# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_b15_2018
_database_code_depnum_ccdc_archive 'CCDC 1909477'
loop_
_audit_author_name
_audit_author_address
'Katarzyna Kazimierczuk' ' Gdansk University of Technology'
_audit_update_record             
;
2019-04-11 deposited with the CCDC.	2020-09-15 downloaded from the CCDC.
;

#------------------ AUDIT DETAILS -------------------------------------------#

_audit_creation_date             2019-03-18
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic


#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
catena-[aqua(μ₃-thiophene-2-acetato-κ⁴O:O,O?:O?)\
(thiophene-2-acetato-κ²O,O?)lead(II)]
;
_chemical_formula_moiety         'C12 H12 O5 Pb S2'
_chemical_formula_sum            'C12 H12 O5 Pb S2'
_chemical_formula_weight         507.53
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.2703(13)
_cell_length_b                   9.7597(17)
_cell_length_c                   11.424(2)
_cell_angle_alpha                104.565(15)
_cell_angle_beta                 103.831(15)
_cell_angle_gamma                99.589(14)
_cell_volume                     739.3(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    6173
_cell_measurement_theta_min      2.46
_cell_measurement_theta_max      29.54
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#
_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_exptl_crystal_density_diffrn    2.28
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             476
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 -1 0.0540
0 0 1 0.0350
2 -4 1 0.1260
-1 3 -1 0.1390
1 0 -1 0.0610
-1 0 1 0.0490

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    11.706
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
;
        Numerical  absorption  correction was  performed
        after the  optimization of  the  crystal-shape
        description due to Herrendorf?s method
        [Herrendorf, 1994]
        Herrendorf,  W. (1994).HABITUS, a program for the
        optimization  of  the  crystal description for
 the numerical absorption correction by means of
        suitable, psi scanned reflections;dissertation
        1994,Karlsruhe;extension 1998,Gießen
;
_exptl_absorpt_correction_T_min  0.1613
_exptl_absorpt_correction_T_max  0.4252

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#


_diffrn_source                   'GeniX Mo, 0.05 x 0.05 mm2 microfocus'
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'parabolic x-ray mirror'
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_type            STOE
_diffrn_detector_area_resol_mean 6.67
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_standards_number         0
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_number            8091
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.459
_diffrn_reflns_theta_max         25.497
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_reflns_Friedel_coverage         0
_reflns_number_total             2753
_reflns_number_gt                2565
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'STOE X-AREA'
_computing_cell_refinement       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   mixed

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0551P)²+0.1310P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         2753
_refine_ls_number_parameters     177
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0281
_refine_ls_wR_factor_ref         0.075
_refine_ls_wR_factor_gt          0.0727
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.081
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.802
_refine_diff_density_min         -1.551
_refine_diff_density_rms         0.235

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 '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'

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
C1 C 0.2669(9) 0.0778(7) 0.8114(6) 0.0211(12) Uani 1 1 d . . . . .
H1 H 0.174391 0.093091 0.856632 0.025 Uiso 1 1 calc R U . . .
C2 C 0.2292(10) -0.0266(8) 0.6999(6) 0.0270(14) Uani 1 1 d . . . . .
H2 H 0.106121 -0.09388 0.65772 0.032 Uiso 1 1 calc R U . . .
C3 C 0.3936(9) -0.0254(7) 0.6520(6) 0.0199(12) Uani 1 1 d . . . . .
H3 H 0.391845 -0.091836 0.574824 0.024 Uiso 1 1 calc R U . . .
C4 C 0.5545(9) 0.0822(6) 0.7297(5) 0.0169(12) Uani 1 1 d . . . . .
C5 C 0.7489(9) 0.1247(7) 0.7092(6) 0.0194(12) Uani 1 1 d . . . . .
H5A H 0.764176 0.043474 0.643073 0.023 Uiso 1 1 calc R U . . .
H5B H 0.852564 0.139519 0.78843 0.023 Uiso 1 1 calc R U . . .
C6 C 0.7776(9) 0.2639(7) 0.6693(5) 0.0171(12) Uani 1 1 d . . . . .
C7 C 0.0146(9) 0.2095(7) 0.0773(6) 0.0243(14) Uani 1 1 d . . . . .
H7 H -0.11692 0.157558 0.05829 0.029 Uiso 1 1 calc R U . . .
C8 C 0.0656(10) 0.3367(7) 0.0507(6) 0.0250(13) Uani 1 1 d . . . . .
H8 H -0.03011 0.380503 0.012739 0.03 Uiso 1 1 calc R U . . .
C9 C 0.2778(7) 0.4037(5) 0.0838(4) 0.0054(9) Uiso 1 1 d . . . . .
H9 H 0.340213 0.489969 0.071022 0.006 Uiso 1 1 calc R U . . .
C10 C 0.3701(8) 0.2980(7) 0.1436(5) 0.0165(11) Uani 1 1 d . . . . .
C11 C 0.5874(9) 0.3156(8) 0.1992(6) 0.0215(13) Uani 1 1 d . . . . .
H11A H 0.659729 0.380586 0.162616 0.026 Uiso 1 1 calc R U . . .
H11B H 0.618047 0.219262 0.174533 0.026 Uiso 1 1 calc R U . . .
C12 C 0.6572(8) 0.3783(6) 0.3425(5) 0.0143(11) Uani 1 1 d . . . . .
O1 O 0.9463(6) 0.3270(5) 0.6758(5) 0.0259(10) Uani 1 1 d . . . . .
O2 O 0.6300(6) 0.3101(5) 0.6301(4) 0.0215(9) Uani 1 1 d . . . . .
O3 O 0.8341(6) 0.3933(5) 0.3991(4) 0.0168(8) Uani 1 1 d . . . . .
O4 O 0.5409(6) 0.4150(5) 0.4027(4) 0.0185(9) Uani 1 1 d . . . . .
O5 O 0.7850(6) 0.7314(5) 0.4723(4) 0.0231(9) Uani 1 1 d . . . . .
H5C H 0.87346 0.727639 0.422287 0.035 Uiso 1 1 d R U . . .
H5D H 0.829701 0.831422 0.524065 0.035 Uiso 1 1 d R U . . .
Pb1 Pb 0.79960(2) 0.53644(2) 0.60710(2) 0.01169(10) Uani 1 1 d . . . . .
S1 S 0.5042(2) 0.17987(19) 0.86106(15) 0.0240(3) Uani 1 1 d . . . . .
S2 S 0.2054(3) 0.1536(2) 0.14662(17) 0.0313(4) Uani 1 1 d . . . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
C1 C2 1.351(9) . ?
C1 S1 1.722(6) . ?
C1 H1 0.95 . ?
C2 C3 1.428(9) . ?
C2 H2 0.95 . ?
C3 C4 1.373(9) . ?
C3 H3 0.95 . ?
C4 C5 1.495(8) . ?
C4 S1 1.719(6) . ?
C5 C6 1.536(8) . ?
C5 H5A 0.99 . ?
C5 H5B 0.99 . ?
C6 O1 1.253(8) . ?
C6 O2 1.260(7) . ?
C7 C8 1.365(10) . ?
C7 S2 1.671(7) . ?
C7 H7 0.95 . ?
C8 C9 1.487(8) . ?
C8 H8 0.95 . ?
C9 C10 1.532(7) . ?
C9 H9 0.95 . ?
C10 C11 1.518(8) . ?
C10 S2 1.703(6) . ?
C11 C12 1.519(8) . ?
C11 H11A 0.99 . ?
C11 H11B 0.99 . ?
C12 O4 1.254(7) . ?
C12 O3 1.259(7) . ?
C12 Pb1 2.867(6) . ?
O1 Pb1 2.658(5) . ?
O2 Pb1 2.452(4) . ?
O3 Pb1 2.528(4) . ?
O3 Pb1 2.660(4) 2_766 ?
O4 Pb1 2.482(4) . ?
O4 Pb1 2.579(4) 2_666 ?
O5 Pb1 2.733(5) . ?
O5 H5C 0.9565 . ?
O5 H5D 0.959 . ?

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
C2 C1 S1 111.3(5) . . ?
C2 C1 H1 124.3 . . ?
S1 C1 H1 124.3 . . ?
C1 C2 C3 112.9(6) . . ?
C1 C2 H2 123.5 . . ?
C3 C2 H2 123.5 . . ?
C4 C3 C2 112.7(6) . . ?
C4 C3 H3 123.7 . . ?
C2 C3 H3 123.7 . . ?
C3 C4 C5 128.9(5) . . ?
C3 C4 S1 110.6(4) . . ?
C5 C4 S1 120.4(5) . . ?
C4 C5 C6 113.8(5) . . ?
C4 C5 H5A 108.8 . . ?
C6 C5 H5A 108.8 . . ?
C4 C5 H5B 108.8 . . ?
C6 C5 H5B 108.8 . . ?
H5A C5 H5B 107.7 . . ?
O1 C6 O2 122.3(6) . . ?
O1 C6 C5 119.1(5) . . ?
O2 C6 C5 118.7(5) . . ?
C8 C7 S2 113.7(5) . . ?
C8 C7 H7 123.2 . . ?
S2 C7 H7 123.2 . . ?
C7 C8 C9 116.9(6) . . ?
C7 C8 H8 121.5 . . ?
C9 C8 H8 121.5 . . ?
C8 C9 C10 102.3(4) . . ?
C8 C9 H9 128.9 . . ?
C10 C9 H9 128.9 . . ?
C11 C10 C9 125.3(5) . . ?
C11 C10 S2 120.6(5) . . ?
C9 C10 S2 114.1(4) . . ?
C10 C11 C12 113.2(5) . . ?
C10 C11 H11A 108.9 . . ?
C12 C11 H11A 108.9 . . ?
C10 C11 H11B 108.9 . . ?
C12 C11 H11B 108.9 . . ?
H11A C11 H11B 107.8 . . ?
O4 C12 O3 120.9(5) . . ?
O4 C12 C11 120.5(5) . . ?
O3 C12 C11 118.7(5) . . ?
O4 C12 Pb1 59.7(3) . . ?
O3 C12 Pb1 61.8(3) . . ?
C11 C12 Pb1 171.8(4) . . ?
C6 O1 Pb1 88.6(4) . . ?
C6 O2 Pb1 98.1(4) . . ?
C12 O3 Pb1 92.2(3) . . ?
C12 O3 Pb1 145.8(4) . 2_766 ?
Pb1 O3 Pb1 110.65(15) . 2_766 ?
C12 O4 Pb1 94.5(3) . . ?
C12 O4 Pb1 147.1(4) . 2_666 ?
Pb1 O4 Pb1 116.23(15) . 2_666 ?
Pb1 O5 H5C 112.9 . . ?
Pb1 O5 H5D 113.7 . . ?
H5C O5 H5D 100.6 . . ?
O2 Pb1 O4 74.76(15) . . ?
O2 Pb1 O3 89.88(14) . . ?
O4 Pb1 O3 51.73(12) . . ?
O2 Pb1 O4 79.14(14) . 2_666 ?
O4 Pb1 O4 63.77(15) . 2_666 ?
O3 Pb1 O4 115.12(13) . 2_666 ?
O2 Pb1 O1 50.84(13) . . ?
O4 Pb1 O1 106.42(15) . . ?
O3 Pb1 O1 79.68(14) . . ?
O4 Pb1 O1 128.67(14) 2_666 . ?
O2 Pb1 O3 127.50(13) . 2_766 ?
O4 Pb1 O3 117.81(13) . 2_766 ?
O3 Pb1 O3 69.35(15) . 2_766 ?
O4 Pb1 O3 153.35(14) 2_666 2_766 ?
O1 Pb1 O3 77.62(13) . 2_766 ?
O2 Pb1 O5 146.01(14) . . ?
O4 Pb1 O5 72.65(14) . . ?
O3 Pb1 O5 77.48(14) . . ?
O4 Pb1 O5 78.09(13) 2_666 . ?
O1 Pb1 O5 150.82(13) . . ?
O3 Pb1 O5 77.48(13) 2_766 . ?
O2 Pb1 C12 83.54(16) . . ?
O4 Pb1 C12 25.86(14) . . ?
O3 Pb1 C12 26.03(14) . . ?
O4 Pb1 C12 89.11(14) 2_666 . ?
O1 Pb1 C12 95.15(16) . . ?
O3 Pb1 C12 92.98(14) 2_766 . ?
O5 Pb1 C12 71.24(15) . . ?
C4 S1 C1 92.4(3) . . ?
C7 S2 C10 93.0(3) . . ?

# END of CIF

####################################################################### 
# 
# 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_b16_2018
_database_code_depnum_ccdc_archive 'CCDC 1909478'
loop_
_audit_author_name
_audit_author_address
'Katarzyna Kazimierczuk'
;Gdansk University of Technology
Poland
;
_audit_update_record             
;
2019-04-11 deposited with the CCDC.	2020-09-15 downloaded from the CCDC.
;

#------------------ AUDIT DETAILS -------------------------------------------#

_audit_creation_date             2019-03-20
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#
_chemical_name_systematic        
;
catena-[bis(μ₂-thiophene-3-acetato-κ³O:O,O?)lead(II)]
;
_chemical_formula_moiety         'C12 H10 O4 Pb S2'
_chemical_formula_sum            'C12 H10 O4 Pb S2'
_chemical_formula_weight         489.51
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'I 2/a'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_Int_Tables_number      15
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   16.8469(18)
_cell_length_b                   10.3757(7)
_cell_length_c                   7.8131(9)
_cell_angle_alpha                90
_cell_angle_beta                 101.473(9)
_cell_angle_gamma                90
_cell_volume                     1338.4(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    120
_cell_measurement_reflns_used    5013
_cell_measurement_theta_min      2.47
_cell_measurement_theta_max      29.39
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.08
_exptl_crystal_density_diffrn    2.429
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             912
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.0310
-2 0 3 0.3500
1 1 -4 0.2960
1 2 0 0.1590
-1 -2 0 0.1130
-1 0 0 0.0530

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    12.922
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
;
        Numerical  absorption  correction was  performed
        after the  optimization of  the  crystal-shape
        description due to Herrendorf?s method
        [Herrendorf, 1994]
        Herrendorf,  W. (1994).HABITUS, a program for the
        optimization  of  the  crystal description for
 the numerical absorption correction by means of
        suitable, psi scanned reflections;dissertation
        1994,Karlsruhe;extension 1998,Gießen
;
_exptl_absorpt_correction_T_min  0.0350
_exptl_absorpt_correction_T_max  0.3506

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#
_diffrn_source                   'GeniX Mo, 0.05 x 0.05 mm2 microfocus'
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'parabolic x-ray mirror'
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_type            STOE
_diffrn_detector_area_resol_mean 6.67
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_standards_number         0
_diffrn_reflns_av_R_equivalents  0.0734
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_number            6475
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.467
_diffrn_reflns_theta_max         25.5
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_reflns_Friedel_coverage         0
_reflns_number_total             1252
_reflns_number_gt                1233
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'STOE X-AREA'
_computing_cell_refinement       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   mixed

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0867P)²+0.5223P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         1252
_refine_ls_number_parameters     104
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.04
_refine_ls_R_factor_gt           0.0397
_refine_ls_wR_factor_ref         0.1065
_refine_ls_wR_factor_gt          0.1062
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_restrained_S_all      1.123
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         2.865
_refine_diff_density_min         -1.962
_refine_diff_density_rms         0.298

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 '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'

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 0.25 0.17525(2) 0.5 0.0161(2) Uani 1 2 d S T P . .
S1 S 0.6540(4) 0.3016(5) 0.8861(8) 0.0327(14) Uani 0.617(12) 1 d . . P A 1
C1 C 0.6460(12) 0.431(2) 0.739(3) 0.021(6) Uiso 0.617(12) 1 d . . P A 1
H1 H 0.688998 0.463758 0.689035 0.025 Uiso 0.617(12) 1 calc R U P A 1
S1A S 0.6647(6) 0.4110(8) 0.7497(11) 0.028(2) Uani 0.383(12) 1 d . . P A 2
C1A C 0.631(2) 0.296(3) 0.877(4) 0.021(8) Uiso 0.383(12) 1 d . . P A 2
H1A H 0.663868 0.227167 0.931845 0.025 Uiso 0.383(12) 1 calc R U P A 2
C2 C 0.5688(5) 0.4780(7) 0.7066(9) 0.0236(14) Uani 1 1 d . . . . .
C3 C 0.5159(4) 0.4109(6) 0.7930(9) 0.0199(12) Uani 1 1 d . . . . .
C4 C 0.5540(7) 0.3108(7) 0.8925(14) 0.028(2) Uani 1 1 d . . . . .
C5 C 0.4280(4) 0.4449(7) 0.7797(9) 0.0229(14) Uani 1 1 d . . . . .
H5A H 0.418712 0.53278 0.730407 0.027 Uiso 1 1 calc R U . . .
H5B H 0.416127 0.446784 0.898818 0.027 Uiso 1 1 calc R U . . .
C6 C 0.3691(4) 0.3533(7) 0.6685(9) 0.0171(13) Uani 1 1 d . . . . .
O1 O 0.2962(4) 0.3506(5) 0.6959(7) 0.0214(10) Uani 1 1 d . . . . .
O2 O 0.3892(3) 0.2842(5) 0.5530(6) 0.0222(9) Uani 1 1 d . . . . .
H2 H 0.557(4) 0.557(7) 0.640(10) 0.012(16) Uiso 1 1 d . . . . .
H4 H 0.527(6) 0.269(11) 0.964(13) 0.04(2) Uiso 1 1 d . . . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 O1 2.405(5) . ?
Pb1 O1 2.405(5) 2_556 ?
Pb1 O2 2.562(5) 2_556 ?
Pb1 O2 2.562(5) . ?
Pb1 O1 2.656(5) 8_554 ?
Pb1 O1 2.656(5) 7_556 ?
Pb1 C6 2.849(7) 2_556 ?
Pb1 C6 2.849(7) . ?
S1 C4 1.699(13) . ?
S1 C1 1.76(2) . ?
C1 C2 1.36(2) . ?
C1 H1 0.95 . ?
S1A C1A 1.73(3) . ?
S1A C2 1.729(13) . ?
C1A C4 1.33(3) . ?
C1A H1A 0.95 . ?
C2 C3 1.406(9) . ?
C2 H2 0.97(7) . ?
C3 C4 1.377(12) . ?
C3 C5 1.506(10) . ?
C4 H4 0.90(11) . ?
C5 C6 1.517(9) . ?
C5 H5A 0.99 . ?
C5 H5B 0.99 . ?
C6 O2 1.251(9) . ?
C6 O1 1.288(9) . ?

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
O1 Pb1 O1 81.7(3) . 2_556 ?
O1 Pb1 O2 86.50(18) . 2_556 ?
O1 Pb1 O2 52.67(18) 2_556 2_556 ?
O1 Pb1 O2 52.67(18) . . ?
O1 Pb1 O2 86.50(18) 2_556 . ?
O2 Pb1 O2 127.6(2) 2_556 . ?
O1 Pb1 O1 122.03(18) . 8_554 ?
O1 Pb1 O1 67.8(2) 2_556 8_554 ?
O2 Pb1 O1 108.75(16) 2_556 8_554 ?
O2 Pb1 O1 76.56(16) . 8_554 ?
O1 Pb1 O1 67.8(2) . 7_556 ?
O1 Pb1 O1 122.03(18) 2_556 7_556 ?
O2 Pb1 O1 76.56(16) 2_556 7_556 ?
O2 Pb1 O1 108.75(16) . 7_556 ?
O1 Pb1 O1 168.4(2) 8_554 7_556 ?
O1 Pb1 C6 84.98(19) . 2_556 ?
O1 Pb1 C6 26.7(2) 2_556 2_556 ?
O2 Pb1 C6 26.05(18) 2_556 2_556 ?
O2 Pb1 C6 109.04(19) . 2_556 ?
O1 Pb1 C6 87.51(18) 8_554 2_556 ?
O1 Pb1 C6 100.03(18) 7_556 2_556 ?
O1 Pb1 C6 26.7(2) . . ?
O1 Pb1 C6 84.98(19) 2_556 . ?
O2 Pb1 C6 109.04(19) 2_556 . ?
O2 Pb1 C6 26.05(18) . . ?
O1 Pb1 C6 100.03(18) 8_554 . ?
O1 Pb1 C6 87.51(18) 7_556 . ?
C6 Pb1 C6 99.2(3) 2_556 . ?
C4 S1 C1 91.6(8) . . ?
C2 C1 S1 109.9(14) . . ?
C2 C1 H1 125.1 . . ?
S1 C1 H1 125.1 . . ?
C1A S1A C2 89.3(13) . . ?
C4 C1A S1A 114(3) . . ?
C4 C1A H1A 123 . . ?
S1A C1A H1A 123 . . ?
C1 C2 C3 114.0(11) . . ?
C3 C2 S1A 111.4(6) . . ?
C1 C2 H2 119(4) . . ?
C3 C2 H2 126(4) . . ?
S1A C2 H2 122(4) . . ?
C4 C3 C2 112.1(7) . . ?
C4 C3 C5 123.8(7) . . ?
C2 C3 C5 124.1(7) . . ?
C1A C4 C3 113.0(17) . . ?
C3 C4 S1 112.3(7) . . ?
C1A C4 H4 128(7) . . ?
C3 C4 H4 119(6) . . ?
S1 C4 H4 128(6) . . ?
C3 C5 C6 114.6(6) . . ?
C3 C5 H5A 108.6 . . ?
C6 C5 H5A 108.6 . . ?
C3 C5 H5B 108.6 . . ?
C6 C5 H5B 108.6 . . ?
H5A C5 H5B 107.6 . . ?
O2 C6 O1 120.8(6) . . ?
O2 C6 C5 122.1(6) . . ?
O1 C6 C5 117.1(6) . . ?
O2 C6 Pb1 64.0(4) . . ?
O1 C6 Pb1 57.0(4) . . ?
C5 C6 Pb1 172.4(5) . . ?
C6 O1 Pb1 96.3(4) . . ?
C6 O1 Pb1 127.6(5) . 7_556 ?
Pb1 O1 Pb1 112.2(2) . 7_556 ?
C6 O2 Pb1 89.9(4) . . ?

# END of CIF
