 151.72(4) . 4_575 ?
O1 Pb1 S2 95.73(5) . . ?
Pb1 S2 Pb1 93.98(2) . 4_576 ?
C7 S2 Pb1 111.03(8) . . ?
C7 S2 Pb1 113.44(8) . 4_576 ?
C1 S1 Pb1 106.65(8) . . ?
C12 O2 C14 117.83(18) . . ?
C2 O1 Pb1 122.09(15) . . ?
C2 O1 C13 117.8(2) . . ?
C13 O1 Pb1 118.21(16) . . ?
C6 C5 H5 120.2 . . ?
C4 C5 H5 120.2 . . ?
C4 C5 C6 119.7(2) . . ?
C6 C1 S1 118.79(19) . . ?
C6 C1 C2 116.8(2) . . ?
C2 C1 S1 124.46(18) . . ?
C5 C6 C1 122.0(2) . . ?
C5 C6 H6 119.0 . . ?
C1 C6 H6 119.0 . . ?
O1 C2 C1 115.8(2) . . ?
O1 C2 C3 122.9(2) . . ?
C3 C2 C1 121.3(2) . . ?
O1 C13 H13A 109.5 . . ?
O1 C13 H13B 109.5 . . ?
O1 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C2 C3 H3 120.1 . . ?
C4 C3 C2 119.8(2) . . ?
C4 C3 H3 120.1 . . ?
C5 C4 H4 119.9 . . ?
C3 C4 C5 120.2(3) . . ?
C3 C4 H4 119.9 . . ?
C9 C8 H8 119.6 . . ?
C9 C8 C7 120.9(2) . . ?
C7 C8 H8 119.6 . . ?
C8 C9 H9 120.1 . . ?
C10 C9 C8 119.7(2) . . ?
C10 C9 H9 120.1 . . ?
C12 C11 H11 120.3 . . ?
C10 C11 H11 120.3 . . ?
C10 C11 C12 119.4(2) . . ?
O2 C12 C11 122.9(2) . . ?
O2 C12 C7 116.2(2) . . ?
C11 C12 C7 120.8(2) . . ?
C8 C7 S2 119.26(18) . . ?
C8 C7 C12 118.4(2) . . ?
C12 C7 S2 122.10(18) . . ?
C9 C10 C11 120.7(2) . . ?
C9 C10 H10 119.7 . . ?
C11 C10 H10 119.7 . . ?
O2 C14 H14A 109.5 . . ?
O2 C14 H14B 109.5 . . ?
O2 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 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 S2 C7 C8 63.2(2) 4_576 . . . ?
Pb1 S2 C7 C8 167.56(17) . . . . ?
Pb1 S2 C7 C12 -121.96(19) 4_576 . . . ?
Pb1 S2 C7 C12 -17.6(2) . . . . ?
Pb1 S1 C1 C6 170.65(18) . . . . ?
Pb1 S1 C1 C2 -9.4(2) . . . . ?
Pb1 O1 C2 C1 18.0(3) . . . . ?
Pb1 O1 C2 C3 -161.8(2) . . . . ?
S1 C1 C6 C5 -177.9(2) . . . . ?
S1 C1 C2 O1 -4.7(4) . . . . ?
S1 C1 C2 C3 175.1(2) . . . . ?
O2 C12 C7 S2 6.0(3) . . . . ?
O2 C12 C7 C8 -179.1(2) . . . . ?
O1 C2 C3 C4 -176.8(3) . . . . ?
C1 C2 C3 C4 3.4(4) . . . . ?
C6 C5 C4 C3 -3.9(4) . . . . ?
C6 C1 C2 O1 175.3(2) . . . . ?
C6 C1 C2 C3 -4.9(4) . . . . ?
C2 C1 C6 C5 2.1(4) . . . . ?
C2 C3 C4 C5 1.1(4) . . . . ?
C13 O1 C2 C1 -177.8(2) . . . . ?
C13 O1 C2 C3 2.4(4) . . . . ?
C4 C5 C6 C1 2.2(4) . . . . ?
C8 C9 C10 C11 1.7(5) . . . . ?
C9 C8 C7 S2 172.8(2) . . . . ?
C9 C8 C7 C12 -2.2(4) . . . . ?
C11 C12 C7 S2 -172.4(2) . . . . ?
C11 C12 C7 C8 2.4(4) . . . . ?
C12 C11 C10 C9 -1.5(5) . . . . ?
C7 C8 C9 C10 0.2(4) . . . . ?
C10 C11 C12 O2 -178.9(3) . . . . ?
C10 C11 C12 C7 -0.6(4) . . . . ?
C14 O2 C12 C11 6.3(4) . . . . ?
C14 O2 C12 C7 -172.1(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.149
_oxdiff_exptl_absorpt_empirical_full_min 0.575
####################################################################### 
# 
# 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_221110_pb-o-sphome_autored
_database_code_depnum_ccdc_archive 'CCDC 2308867'
loop_
_audit_author_name
_audit_author_address
'Ryohei Akiyoshi'
;Kwansei Gakuin University
Japan
;
_audit_update_record             
;
2023-11-18 deposited with the CCDC.	2023-12-27 downloaded from the CCDC.
;
_audit_creation_date             2022-11-11
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C28 H28 O4 Pb2 S4'
_chemical_formula_sum            'C28 H28 O4 Pb2 S4'
_chemical_formula_weight         971.12
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Pb C14 O2 S2'
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'
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      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 1 2/n 1'
_space_group_name_Hall           '-P 2yac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z-1/2'

_cell_length_a                   7.6715(4)
_cell_length_b                   5.1900(2)
_cell_length_c                   34.4254(13)
_cell_angle_alpha                90
_cell_angle_beta                 90.992(4)
_cell_angle_gamma                90
_cell_volume                     1370.44(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7797
_cell_measurement_temperature    150
_cell_measurement_theta_max      31.2140
_cell_measurement_theta_min      2.3720
_shelx_estimated_absorpt_T_max   0.951
_shelx_estimated_absorpt_T_min   0.460
_exptl_absorpt_coefficient_mu    12.609
_exptl_absorpt_correction_T_max  0.02074
_exptl_absorpt_correction_T_min  0.00670
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark brown'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    2.353
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.073
_exptl_crystal_size_mid          0.064
_exptl_crystal_size_min          0.004
_exptl_crystal_size_rad          0.400
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0197
_diffrn_reflns_av_unetI/netI     0.0169
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            9739
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.364
_diffrn_reflns_theta_min         2.367
_diffrn_ambient_temperature      150
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00  70.00   0.50   30.00    --  -20.00  45.00   0.00  360
  2  ω   -110.00  70.00   0.50   30.00    --  -20.00  45.00  90.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0486904000
_diffrn_orient_matrix_UB_12      0.1026860000
_diffrn_orient_matrix_UB_13      0.0080338000
_diffrn_orient_matrix_UB_21      0.0241881000
_diffrn_orient_matrix_UB_22      -0.0413183000
_diffrn_orient_matrix_UB_23      0.0189744000
_diffrn_orient_matrix_UB_31      0.0747929000
_diffrn_orient_matrix_UB_32      0.0801683000
_diffrn_orient_matrix_UB_33      -0.0004888000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2229
_reflns_number_total             2785
_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       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.995
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.212
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         2785
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0344
_refine_ls_restrained_S_all      1.122
_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)+(0.0519P)²+1.1143P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0855
_refine_ls_wR_factor_ref         0.0906
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C3(H3), C5(H5), C6(H6), C9(H9), C12(H12), C11(H11)
2.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C13(H13A,H13B,H13C)
;
_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
Pb2 Pb 0.250000 0.33647(5) 0.750000 0.03454(12) Uani 1 2 d S T P . .
Pb1 Pb 0.750000 0.85310(5) 0.750000 0.03351(12) Uani 1 2 d S T P . .
S1 S 0.60715(19) 0.4049(3) 0.71468(4) 0.0321(3) Uani 1 1 d . . . . .
S2 S 0.1073(2) -0.1081(3) 0.71366(4) 0.0337(3) Uani 1 1 d . . . . .
O2 O -0.0732(5) -0.0117(8) 0.54592(11) 0.0360(8) Uani 1 1 d . . . . .
O1 O 0.4265(5) 0.4917(7) 0.54683(11) 0.0353(8) Uani 1 1 d . . . . .
C2 C 0.4449(7) 0.2487(9) 0.64732(15) 0.0330(11) Uani 1 1 d . . . . .
H2 H 0.404514 0.108367 0.662430 0.040 Uiso 1 1 calc R U . . .
C7 C 0.0518(7) -0.0658(10) 0.66380(15) 0.0303(11) Uani 1 1 d . . . . .
C8 C 0.1102(7) -0.2446(9) 0.63676(15) 0.0326(11) Uani 1 1 d . . . . .
H8 H 0.181087 -0.384667 0.645159 0.039 Uiso 1 1 calc R U . . .
C1 C 0.5475(7) 0.4380(10) 0.66489(15) 0.0289(10) Uani 1 1 d . . . . .
C3 C 0.4005(7) 0.2611(9) 0.60817(15) 0.0323(10) Uani 1 1 d . . . . .
H3 H 0.328853 0.131801 0.596620 0.039 Uiso 1 1 calc R U . . .
C5 C 0.5651(7) 0.6531(8) 0.60314(16) 0.0321(12) Uani 1 1 d . . . . .
H5 H 0.607146 0.791518 0.587853 0.038 Uiso 1 1 calc R U . . .
C10 C -0.0372(7) -0.0173(10) 0.58519(15) 0.0308(11) Uani 1 1 d . . . . .
C6 C 0.6073(8) 0.6416(8) 0.64207(17) 0.0334(12) Uani 1 1 d . . . . .
H6 H 0.677519 0.772741 0.653548 0.040 Uiso 1 1 calc R U . . .
C9 C 0.0664(7) -0.2200(10) 0.59812(15) 0.0329(11) Uani 1 1 d . . . . .
H9 H 0.107411 -0.343215 0.580029 0.040 Uiso 1 1 calc R U . . .
C12 C -0.0506(7) 0.1388(8) 0.65054(17) 0.0324(12) Uani 1 1 d . . . . .
H12 H -0.090022 0.263838 0.668529 0.039 Uiso 1 1 calc R U . . .
C4 C 0.4616(7) 0.4642(10) 0.58601(16) 0.0304(11) Uani 1 1 d . . . . .
C11 C -0.0958(7) 0.1633(8) 0.61157(17) 0.0331(12) Uani 1 1 d . . . . .
H11 H -0.166480 0.303152 0.602999 0.040 Uiso 1 1 calc R U . . .
C14 C -0.1659(8) 0.2062(10) 0.53108(17) 0.0413(13) Uani 1 1 d . . . . .
H14A H -0.168666 0.199836 0.502627 0.062 Uiso 1 1 calc R U . . .
H14B H -0.107440 0.364480 0.539726 0.062 Uiso 1 1 calc R U . . .
H14C H -0.285411 0.203932 0.540700 0.062 Uiso 1 1 calc R U . . .
C13 C 0.3378(8) 0.2835(10) 0.52781(16) 0.0407(12) Uani 1 1 d . . . . .
H13A H 0.331865 0.316248 0.499778 0.061 Uiso 1 1 calc R U . . .
H13B H 0.219434 0.268925 0.537849 0.061 Uiso 1 1 calc R U . . .
H13C H 0.401224 0.122579 0.532752 0.061 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
Pb2 S1 3.0375(14) 2_556 ?
Pb2 S1 3.0375(15) . ?
Pb2 S2 2.8354(15) . ?
Pb2 S2 2.8354(14) 2_556 ?
Pb1 S1 2.8363(14) . ?
Pb1 S1 2.8363(14) 2_656 ?
Pb1 S2 3.0393(15) 2_566 ?
Pb1 S2 3.0393(15) 1_665 ?
S1 C1 1.775(5) . ?
S2 C7 1.775(5) . ?
O2 C10 1.375(6) . ?
O2 C14 1.426(6) . ?
O1 C4 1.378(6) . ?
O1 C13 1.430(6) . ?
C2 H2 0.9500 . ?
C2 C1 1.391(7) . ?
C2 C3 1.386(7) . ?
C7 C8 1.394(7) . ?
C7 C12 1.393(7) . ?
C8 H8 0.9500 . ?
C8 C9 1.372(7) . ?
C1 C6 1.399(7) . ?
C3 H3 0.9500 . ?
C3 C4 1.388(7) . ?
C5 H5 0.9500 . ?
C5 C6 1.375(8) . ?
C5 C4 1.387(7) . ?
C10 C9 1.387(7) . ?
C10 C11 1.385(7) . ?
C6 H6 0.9500 . ?
C9 H9 0.9500 . ?
C12 H12 0.9500 . ?
C12 C11 1.386(8) . ?
C11 H11 0.9500 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 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
S1 Pb2 S1 166.58(5) . 2_556 ?
S2 Pb2 S1 105.22(4) . . ?
S2 Pb2 S1 105.22(4) 2_556 2_556 ?
S2 Pb2 S1 85.85(4) 2_556 . ?
S2 Pb2 S1 85.85(4) . 2_556 ?
S2 Pb2 S2 71.08(6) 2_556 . ?
S1 Pb1 S1 69.79(6) 2_656 . ?
S1 Pb1 S2 102.85(4) . 1_665 ?
S1 Pb1 S2 83.47(4) 2_656 1_665 ?
S1 Pb1 S2 83.47(4) . 2_566 ?
S1 Pb1 S2 102.85(4) 2_656 2_566 ?
S2 Pb1 S2 172.40(5) 2_566 1_665 ?
Pb1 S1 Pb2 105.59(4) . . ?
C1 S1 Pb2 100.29(17) . . ?
C1 S1 Pb1 115.20(18) . . ?
Pb2 S2 Pb1 102.50(4) . 1_445 ?
C7 S2 Pb2 114.24(18) . . ?
C7 S2 Pb1 101.73(18) . 1_445 ?
C10 O2 C14 117.3(4) . . ?
C4 O1 C13 117.0(4) . . ?
C1 C2 H2 119.4 . . ?
C3 C2 H2 119.4 . . ?
C3 C2 C1 121.2(5) . . ?
C8 C7 S2 119.3(4) . . ?
C12 C7 S2 122.4(4) . . ?
C12 C7 C8 118.3(5) . . ?
C7 C8 H8 119.7 . . ?
C9 C8 C7 120.6(5) . . ?
C9 C8 H8 119.7 . . ?
C2 C1 S1 119.1(4) . . ?
C2 C1 C6 118.6(5) . . ?
C6 C1 S1 122.3(4) . . ?
C2 C3 H3 120.3 . . ?
C2 C3 C4 119.4(5) . . ?
C4 C3 H3 120.3 . . ?
C6 C5 H5 119.8 . . ?
C6 C5 C4 120.5(5) . . ?
C4 C5 H5 119.8 . . ?
O2 C10 C9 115.8(5) . . ?
O2 C10 C11 124.6(5) . . ?
C11 C10 C9 119.5(5) . . ?
C1 C6 H6 119.8 . . ?
C5 C6 C1 120.4(5) . . ?
C5 C6 H6 119.8 . . ?
C8 C9 C10 120.7(5) . . ?
C8 C9 H9 119.6 . . ?
C10 C9 H9 119.6 . . ?
C7 C12 H12 119.4 . . ?
C11 C12 C7 121.2(5) . . ?
C11 C12 H12 119.4 . . ?
O1 C4 C3 123.7(5) . . ?
O1 C4 C5 116.3(5) . . ?
C5 C4 C3 120.0(5) . . ?
C10 C11 C12 119.6(5) . . ?
C10 C11 H11 120.2 . . ?
C12 C11 H11 120.2 . . ?
O2 C14 H14A 109.5 . . ?
O2 C14 H14B 109.5 . . ?
O2 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O1 C13 H13A 109.5 . . ?
O1 C13 H13B 109.5 . . ?
O1 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 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 S1 C1 C2 -54.2(4) . . . . ?
Pb2 S1 C1 C6 129.1(4) . . . . ?
Pb2 S2 C7 C8 129.8(4) . . . . ?
Pb2 S2 C7 C12 -51.0(5) . . . . ?
Pb1 S1 C1 C2 -167.0(3) . . . . ?
Pb1 S1 C1 C6 16.3(5) . . . . ?
Pb1 S2 C7 C8 -120.6(4) 1_445 . . . ?
Pb1 S2 C7 C12 58.6(4) 1_445 . . . ?
S1 C1 C6 C5 176.7(4) . . . . ?
S2 C7 C8 C9 178.6(4) . . . . ?
S2 C7 C12 C11 -178.3(4) . . . . ?
O2 C10 C9 C8 -179.9(5) . . . . ?
O2 C10 C11 C12 -179.7(5) . . . . ?
C2 C1 C6 C5 0.0(8) . . . . ?
C2 C3 C4 O1 179.1(5) . . . . ?
C2 C3 C4 C5 -0.4(8) . . . . ?
C7 C8 C9 C10 -0.1(8) . . . . ?
C7 C12 C11 C10 -0.6(8) . . . . ?
C8 C7 C12 C11 0.9(8) . . . . ?
C1 C2 C3 C4 0.9(8) . . . . ?
C3 C2 C1 S1 -177.5(4) . . . . ?
C3 C2 C1 C6 -0.7(8) . . . . ?
C6 C5 C4 O1 -179.9(5) . . . . ?
C6 C5 C4 C3 -0.3(8) . . . . ?
C9 C10 C11 C12 -0.2(8) . . . . ?
C12 C7 C8 C9 -0.6(8) . . . . ?
C4 C5 C6 C1 0.5(8) . . . . ?
C11 C10 C9 C8 0.5(8) . . . . ?
C14 O2 C10 C9 -174.5(5) . . . . ?
C14 O2 C10 C11 5.1(8) . . . . ?
C13 O1 C4 C3 -6.8(7) . . . . ?
C13 O1 C4 C5 172.8(5) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.592
_oxdiff_exptl_absorpt_empirical_full_min 0.760
####################################################################### 
# 
# 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_ak31-4_autored
_database_code_depnum_ccdc_archive 'CCDC 2308866'
loop_
_audit_author_name
_audit_author_address
'Ryohei Akiyoshi'
;Kwansei Gakuin University
Japan
;
_audit_update_record             
;
2023-11-18 deposited with the CCDC.	2023-12-27 downloaded from the CCDC.
;
_audit_creation_date             2022-11-07
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C14 H14 O2 Pb S2'
_chemical_formula_sum            'C14 H14 O2 Pb S2'
_chemical_formula_weight         485.56
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H S O Pb'
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'
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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   4.1327(2)
_cell_length_b                   31.0738(11)
_cell_length_c                   11.0299(4)
_cell_angle_alpha                90
_cell_angle_beta                 95.467(4)
_cell_angle_gamma                90
_cell_volume                     1410.00(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8790
_cell_measurement_temperature    150
_cell_measurement_theta_max      31.2270
_cell_measurement_theta_min      1.9920
_shelx_estimated_absorpt_T_max   0.887
_shelx_estimated_absorpt_T_min   0.374
_exptl_absorpt_coefficient_mu    12.255
_exptl_absorpt_correction_T_max  0.02129
_exptl_absorpt_correction_T_min  0.00705
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.287
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_crystal_size_rad          0.400
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10000
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.363
_diffrn_reflns_theta_min         2.622
_diffrn_ambient_temperature      150
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00  70.00   0.50   45.00    --  -20.00  45.00   0.00  360
  2  ω   -110.00  70.00   0.50   45.00    --  -20.00  45.00  90.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0457151000
_diffrn_orient_matrix_UB_12      -0.0212803000
_diffrn_orient_matrix_UB_13      0.0140562000
_diffrn_orient_matrix_UB_21      -0.0296867000
_diffrn_orient_matrix_UB_22      -0.0046896000
_diffrn_orient_matrix_UB_23      -0.0630593000
_diffrn_orient_matrix_UB_31      0.1635302000
_diffrn_orient_matrix_UB_32      -0.0068131000
_diffrn_orient_matrix_UB_33      -0.0008996000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2439
_reflns_number_total             2758
_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       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         2.221
_refine_diff_density_min         -1.031
_refine_diff_density_rms         0.199
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         2758
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0370
_refine_ls_restrained_S_all      1.079
_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)+(0.0604P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0874
_refine_ls_wR_factor_ref         0.0908
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C10(H10), C12(H12), C2(H2), C8(H8), C3(H3), C4(H4), C6(H6)
2.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C13(H13A,H13B,H13C)
;
_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 0.12350(6) 0.55987(2) 0.43223(2) 0.03709(12) Uani 1 1 d . . . . .
S1 S 0.6164(4) 0.57438(5) 0.26212(13) 0.0377(3) Uani 1 1 d . . . . .
S2 S 0.2910(4) 0.47803(5) 0.38792(13) 0.0370(3) Uani 1 1 d . . . . .
O2 O -0.1807(12) 0.34250(15) 0.1954(4) 0.0483(11) Uani 1 1 d . . . . .
O1 O 0.6406(13) 0.72202(14) 0.4849(4) 0.0502(11) Uani 1 1 d . . . . .
C11 C -0.235(2) 0.4517(2) 0.0696(6) 0.0474(15) Uani 1 1 d . . . . .
H11 H -0.324595 0.466960 -0.000362 0.057 Uiso 1 1 calc R U . . .
C10 C -0.2849(17) 0.4076(2) 0.0757(6) 0.0432(14) Uani 1 1 d . . . . .
H10 H -0.406643 0.392822 0.011272 0.052 Uiso 1 1 calc R U . . .
C9 C -0.1532(17) 0.3858(2) 0.1780(6) 0.0419(14) Uani 1 1 d . . . . .
C12 C -0.0599(17) 0.4740(2) 0.1614(5) 0.0430(14) Uani 1 1 d . . . . .
H12 H -0.024654 0.504019 0.154256 0.052 Uiso 1 1 calc R U . . .
C7 C 0.0634(16) 0.4520(2) 0.2639(5) 0.0376(13) Uani 1 1 d . . . . .
C2 C 0.8465(16) 0.6511(2) 0.1846(6) 0.0439(14) Uani 1 1 d . . . . .
H2 H 0.897102 0.635506 0.114727 0.053 Uiso 1 1 calc R U . . .
C8 C 0.0239(16) 0.4074(2) 0.2722(6) 0.0384(13) Uani 1 1 d . . . . .
H8 H 0.117218 0.392173 0.341514 0.046 Uiso 1 1 calc R U . . .
C1 C 0.7056(15) 0.63035(19) 0.2770(5) 0.0364(12) Uani 1 1 d . . . . .
C14 C -0.386(2) 0.3190(2) 0.1051(7) 0.0537(18) Uani 1 1 d . . . . .
H14A H -0.289713 0.319730 0.027264 0.080 Uiso 1 1 calc R U . . .
H14B H -0.601767 0.332328 0.095151 0.080 Uiso 1 1 calc R U . . .
H14C H -0.405302 0.289121 0.131565 0.080 Uiso 1 1 calc R U . . .
C3 C 0.9140(17) 0.6947(2) 0.1939(7) 0.0469(15) Uani 1 1 d . . . . .
H3 H 1.008115 0.708957 0.129586 0.056 Uiso 1 1 calc R U . . .
C4 C 0.8461(19) 0.7178(2) 0.2956(7) 0.0508(17) Uani 1 1 d . . . . .
H4 H 0.894779 0.747635 0.301965 0.061 Uiso 1 1 calc R U . . .
C6 C 0.6346(16) 0.65315(19) 0.3799(6) 0.0390(13) Uani 1 1 d . . . . .
H6 H 0.538398 0.638982 0.443847 0.047 Uiso 1 1 calc R U . . .
C5 C 0.7057(16) 0.6967(2) 0.3881(6) 0.0426(14) Uani 1 1 d . . . . .
C13 C 0.482(2) 0.7025(2) 0.5786(6) 0.0513(17) Uani 1 1 d . . . . .
H13A H 0.292198 0.686532 0.542889 0.077 Uiso 1 1 calc R U . . .
H13B H 0.412236 0.724790 0.633369 0.077 Uiso 1 1 calc R U . . .
H13C H 0.632384 0.682742 0.624591 0.077 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 S1 2.9329(16) . ?
Pb1 S1 2.7141(16) 1_455 ?
Pb1 S2 2.6926(15) . ?
Pb1 S2 2.9839(16) 3_566 ?
S1 C1 1.782(6) . ?
S2 C7 1.779(6) . ?
O2 C9 1.365(8) . ?
O2 C14 1.442(8) . ?
O1 C5 1.373(8) . ?
O1 C13 1.411(9) . ?
C11 H11 0.9500 . ?
C11 C10 1.387(9) . ?
C11 C12 1.374(10) . ?
C10 H10 0.9500 . ?
C10 C9 1.383(9) . ?
C9 C8 1.386(9) . ?
C12 H12 0.9500 . ?
C12 C7 1.375(9) . ?
C7 C8 1.399(8) . ?
C2 H2 0.9500 . ?
C2 C1 1.381(9) . ?
C2 C3 1.386(9) . ?
C8 H8 0.9500 . ?
C1 C6 1.393(9) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C3 H3 0.9500 . ?
C3 C4 1.383(10) . ?
C4 H4 0.9500 . ?
C4 C5 1.386(10) . ?
C6 H6 0.9500 . ?
C6 C5 1.386(9) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 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
S1 Pb1 S1 94.00(4) 1_455 . ?
S1 Pb1 S2 94.06(4) 1_455 3_566 ?
S1 Pb1 S2 164.52(4) . 3_566 ?
S2 Pb1 S1 79.79(5) . . ?
S2 Pb1 S1 103.08(5) . 1_455 ?
S2 Pb1 S2 85.52(5) . 3_566 ?
Pb1 S1 Pb1 94.00(4) 1_655 . ?
C1 S1 Pb1 87.7(2) . 1_655 ?
C1 S1 Pb1 104.0(2) . . ?
Pb1 S2 Pb1 94.49(5) . 3_566 ?
C7 S2 Pb1 116.3(2) . . ?
C7 S2 Pb1 92.1(2) . 3_566 ?
C9 O2 C14 116.9(5) . . ?
C5 O1 C13 117.5(5) . . ?
C10 C11 H11 119.0 . . ?
C12 C11 H11 119.0 . . ?
C12 C11 C10 122.1(6) . . ?
C11 C10 H10 120.8 . . ?
C9 C10 C11 118.4(6) . . ?
C9 C10 H10 120.8 . . ?
O2 C9 C10 124.5(6) . . ?
O2 C9 C8 114.7(6) . . ?
C10 C9 C8 120.8(6) . . ?
C11 C12 H12 120.5 . . ?
C11 C12 C7 119.0(6) . . ?
C7 C12 H12 120.5 . . ?
C12 C7 S2 122.3(5) . . ?
C12 C7 C8 120.5(6) . . ?
C8 C7 S2 117.1(5) . . ?
C1 C2 H2 120.1 . . ?
C1 C2 C3 119.9(6) . . ?
C3 C2 H2 120.1 . . ?
C9 C8 C7 119.2(6) . . ?
C9 C8 H8 120.4 . . ?
C7 C8 H8 120.4 . . ?
C2 C1 S1 119.1(5) . . ?
C2 C1 C6 120.0(6) . . ?
C6 C1 S1 120.9(5) . . ?
O2 C14 H14A 109.5 . . ?
O2 C14 H14B 109.5 . . ?
O2 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C2 C3 H3 119.6 . . ?
C4 C3 C2 120.8(6) . . ?
C4 C3 H3 119.6 . . ?
C3 C4 H4 120.5 . . ?
C3 C4 C5 118.9(6) . . ?
C5 C4 H4 120.5 . . ?
C1 C6 H6 120.3 . . ?
C5 C6 C1 119.3(6) . . ?
C5 C6 H6 120.3 . . ?
O1 C5 C4 115.3(6) . . ?
O1 C5 C6 123.7(6) . . ?
C6 C5 C4 121.0(6) . . ?
O1 C13 H13A 109.5 . . ?
O1 C13 H13B 109.5 . . ?
O1 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 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 C1 C2 -159.5(5) . . . . ?
Pb1 S1 C1 C2 107.0(5) 1_655 . . . ?
Pb1 S1 C1 C6 20.5(6) . . . . ?
Pb1 S1 C1 C6 -73.1(5) 1_655 . . . ?
Pb1 S2 C7 C12 128.9(5) 3_566 . . . ?
Pb1 S2 C7 C12 32.9(6) . . . . ?
Pb1 S2 C7 C8 -53.5(5) 3_566 . . . ?
Pb1 S2 C7 C8 -149.6(4) . . . . ?
S1 C1 C6 C5 -179.7(5) . . . . ?
S2 C7 C8 C9 179.7(5) . . . . ?
O2 C9 C8 C7 -179.3(6) . . . . ?
C11 C10 C9 O2 -179.3(6) . . . . ?
C11 C10 C9 C8 0.1(10) . . . . ?
C11 C12 C7 S2 -179.7(6) . . . . ?
C11 C12 C7 C8 2.9(10) . . . . ?
C10 C11 C12 C7 -1.5(11) . . . . ?
C10 C9 C8 C7 1.2(10) . . . . ?
C12 C11 C10 C9 0.0(11) . . . . ?
C12 C7 C8 C9 -2.7(9) . . . . ?
C2 C1 C6 C5 0.2(10) . . . . ?
C2 C3 C4 C5 -0.6(11) . . . . ?
C1 C2 C3 C4 0.9(11) . . . . ?
C1 C6 C5 O1 179.0(6) . . . . ?
C1 C6 C5 C4 0.0(10) . . . . ?
C14 O2 C9 C10 -5.7(9) . . . . ?
C14 O2 C9 C8 174.8(6) . . . . ?
C3 C2 C1 S1 179.2(5) . . . . ?
C3 C2 C1 C6 -0.7(10) . . . . ?
C3 C4 C5 O1 -178.9(6) . . . . ?
C3 C4 C5 C6 0.2(11) . . . . ?
C13 O1 C5 C4 176.8(6) . . . . ?
C13 O1 C5 C6 -2.3(10) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.506
_oxdiff_exptl_absorpt_empirical_full_min 0.543
