# Electronic Supplementary Material (ESI) for RSC Advances.
# 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_ip2-2697_d7
_database_code_depnum_ccdc_archive 'CCDC 2350383'
loop_
_audit_author_name
_audit_author_address
'Daniel Fuhrmann'
;University of Leipzig
Germany
;
_audit_update_record             
;
2024-04-23 deposited with the CCDC.	2024-07-03 downloaded from the CCDC.
;

_audit_creation_date             2022-07-12T22:47:23-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

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

_chemical_formula_sum            'C30 H24 Br4 N8 O2 Pb2'
_chemical_formula_weight         1262.59

#----------------------------------------------------------------------------#
#                   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                   7.7597(5)
_cell_length_b                   9.1203(5)
_cell_length_c                   12.5054(7)
_cell_angle_alpha                102.924(4)
_cell_angle_beta                 97.329(4)
_cell_angle_gamma                97.611(5)
_cell_volume                     843.60(9)
_cell_formula_units_Z            1
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    12201
_cell_measurement_theta_min      2.68
_cell_measurement_theta_max      28.25

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

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.236
_exptl_crystal_size_mid          0.153
_exptl_crystal_size_min          0.058
_exptl_crystal_density_diffrn    2.485
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             580

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

_exptl_absorpt_coefficient_mu    14.78
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270. Afterwards scaling of
reflection intensities was performed within STOE LANA. J. Koziskova, F. Hahn,
J. Richter, J. Kozisek, Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136-140.
;
_exptl_absorpt_correction_T_min  0.0841
_exptl_absorpt_correction_T_max  0.3416
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2 -1 4 0.0250
2 1 -4 0.0330
4 -1 -4 0.0400
3 0 4 0.0480
0 -4 -1 0.1230
-2 -4 -4 0.1140
-3 0 -4 0.1160
-1 4 0 0.1130


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

_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'

_diffrn_detector                 'image plate (34 cm diameter / schwenk)'
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_detector_area_resol_mean 6.67

_diffrn_source                   
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_type              ?
_diffrn_radiation_probe          x-ray
_diffrn_source_target            ?
_diffrn_source_voltage           50
_diffrn_source_current           40.000
_diffrn_source_power             2.000
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_collimation    '0.5 mm diameter, multiple pinhole'

_diffrn_ambient_temperature      200

_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_measurement_details      
; 208 frames, detector distance = 110 mm
;
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_unetI/netI     0.0446
_diffrn_reflns_number            6695
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.684
_diffrn_reflns_theta_max         26.997
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_reflns_Friedel_coverage         0
_reflns_number_total             3657
_reflns_number_gt                3227
_reflns_threshold_expression     'I > 2σ(I)'

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

_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_data_collection       
;
X-Area WinXpose 2.0.22.0 (STOE, 2016)
;
_computing_cell_refinement       
;
X-Area Recipe 1.36.0.0 (STOE, 2020)
;
_computing_data_reduction        
;
X-Area Integrate 1.78.3.0 (STOE, 2020)
X-Area LANA 1.83.8.0 (STOE, 2020)
;
_computing_publication_material  
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.90, Darmstadt 2020
;

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

_atom_sites_solution_primary     direct
_atom_sites_solution_hydrogens   geom

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

_shelx_SHELXL_version_number     2018/3
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0729P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         3657
_refine_ls_number_parameters     209
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0363
_refine_ls_wR_factor_ref         0.1016
_refine_ls_wR_factor_gt          0.0988
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.011
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.88
_refine_diff_density_min         -2.355
_refine_diff_density_rms         0.213

#----------------------------------------------------------------------------#
#                   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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 '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'
Br Br -0.2901 2.4595 '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 0.4574(9) 0.5390(8) 0.1677(5) 0.0341(14) Uani 1 1 d . . . . .
H1 H 0.398144 0.591243 0.120397 0.041 Uiso 1 1 calc R U . . .
C2 C 0.4805(10) 0.3923(8) 0.1230(5) 0.0368(15) Uani 1 1 d . . . . .
H2 H 0.438854 0.345045 0.046619 0.044 Uiso 1 1 calc R U . . .
C3 C 0.5658(10) 0.3140(7) 0.1916(6) 0.0361(15) Uani 1 1 d . . . . .
H3 H 0.583324 0.212504 0.162725 0.043 Uiso 1 1 calc R U . . .
C4 C 0.6250(9) 0.3867(7) 0.3027(5) 0.0300(13) Uani 1 1 d . . . . .
H4 H 0.682259 0.335576 0.351656 0.036 Uiso 1 1 calc R U . . .
C5 C 0.5983(8) 0.5370(7) 0.3411(5) 0.0276(12) Uani 1 1 d . . . . .
C6 C 0.6638(9) 0.6187(7) 0.4588(5) 0.0278(12) Uani 1 1 d . . . . .
C7 C 0.7827(9) 0.7720(7) 0.6628(5) 0.0326(13) Uani 1 1 d . . . . .
H7 H 0.832577 0.829545 0.735866 0.039 Uiso 1 1 calc R U . . .
C8 C 0.8190(8) 0.6234(7) 0.6261(5) 0.0263(12) Uani 1 1 d . . . . .
C9 C 0.9170(8) 0.5461(7) 0.6997(5) 0.0257(12) Uani 1 1 d . . . . .
C10 C 0.9806(9) 0.6173(7) 0.8126(5) 0.0314(13) Uani 1 1 d . . . . .
H10 H 0.96934 0.720521 0.84142 0.038 Uiso 1 1 calc R U . . .
C11 C 1.0589(10) 0.5380(8) 0.8810(6) 0.0366(15) Uani 1 1 d . . . . .
H11 H 1.099506 0.586213 0.957316 0.044 Uiso 1 1 calc R U . . .
C12 C 1.0792(9) 0.3867(8) 0.8391(5) 0.0317(13) Uani 1 1 d . . . . .
C13 C 1.0220(9) 0.3156(7) 0.7270(5) 0.0313(13) Uani 1 1 d . . . . .
H13 H 1.038288 0.213826 0.697666 0.038 Uiso 1 1 calc R U . . .
C14 C 0.9403(8) 0.3968(7) 0.6585(5) 0.0288(12) Uani 1 1 d . . . . .
H14 H 0.899799 0.348824 0.582171 0.035 Uiso 1 1 calc R U . . .
C15 C 1.1611(11) 0.1571(8) 0.8805(6) 0.0409(16) Uani 1 1 d . . . . .
H15A H 1.042602 0.101939 0.846658 0.061 Uiso 1 1 calc R U . . .
H15B H 1.202581 0.12072 0.945706 0.061 Uiso 1 1 calc R U . . .
H15C H 1.241478 0.139157 0.826347 0.061 Uiso 1 1 calc R U . . .
N1 N 0.5141(7) 0.6123(6) 0.2744(4) 0.0301(11) Uani 1 1 d . . . . .
N2 N 0.6159(8) 0.7546(6) 0.4934(4) 0.0317(11) Uani 1 1 d . . . . .
N3 N 0.6821(8) 0.8329(6) 0.5987(5) 0.0357(13) Uani 1 1 d . . . . .
N4 N 0.7605(7) 0.5478(6) 0.5216(4) 0.0271(10) Uani 1 1 d . . . . .
O1 O 1.1560(7) 0.3196(6) 0.9145(4) 0.0373(11) Uani 1 1 d . . . . .
Pb1 Pb 0.41871(3) 0.87710(2) 0.34847(2) 0.03089(11) Uani 1 1 d . . . . .
Br1 Br 0.75352(10) 1.05532(7) 0.39726(6) 0.03880(17) Uani 1 1 d . . . . .
Br2 Br 0.34465(10) 0.90056(8) 0.12610(5) 0.04066(18) 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 N1 1.339(8) . ?
C1 C2 1.375(9) . ?
C2 C3 1.391(9) . ?
C3 C4 1.388(9) . ?
C4 C5 1.399(9) . ?
C5 N1 1.353(7) . ?
C5 C6 1.483(8) . ?
C6 N2 1.336(8) . ?
C6 N4 1.343(8) . ?
C7 N3 1.310(8) . ?
C7 C8 1.408(8) . ?
C8 N4 1.323(8) . ?
C8 C9 1.476(8) . ?
C9 C14 1.388(8) . ?
C9 C10 1.409(8) . ?
C10 C11 1.372(9) . ?
C11 C12 1.400(10) . ?
C12 O1 1.353(7) . ?
C12 C13 1.392(8) . ?
C13 C14 1.398(8) . ?
C15 O1 1.455(8) . ?
N1 Pb1 2.624(5) . ?
N2 N3 1.347(7) . ?
N2 Pb1 2.743(5) . ?
Pb1 Br1 2.7924(8) . ?
Pb1 Br2 2.8285(7) . ?

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
N1 C1 C2 123.5(6) . . ?
C1 C2 C3 118.9(6) . . ?
C4 C3 C2 119.0(6) . . ?
C3 C4 C5 118.5(6) . . ?
N1 C5 C4 122.4(6) . . ?
N1 C5 C6 117.9(5) . . ?
C4 C5 C6 119.7(5) . . ?
N2 C6 N4 126.0(5) . . ?
N2 C6 C5 116.6(5) . . ?
N4 C6 C5 117.4(5) . . ?
N3 C7 C8 121.7(6) . . ?
N4 C8 C7 119.0(5) . . ?
N4 C8 C9 118.1(5) . . ?
C7 C8 C9 122.9(5) . . ?
C14 C9 C10 118.8(5) . . ?
C14 C9 C8 119.4(5) . . ?
C10 C9 C8 121.7(5) . . ?
C11 C10 C9 120.2(6) . . ?
C10 C11 C12 120.4(6) . . ?
O1 C12 C13 124.6(6) . . ?
O1 C12 C11 115.2(6) . . ?
C13 C12 C11 120.2(6) . . ?
C12 C13 C14 118.7(6) . . ?
C9 C14 C13 121.4(5) . . ?
C1 N1 C5 117.8(5) . . ?
C1 N1 Pb1 118.3(4) . . ?
C5 N1 Pb1 123.4(4) . . ?
C6 N2 N3 116.9(5) . . ?
C6 N2 Pb1 120.6(4) . . ?
N3 N2 Pb1 122.2(4) . . ?
C7 N3 N2 119.7(5) . . ?
C8 N4 C6 116.3(5) . . ?
C12 O1 C15 118.3(5) . . ?
N1 Pb1 N2 60.84(16) . . ?
N1 Pb1 Br1 97.69(12) . . ?
N2 Pb1 Br1 74.14(12) . . ?
N1 Pb1 Br2 88.72(11) . . ?
N2 Pb1 Br2 145.48(12) . . ?
Br1 Pb1 Br2 96.13(2) . . ?


# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
_chemical_melting_point          502
_exptl_crystal_recrystallization_method 'Diffusion experiment'
####################################################################### 
# 
# 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_ip2-2694_d15
_database_code_depnum_ccdc_archive 'CCDC 2350384'
loop_
_audit_author_name
_audit_author_address
'Daniel Fuhrmann'
;University of Leipzig
Germany
;
_audit_update_record             
;
2024-04-23 deposited with the CCDC.	2024-07-03 downloaded from the CCDC.
;

_audit_creation_date             2022-07-10T18:33:32-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

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

_chemical_formula_sum            'C36 H30 N10 O6 Pb2 S2'
_chemical_formula_weight         1177.2

#----------------------------------------------------------------------------#
#                   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                   9.7327(6)
_cell_length_b                   10.2844(6)
_cell_length_c                   10.5326(7)
_cell_angle_alpha                81.463(5)
_cell_angle_beta                 68.068(5)
_cell_angle_gamma                86.765(5)
_cell_volume                     967.13(11)
_cell_formula_units_Z            1
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    10802
_cell_measurement_theta_min      2.45
_cell_measurement_theta_max      28.28

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

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.135
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.104
_exptl_crystal_density_diffrn    2.021
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             560

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

_exptl_absorpt_coefficient_mu    8.88
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270. Afterwards scaling of
reflection intensities was performed within STOE LANA. J. Koziskova, F. Hahn,
J. Richter, J. Kozisek, Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136-140.
;
_exptl_absorpt_correction_T_min  0.2185
_exptl_absorpt_correction_T_max  0.4198
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
5 -3 3 0.1240
2 -4 5 0.0920
-2 -4 5 0.0850
5 3 -4 0.0560
0 4 -5 0.0430
5 5 4 0.0630
0 5 5 0.0770
4 -4 -5 0.0760
-1 -5 -5 0.0410
-5 -2 -1 0.0750
-5 2 -2 0.1080

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

_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'

_diffrn_detector                 'image plate (34 cm diameter / schwenk)'
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_detector_area_resol_mean 6.67

_diffrn_source                   
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_type              ?
_diffrn_radiation_probe          x-ray
_diffrn_source_target            ?
_diffrn_source_voltage           50
_diffrn_source_current           40.000
_diffrn_source_power             2.000
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_collimation    '0.5 mm diameter, multiple pinhole'

_diffrn_ambient_temperature      200

_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_measurement_details      
; 225 frames, detector distance = 110 mm
;
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_number            9247
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.698
_diffrn_reflns_theta_max         27.939
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.987
_reflns_Friedel_coverage         0
_reflns_number_total             4574
_reflns_number_gt                3900
_reflns_threshold_expression     'I > 2σ(I)'

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

_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_data_collection       
;
X-Area WinXpose 2.0.22.0 (STOE, 2016)
;
_computing_cell_refinement       
;
X-Area Recipe 1.36.0.0 (STOE, 2020)
;
_computing_data_reduction        
;
X-Area Integrate 1.78.3.0 (STOE, 2020)
X-Area LANA 1.83.8.0 (STOE, 2020)
;
_computing_publication_material  
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.90, Darmstadt 2020
;

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

_atom_sites_solution_primary     direct
_atom_sites_solution_hydrogens   geom

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

_shelx_SHELXL_version_number     2018/3
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0334P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         4574
_refine_ls_number_parameters     255
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0254
_refine_ls_wR_factor_ref         0.0572
_refine_ls_wR_factor_gt          0.0556
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_restrained_S_all      0.984
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.671
_refine_diff_density_min         -1.57
_refine_diff_density_rms         0.124

#----------------------------------------------------------------------------#
#                   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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 '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 1.0642(5) 0.9148(4) 0.3528(5) 0.0341(10) Uani 1 1 d . . . . .
C2 C 0.6410(5) 0.8815(4) 0.2610(4) 0.0283(9) Uani 1 1 d . . . . .
C3 C 0.6409(7) 0.8717(5) 0.1192(5) 0.0526(14) Uani 1 1 d . . . . .
H3A H 0.725745 0.92019 0.048664 0.079 Uiso 1 1 calc R U . . .
H3B H 0.548912 0.909512 0.112066 0.079 Uiso 1 1 calc R U . . .
H3C H 0.647942 0.779188 0.104951 0.079 Uiso 1 1 calc R U . . .
C4 C 0.7877(5) 0.5723(4) 0.5828(5) 0.0344(10) Uani 1 1 d . . . . .
H4 H 0.876463 0.62142 0.554263 0.041 Uiso 1 1 calc R U . . .
C5 C 0.7944(5) 0.4368(4) 0.6108(4) 0.0329(10) Uani 1 1 d . . . . .
H5 H 0.886477 0.394044 0.599334 0.039 Uiso 1 1 calc R U . . .
C6 C 0.6658(5) 0.3648(4) 0.6555(4) 0.0318(9) Uani 1 1 d . . . . .
H6 H 0.66738 0.271869 0.677366 0.038 Uiso 1 1 calc R U . . .
C7 C 0.5341(5) 0.4305(4) 0.6681(4) 0.0283(9) Uani 1 1 d . . . . .
H7 H 0.443973 0.38345 0.696745 0.034 Uiso 1 1 calc R U . . .
C8 C 0.5367(4) 0.5664(4) 0.6379(4) 0.0216(8) Uani 1 1 d . . . . .
C9 C 0.3959(4) 0.6389(4) 0.6520(4) 0.0216(7) Uani 1 1 d . . . . .
C10 C 0.1508(4) 0.7662(4) 0.6712(4) 0.0288(9) Uani 1 1 d . . . . .
H10 H 0.061251 0.811199 0.676631 0.035 Uiso 1 1 calc R U . . .
C11 C 0.1444(4) 0.6330(4) 0.7303(4) 0.0238(8) Uani 1 1 d . . . . .
C12 C 0.0059(4) 0.5601(4) 0.8067(4) 0.0252(8) Uani 1 1 d . . . . .
C13 C -0.1320(4) 0.6244(4) 0.8596(4) 0.0312(9) Uani 1 1 d . . . . .
H13 H -0.137216 0.717543 0.842362 0.037 Uiso 1 1 calc R U . . .
C14 C -0.2577(5) 0.5536(4) 0.9351(5) 0.0330(10) Uani 1 1 d . . . . .
H14 H -0.349203 0.598199 0.971807 0.04 Uiso 1 1 calc R U . . .
C15 C -0.2539(5) 0.4170(4) 0.9591(4) 0.0300(9) Uani 1 1 d . . . . .
C16 C -0.1197(5) 0.3515(4) 0.9067(4) 0.0309(9) Uani 1 1 d . . . . .
H16 H -0.116031 0.258221 0.922184 0.037 Uiso 1 1 calc R U . . .
C17 C 0.0080(5) 0.4229(4) 0.8323(4) 0.0310(9) Uani 1 1 d . . . . .
H17 H 0.099405 0.377735 0.79749 0.037 Uiso 1 1 calc R U . . .
C18 C -0.3871(5) 0.2169(5) 1.0626(5) 0.0406(11) Uani 1 1 d . . . . .
H18A H -0.350734 0.180397 0.975117 0.061 Uiso 1 1 calc R U . . .
H18B H -0.488531 0.186551 1.117182 0.061 Uiso 1 1 calc R U . . .
H18C H -0.323084 0.187633 1.114443 0.061 Uiso 1 1 calc R U . . .
N1 N 0.9601(5) 0.8545(4) 0.4303(5) 0.0493(11) Uani 1 1 d . . . . .
N2 N 0.6616(4) 0.6368(3) 0.5942(4) 0.0286(7) Uani 1 1 d . . . . .
N3 N 0.4044(4) 0.7657(3) 0.6005(3) 0.0269(7) Uani 1 1 d . . . . .
N4 N 0.2776(4) 0.8301(3) 0.6088(4) 0.0292(8) Uani 1 1 d . . . . .
N5 N 0.2704(3) 0.5695(3) 0.7164(3) 0.0244(7) Uani 1 1 d . . . . .
O1 O 0.7213(4) 0.8044(4) 0.3072(3) 0.0498(9) Uani 1 1 d . . . . .
O2 O 0.5631(4) 0.9657(3) 0.3286(3) 0.0421(8) Uani 1 1 d . . . . .
O3 O -0.3855(3) 0.3575(3) 1.0351(3) 0.0366(7) Uani 1 1 d . . . . .
Pb1 Pb 0.67262(2) 0.89256(2) 0.51865(2) 0.02596(5) Uani 1 1 d . . . . .
S1 S 1.20948(15) 0.99623(13) 0.24668(13) 0.0448(3) 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 N1 1.175(6) . ?
C1 S1 1.620(5) . ?
C2 O2 1.241(5) . ?
C2 O1 1.254(5) . ?
C2 C3 1.512(6) . ?
C2 Pb1 2.862(4) . ?
C4 N2 1.335(5) . ?
C4 C5 1.384(6) . ?
C5 C6 1.377(6) . ?
C6 C7 1.385(6) . ?
C7 C8 1.385(6) . ?
C8 N2 1.341(5) . ?
C8 C9 1.490(5) . ?
C9 N3 1.331(5) . ?
C9 N5 1.341(5) . ?
C10 N4 1.320(5) . ?
C10 C11 1.413(6) . ?
C11 N5 1.325(5) . ?
C11 C12 1.466(5) . ?
C12 C17 1.397(6) . ?
C12 C13 1.414(5) . ?
C13 C14 1.364(6) . ?
C14 C15 1.390(6) . ?
C15 O3 1.354(5) . ?
C15 C16 1.392(6) . ?
C16 C17 1.379(6) . ?
C18 O3 1.431(5) . ?
N1 Pb1 2.625(4) . ?
N2 Pb1 2.628(3) . ?
N3 N4 1.347(5) . ?
N3 Pb1 2.762(4) . ?
O1 Pb1 2.402(3) . ?
O2 Pb1 2.600(3) . ?
O2 Pb1 2.745(3) 2_676 ?

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
N1 C1 S1 179.0(5) . . ?
O2 C2 O1 121.4(4) . . ?
O2 C2 C3 119.6(4) . . ?
O1 C2 C3 119.0(4) . . ?
O2 C2 Pb1 65.3(2) . . ?
O1 C2 Pb1 56.2(2) . . ?
C3 C2 Pb1 174.1(3) . . ?
N2 C4 C5 122.7(4) . . ?
C6 C5 C4 119.2(4) . . ?
C5 C6 C7 118.7(4) . . ?
C6 C7 C8 118.6(4) . . ?
N2 C8 C7 122.8(4) . . ?
N2 C8 C9 117.8(3) . . ?
C7 C8 C9 119.4(4) . . ?
N3 C9 N5 125.5(3) . . ?
N3 C9 C8 118.1(3) . . ?
N5 C9 C8 116.5(3) . . ?
N4 C10 C11 122.0(4) . . ?
N5 C11 C10 118.5(4) . . ?
N5 C11 C12 117.7(4) . . ?
C10 C11 C12 123.8(3) . . ?
C17 C12 C13 117.9(4) . . ?
C17 C12 C11 120.0(3) . . ?
C13 C12 C11 122.1(4) . . ?
C14 C13 C12 120.4(4) . . ?
C13 C14 C15 121.0(4) . . ?
O3 C15 C14 115.7(4) . . ?
O3 C15 C16 124.7(4) . . ?
C14 C15 C16 119.6(4) . . ?
C17 C16 C15 119.6(4) . . ?
C16 C17 C12 121.5(4) . . ?
C1 N1 Pb1 135.1(4) . . ?
C4 N2 C8 117.9(4) . . ?
C4 N2 Pb1 118.6(3) . . ?
C8 N2 Pb1 123.4(2) . . ?
C9 N3 N4 118.0(3) . . ?
C9 N3 Pb1 118.5(2) . . ?
N4 N3 Pb1 122.8(2) . . ?
C10 N4 N3 118.9(3) . . ?
C11 N5 C9 117.1(3) . . ?
C2 O1 Pb1 98.1(3) . . ?
C2 O2 Pb1 89.0(3) . . ?
C2 O2 Pb1 163.7(3) . 2_676 ?
Pb1 O2 Pb1 97.73(10) . 2_676 ?
C15 O3 C18 117.7(3) . . ?
O1 Pb1 O2 51.38(10) . . ?
O1 Pb1 N1 77.54(14) . . ?
O2 Pb1 N1 115.90(13) . . ?
O1 Pb1 N2 76.37(11) . . ?
O2 Pb1 N2 113.00(11) . . ?
N1 Pb1 N2 83.65(12) . . ?
O1 Pb1 O2 131.13(11) . 2_676 ?
O2 Pb1 O2 82.27(10) . 2_676 ?
N1 Pb1 O2 146.72(13) . 2_676 ?
N2 Pb1 O2 116.12(10) . 2_676 ?
O1 Pb1 N3 83.38(12) . . ?
O2 Pb1 N3 72.71(11) . . ?
N1 Pb1 N3 143.21(12) . . ?
N2 Pb1 N3 61.26(10) . . ?
O2 Pb1 N3 66.71(10) 2_676 . ?
O1 Pb1 C2 25.71(11) . . ?
O2 Pb1 C2 25.69(10) . . ?
N1 Pb1 C2 96.56(14) . . ?
N2 Pb1 C2 95.47(11) . . ?
O2 Pb1 C2 107.09(11) 2_676 . ?
N3 Pb1 C2 77.51(11) . . ?



# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
_chemical_melting_point          478
_exptl_crystal_recrystallization_method 'Diffusion experiment'
