# Electronic Supplementary Material (ESI) for CrystEngComm.
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 2310953'
loop_
_audit_author_name
_audit_author_address
'Damir Safin'
;Tyumen State University
Russia
;
_audit_update_record             
;
2023-11-29 deposited with the CCDC.	2024-02-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20  H15  N5  Pb1  S2'
_chemical_formula_sum            'C20 H15 N5 Pb S2'
_chemical_formula_weight         596.68

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'
N N 0.0061 0.0033 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

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

_cell_length_a                   5.6513(12)
_cell_length_b                   19.384(4)
_cell_length_c                   18.237(4)
_cell_angle_alpha                90
_cell_angle_beta                 98.331(8)
_cell_angle_gamma                90
_cell_volume                     1976.7(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4457
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      24.58

_exptl_crystal_description       needle
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.005
_exptl_crystal_F_000             1136
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.155
_exptl_crystal_size_mid          0.023
_exptl_crystal_size_min          0.019
_exptl_absorpt_coefficient_mu    8.762
_shelx_estimated_absorpt_T_min   0.344
_shelx_estimated_absorpt_T_max   0.851
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7076
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON III-14'
_diffrn_measurement_method       'omega and phi'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            29693
_diffrn_reflns_av_unetI/netI     0.0807
_diffrn_reflns_av_R_equivalents  0.1483
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.385
_diffrn_reflns_theta_max         25.340
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             3558
_reflns_number_gt                3040
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'APEX3 Software (Bruker, 2019)'
_computing_cell_refinement       'APEX3 Software (Bruker, 2019)'
_computing_data_reduction        'APEX3 Software (Bruker, 2019)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1014P)²+198.1175P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3558
_refine_ls_number_parameters     256
_refine_ls_number_restraints     239
_refine_ls_R_factor_all          0.1394
_refine_ls_R_factor_gt           0.1221
_refine_ls_wR_factor_ref         0.2754
_refine_ls_wR_factor_gt          0.2664
_refine_ls_goodness_of_fit_ref   1.235
_refine_ls_restrained_S_all      1.195
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Pb Pb 0.76023(16) 0.41811(5) 0.46935(5) 0.0154(3) Uani 1 1 d . . . . .
S1 S 0.2833(11) 0.4533(3) 0.4303(3) 0.0169(12) Uani 1 1 d . U . . .
S2 S 0.5940(12) 0.3367(4) 0.5886(3) 0.0210(13) Uani 1 1 d . . . . .
N1 N 0.920(4) 0.3075(11) 0.4090(11) 0.0191(15) Uani 1 1 d . . . . .
N2 N 0.587(4) 0.3899(11) 0.3343(11) 0.0167(15) Uani 1 1 d . . . . .
N3 N 0.427(4) 0.4346(11) 0.2946(11) 0.0171(16) Uani 1 1 d . . . . .
N4 N 0.132(4) 0.5138(10) 0.3029(11) 0.0134(19) Uani 1 1 d . U . . .
H4A H 0.044567 0.533439 0.333282 0.016 Uiso 1 1 calc R U . . .
N5 N 0.218(4) 0.4281(13) 0.6000(12) 0.027(4) Uani 1 1 d . . . . .
C1 C 0.375(4) 0.3904(13) 0.5958(13) 0.015(3) Uani 1 1 d . U . . .
C2 C 1.105(5) 0.2736(14) 0.4466(14) 0.021(2) Uani 1 1 d . . . . .
H2 H 1.134676 0.278224 0.499015 0.025 Uiso 1 1 d R U . . .
C3 C 1.253(5) 0.2320(14) 0.4141(14) 0.021(3) Uani 1 1 d . . . . .
H3 H 1.390017 0.211693 0.441951 0.025 Uiso 1 1 d R U . . .
C4 C 1.197(5) 0.2203(14) 0.3364(13) 0.019(3) Uani 1 1 d . . . . .
H4 H 1.281910 0.186982 0.312271 0.022 Uiso 1 1 d R U . . .
C5 C 1.015(4) 0.2582(12) 0.2981(12) 0.013(2) Uani 1 1 d . . . . .
H5 H 0.982732 0.253958 0.245711 0.016 Uiso 1 1 d R U . . .
C6 C 0.879(5) 0.3027(13) 0.3345(13) 0.0168(18) Uani 1 1 d . . . . .
C7 C 0.698(5) 0.3474(14) 0.2954(13) 0.0174(11) Uani 1 1 d . . . . .
C8 C 0.295(4) 0.4660(13) 0.3338(13) 0.0146(17) Uani 1 1 d . . . . .
C9 C 0.087(4) 0.5354(12) 0.2286(13) 0.0121(19) Uani 1 1 d . U . . .
C10 C -0.126(4) 0.5708(13) 0.2076(13) 0.016(3) Uani 1 1 d . . . . .
H10 H -0.226302 0.579287 0.244094 0.019 Uiso 1 1 d R U . . .
C11 C -0.199(5) 0.5943(13) 0.1366(13) 0.017(3) Uani 1 1 d . . . . .
H11 H -0.336639 0.622560 0.125635 0.021 Uiso 1 1 d R U . . .
C12 C -0.061(5) 0.5755(14) 0.0811(13) 0.020(3) Uani 1 1 d . . . . .
H12 H -0.113546 0.586305 0.030516 0.024 Uiso 1 1 d R U . . .
C13 C 0.151(5) 0.5402(14) 0.1022(13) 0.018(3) Uani 1 1 d . . . . .
H13 H 0.250184 0.529749 0.065949 0.022 Uiso 1 1 d R U . . .
C14 C 0.221(4) 0.5204(12) 0.1747(12) 0.012(3) Uani 1 1 d . . . . .
H14 H 0.366657 0.495552 0.186907 0.015 Uiso 1 1 d R U . . .
C15 C 0.652(5) 0.3485(13) 0.2128(13) 0.0174(11) Uani 1 1 d . . . . .
C16 C 0.819(5) 0.3802(14) 0.1759(13) 0.018(3) Uani 1 1 d . . . . .
H16 H 0.965537 0.396606 0.202455 0.022 Uiso 1 1 d R U . . .
C17 C 0.771(5) 0.3887(13) 0.0996(13) 0.015(3) Uani 1 1 d . . . . .
H17 H 0.885083 0.411547 0.074620 0.018 Uiso 1 1 d R U . . .
C18 C 0.565(5) 0.3645(13) 0.0602(14) 0.018(3) Uani 1 1 d . . . . .
H18 H 0.532123 0.372121 0.008234 0.021 Uiso 1 1 d R U . . .
C19 C 0.402(5) 0.3291(15) 0.0965(14) 0.022(3) Uani 1 1 d . . . . .
H19 H 0.261895 0.309262 0.069716 0.026 Uiso 1 1 d R U . . .
C20 C 0.451(5) 0.3232(14) 0.1744(13) 0.020(3) Uani 1 1 d . . . . .
H20 H 0.337950 0.300771 0.200038 0.024 Uiso 1 1 d 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
Pb N2 2.57(2) . ?
Pb N1 2.63(2) . ?
Pb S1 2.771(7) . ?
Pb S2 2.949(7) . ?
Pb S1 3.123(6) 3_666 ?
Pb S1 3.212(6) 1_655 ?
Pb Pb 4.219(2) 3_766 ?
Pb Pb 4.575(2) 3_666 ?
S1 C8 1.79(2) . ?
S2 C1 1.64(2) . ?
N1 C2 1.34(3) . ?
N1 C6 1.35(3) . ?
N2 C7 1.31(3) . ?
N2 N3 1.38(3) . ?
N3 C8 1.26(3) . ?
N4 C8 1.37(3) . ?
N4 C9 1.41(3) . ?
N4 H4A 0.8800 . ?
N5 C1 1.16(3) . ?
C2 C3 1.36(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.42(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.37(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.39(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.45(4) . ?
C7 C15 1.49(3) . ?
C9 C14 1.36(3) . ?
C9 C10 1.39(3) . ?
C10 C11 1.38(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.41(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.38(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.38(3) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 C20 1.34(4) . ?
C15 C16 1.38(4) . ?
C16 C17 1.39(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.36(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.39(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.41(3) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?

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
N2 Pb N1 62.1(7) . . ?
N2 Pb S1 65.5(5) . . ?
N1 Pb S1 118.3(5) . . ?
N2 Pb S2 118.3(5) . . ?
N1 Pb S2 92.2(5) . . ?
S1 Pb S2 85.36(19) . . ?
N2 Pb S1 132.7(5) . 3_666 ?
N1 Pb S1 163.2(5) . 3_666 ?
S1 Pb S1 78.34(19) . 3_666 ?
S2 Pb S1 86.24(18) . 3_666 ?
N2 Pb S1 93.9(5) . 1_655 ?
N1 Pb S1 72.4(5) . 1_655 ?
S1 Pb S1 141.5(2) . 1_655 ?
S2 Pb S1 132.74(17) . 1_655 ?
S1 Pb S1 96.52(16) 3_666 1_655 ?
N2 Pb Pb 123.6(5) . 3_766 ?
N1 Pb Pb 118.6(5) . 3_766 ?
S1 Pb Pb 116.52(14) . 3_766 ?
S2 Pb Pb 117.92(14) . 3_766 ?
S1 Pb Pb 49.16(12) 3_666 3_766 ?
S1 Pb Pb 47.36(11) 1_655 3_766 ?
N2 Pb Pb 102.3(5) . 3_666 ?
N1 Pb Pb 160.1(5) . 3_666 ?
S1 Pb Pb 41.96(13) . 3_666 ?
S2 Pb Pb 84.62(13) . 3_666 ?
S1 Pb Pb 36.38(12) 3_666 3_666 ?
S1 Pb Pb 123.48(12) 1_655 3_666 ?
Pb Pb Pb 79.87(4) 3_766 3_666 ?
C8 S1 Pb 96.5(8) . . ?
C8 S1 Pb 118.9(8) . 3_666 ?
Pb S1 Pb 101.66(19) . 3_666 ?
C1 S2 Pb 92.6(9) . . ?
C2 N1 C6 119(2) . . ?
C2 N1 Pb 118.5(16) . . ?
C6 N1 Pb 117.3(17) . . ?
C7 N2 N3 116(2) . . ?
C7 N2 Pb 120.4(16) . . ?
N3 N2 Pb 119.9(14) . . ?
C8 N3 N2 114(2) . . ?
C8 N4 C9 128(2) . . ?
C8 N4 H4A 116.0 . . ?
C9 N4 H4A 116.0 . . ?
N5 C1 S2 179(2) . . ?
N1 C2 C3 123(2) . . ?
N1 C2 H2 118.6 . . ?
C3 C2 H2 117.9 . . ?
C2 C3 C4 118(2) . . ?
C2 C3 H3 121.2 . . ?
C4 C3 H3 120.8 . . ?
C5 C4 C3 118(2) . . ?
C5 C4 H4 121.3 . . ?
C3 C4 H4 121.1 . . ?
C4 C5 C6 121(2) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 H5 119.6 . . ?
N1 C6 C5 120(2) . . ?
N1 C6 C7 118(2) . . ?
C5 C6 C7 123(2) . . ?
N2 C7 C6 118(2) . . ?
N2 C7 C15 121(2) . . ?
C6 C7 C15 121(2) . . ?
N3 C8 N4 121(2) . . ?
N3 C8 S1 127(2) . . ?
N4 C8 S1 112.3(17) . . ?
C14 C9 C10 117(2) . . ?
C14 C9 N4 126(2) . . ?
C10 C9 N4 116(2) . . ?
C11 C10 C9 123(2) . . ?
C11 C10 H10 118.4 . . ?
C9 C10 H10 118.2 . . ?
C10 C11 C12 118(2) . . ?
C10 C11 H11 120.7 . . ?
C12 C11 H11 121.3 . . ?
C13 C12 C11 118(2) . . ?
C13 C12 H12 120.9 . . ?
C11 C12 H12 120.9 . . ?
C14 C13 C12 122(2) . . ?
C14 C13 H13 119.2 . . ?
C12 C13 H13 119.2 . . ?
C9 C14 C13 121(2) . . ?
C9 C14 H14 119.6 . . ?
C13 C14 H14 119.2 . . ?
C20 C15 C16 120(2) . . ?
C20 C15 C7 122(2) . . ?
C16 C15 C7 118(2) . . ?
C15 C16 C17 120(2) . . ?
C15 C16 H16 120.3 . . ?
C17 C16 H16 120.1 . . ?
C18 C17 C16 121(2) . . ?
C18 C17 H17 119.7 . . ?
C16 C17 H17 119.2 . . ?
C17 C18 C19 120(2) . . ?
C17 C18 H18 120.0 . . ?
C19 C18 H18 120.4 . . ?
C18 C19 C20 118(2) . . ?
C18 C19 H19 120.9 . . ?
C20 C19 H19 120.8 . . ?
C15 C20 C19 122(2) . . ?
C15 C20 H20 119.4 . . ?
C19 C20 H20 118.9 . . ?

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
C7 N2 N3 C8 168(2) . . . . ?
Pb N2 N3 C8 -32(3) . . . . ?
C6 N1 C2 C3 -2(4) . . . . ?
Pb N1 C2 C3 -157(2) . . . . ?
N1 C2 C3 C4 -4(4) . . . . ?
C2 C3 C4 C5 8(4) . . . . ?
C3 C4 C5 C6 -5(4) . . . . ?
C2 N1 C6 C5 6(4) . . . . ?
Pb N1 C6 C5 160.6(18) . . . . ?
C2 N1 C6 C7 -172(2) . . . . ?
Pb N1 C6 C7 -17(3) . . . . ?
C4 C5 C6 N1 -2(4) . . . . ?
C4 C5 C6 C7 175(2) . . . . ?
N3 N2 C7 C6 176(2) . . . . ?
Pb N2 C7 C6 17(3) . . . . ?
N3 N2 C7 C15 0(4) . . . . ?
Pb N2 C7 C15 -158.9(18) . . . . ?
N1 C6 C7 N2 0(4) . . . . ?
C5 C6 C7 N2 -177(2) . . . . ?
N1 C6 C7 C15 176(2) . . . . ?
C5 C6 C7 C15 -1(4) . . . . ?
N2 N3 C8 N4 178(2) . . . . ?
N2 N3 C8 S1 -5(3) . . . . ?
C9 N4 C8 N3 -1(4) . . . . ?
C9 N4 C8 S1 -178.2(18) . . . . ?
Pb S1 C8 N3 32(2) . . . . ?
Pb S1 C8 N3 139(2) 3_666 . . . ?
Pb S1 C8 N4 -150.6(16) . . . . ?
Pb S1 C8 N4 -43(2) 3_666 . . . ?
C8 N4 C9 C14 -11(4) . . . . ?
C8 N4 C9 C10 164(2) . . . . ?
C14 C9 C10 C11 -4(4) . . . . ?
N4 C9 C10 C11 -179(2) . . . . ?
C9 C10 C11 C12 6(4) . . . . ?
C10 C11 C12 C13 -6(4) . . . . ?
C11 C12 C13 C14 3(4) . . . . ?
C10 C9 C14 C13 1(4) . . . . ?
N4 C9 C14 C13 175(2) . . . . ?
C12 C13 C14 C9 -1(4) . . . . ?
N2 C7 C15 C20 -74(4) . . . . ?
C6 C7 C15 C20 110(3) . . . . ?
N2 C7 C15 C16 102(3) . . . . ?
C6 C7 C15 C16 -73(3) . . . . ?
C20 C15 C16 C17 3(4) . . . . ?
C7 C15 C16 C17 -173(2) . . . . ?
C15 C16 C17 C18 -2(4) . . . . ?
C16 C17 C18 C19 -2(4) . . . . ?
C17 C18 C19 C20 4(4) . . . . ?
C16 C15 C20 C19 -1(4) . . . . ?
C7 C15 C20 C19 175(3) . . . . ?
C18 C19 C20 C15 -2(4) . . . . ?

_refine_diff_density_max         6.893
_refine_diff_density_min         -6.925
_refine_diff_density_rms         0.504

####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 2324741'
loop_
_audit_author_name
_audit_author_address
'Damir Safin'
;Tyumen State University
Russia
;
_audit_update_record             
;
2024-01-10 deposited with the CCDC.	2024-02-15 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT971_3                   
;
PROBLEM: Check Calcd Resid. Dens.  0.95Ang From Pb              4.78 eA-3 
RESPONSE: It is likely caused by nonideal absorption correction of the data 
;
_vrf_PLAT094_3                   
;
PROBLEM: Ratio of Maximum / Minimum Residual Density ....       6.80 Report 
RESPONSE: A residual close to Pb could not be removed by absorption correction 
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2019/2
_shelx_SHELXL_version_number     2019/2
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H9 N6 Pb S2, C N S'
_chemical_formula_sum            'C9 H9 N7 Pb S3'
_chemical_formula_weight         518.60

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'
N N 0.0061 0.0033 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 2/a'
_space_group_name_Hall           '-I 2ya'

_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.
;

loop_
_space_group_symop_operation_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                   7.8039(4)
_cell_length_b                   11.1545(7)
_cell_length_c                   33.709(2)
_cell_angle_alpha                90
_cell_angle_beta                 90.944(2)
_cell_angle_gamma                90
_cell_volume                     2933.9(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9933
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      30.63

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.348
_exptl_crystal_F_000             1936
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    11.927
_shelx_estimated_absorpt_T_min   0.449
_shelx_estimated_absorpt_T_max   0.796
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.676
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'SADABS, Bruker 2010'

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON III-14'
_diffrn_measurement_method       'omega and phi'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            41141
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_theta_min         2.417
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4472
_reflns_number_gt                4017
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'APEX3 Software (Bruker, 2019)'
_computing_cell_refinement       'APEX3 Software (Bruker, 2019)'
_computing_data_reduction        'APEX3 Software (Bruker, 2019)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Diamond vers. 3.2k'
_computing_publication_material  'WinGX vers. 2018.3'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0161P)²+23.5503P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4472
_refine_ls_number_parameters     181
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0221
_refine_ls_wR_factor_ref         0.0482
_refine_ls_wR_factor_gt          0.0464
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Pb Pb 0.55117(2) 0.39464(2) 0.07580(2) 0.00944(4) Uani 1 1 d . . . . .
S1 S 0.40195(11) 0.57983(7) 0.12234(2) 0.01209(15) Uani 1 1 d . . . . .
N1 N 0.5559(4) 0.1661(2) 0.08362(8) 0.0126(5) Uani 1 1 d . . . . .
N2 N 0.4511(3) 0.3145(2) 0.14068(8) 0.0110(5) Uani 1 1 d . . . . .
N3 N 0.3917(4) 0.3878(2) 0.17101(8) 0.0121(5) Uani 1 1 d . . . . .
H3A H 0.399026 0.364465 0.194997 0.015 Uiso 1 1 d R U . . .
N4 N 0.3267(4) 0.5670(3) 0.19829(9) 0.0191(6) Uani 1 1 d . . . . .
H4A H 0.321793 0.536319 0.219580 0.023 Uiso 1 1 d R U . . .
H4B H 0.307463 0.635329 0.195080 0.023 Uiso 1 1 d R U . . .
N5 N 0.3496(4) 0.1533(3) 0.17881(9) 0.0152(6) Uani 1 1 d D . . . .
H5A H 0.336321 0.074724 0.182514 0.018 Uiso 1 1 d DR U . . .
H5B H 0.299321 0.198994 0.195914 0.018 Uiso 1 1 d DR U . . .
C1 C 0.6137(5) 0.0943(3) 0.05499(10) 0.0164(7) Uani 1 1 d . . . . .
H1 H 0.654904 0.129998 0.031403 0.020 Uiso 1 1 calc R U . . .
C2 C 0.6163(5) -0.0288(3) 0.05807(11) 0.0192(7) Uani 1 1 d . . . . .
H2 H 0.657031 -0.076981 0.036988 0.023 Uiso 1 1 calc R U . . .
C3 C 0.5579(5) -0.0806(3) 0.09275(11) 0.0170(7) Uani 1 1 d . . . . .
H3 H 0.560270 -0.165177 0.096071 0.020 Uiso 1 1 calc R U . . .
C4 C 0.4963(4) -0.0074(3) 0.12242(10) 0.0152(6) Uani 1 1 d . . . . .
H4 H 0.454585 -0.041220 0.146257 0.018 Uiso 1 1 calc R U . . .
C5 C 0.4959(4) 0.1157(3) 0.11699(9) 0.0107(6) Uani 1 1 d . . . . .
C6 C 0.4276(4) 0.2001(3) 0.14726(9) 0.0107(6) Uani 1 1 d . . . . .
C7 C 0.3727(4) 0.5062(3) 0.16628(10) 0.0123(6) Uani 1 1 d . . . . .
S2 S -0.07291(10) 0.34144(8) 0.02236(2) 0.01538(16) Uani 1 1 d . . . . .
C8 C 0.1229(4) 0.3369(3) 0.04043(9) 0.0104(6) Uani 1 1 d . . . . .
N6 N 0.2596(4) 0.3358(3) 0.05495(9) 0.0165(6) Uani 1 1 d . . . . .
S3 S 0.76780(11) 0.13523(8) 0.20611(3) 0.01570(16) Uani 1 1 d . . . . .
C9 C 0.9548(5) 0.1458(3) 0.22956(10) 0.0159(7) Uani 1 1 d . . . . .
N7 N 1.0856(4) 0.1539(3) 0.24664(9) 0.0202(6) Uani 1 1 d . . . . .


_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
Pb N6 2.459(3) . ?
Pb N2 2.499(3) . ?
Pb N1 2.563(3) . ?
Pb S1 2.8538(8) . ?
S1 C7 1.712(3) . ?
N1 C1 1.338(4) . ?
N1 C5 1.349(4) . ?
N2 C6 1.310(4) . ?
N2 N3 1.394(4) . ?
N3 C7 1.339(4) . ?
N3 H3A 0.8505 . ?
N4 C7 1.329(4) . ?
N4 H4A 0.7967 . ?
N4 H4B 0.7834 . ?
N5 C6 1.340(4) . ?
N5 H5A 0.8918 . ?
N5 H5B 0.8680 . ?
C1 C2 1.377(5) . ?
C1 H1 0.9500 . ?
C2 C3 1.388(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.384(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.385(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.493(4) . ?
S2 C8 1.637(3) . ?
C8 N6 1.167(4) . ?
S3 C9 1.653(4) . ?
C9 N7 1.167(5) . ?

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
N6 Pb N2 81.59(9) . . ?
N6 Pb N1 77.03(10) . . ?
N2 Pb N1 63.81(9) . . ?
N6 Pb S1 88.08(7) . . ?
N2 Pb S1 69.00(6) . . ?
N1 Pb S1 131.97(6) . . ?
C7 S1 Pb 100.95(11) . . ?
C1 N1 C5 118.5(3) . . ?
C1 N1 Pb 121.7(2) . . ?
C5 N1 Pb 119.8(2) . . ?
C6 N2 N3 113.4(3) . . ?
C6 N2 Pb 122.9(2) . . ?
N3 N2 Pb 123.00(19) . . ?
C7 N3 N2 121.9(3) . . ?
C7 N3 H3A 114.9 . . ?
N2 N3 H3A 120.0 . . ?
C7 N4 H4A 122.0 . . ?
C7 N4 H4B 115.9 . . ?
H4A N4 H4B 122.1 . . ?
C6 N5 H5A 123.3 . . ?
C6 N5 H5B 121.0 . . ?
H5A N5 H5B 115.4 . . ?
N1 C1 C2 123.2(3) . . ?
N1 C1 H1 118.4 . . ?
C2 C1 H1 118.4 . . ?
C1 C2 C3 118.3(3) . . ?
C1 C2 H2 120.8 . . ?
C3 C2 H2 120.8 . . ?
C4 C3 C2 119.1(3) . . ?
C4 C3 H3 120.5 . . ?
C2 C3 H3 120.5 . . ?
C3 C4 C5 119.3(3) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
N1 C5 C4 121.6(3) . . ?
N1 C5 C6 116.1(3) . . ?
C4 C5 C6 122.3(3) . . ?
N2 C6 N5 125.5(3) . . ?
N2 C6 C5 116.5(3) . . ?
N5 C6 C5 118.0(3) . . ?
N4 C7 N3 116.0(3) . . ?
N4 C7 S1 120.0(3) . . ?
N3 C7 S1 124.1(2) . . ?
N6 C8 S2 176.8(3) . . ?
C8 N6 Pb 162.3(3) . . ?
N7 C9 S3 179.0(3) . . ?

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
C6 N2 N3 C7 -166.3(3) . . . . ?
Pb N2 N3 C7 4.9(4) . . . . ?
C5 N1 C1 C2 -0.6(5) . . . . ?
Pb N1 C1 C2 -179.3(3) . . . . ?
N1 C1 C2 C3 -0.7(6) . . . . ?
C1 C2 C3 C4 1.4(6) . . . . ?
C2 C3 C4 C5 -0.7(5) . . . . ?
C1 N1 C5 C4 1.3(5) . . . . ?
Pb N1 C5 C4 -180.0(2) . . . . ?
C1 N1 C5 C6 -177.9(3) . . . . ?
Pb N1 C5 C6 0.8(4) . . . . ?
C3 C4 C5 N1 -0.7(5) . . . . ?
C3 C4 C5 C6 178.5(3) . . . . ?
N3 N2 C6 N5 2.2(5) . . . . ?
Pb N2 C6 N5 -169.0(2) . . . . ?
N3 N2 C6 C5 -177.0(3) . . . . ?
Pb N2 C6 C5 11.8(4) . . . . ?
N1 C5 C6 N2 -7.9(4) . . . . ?
C4 C5 C6 N2 172.8(3) . . . . ?
N1 C5 C6 N5 172.8(3) . . . . ?
C4 C5 C6 N5 -6.5(5) . . . . ?
N2 N3 C7 N4 -175.4(3) . . . . ?
N2 N3 C7 S1 5.2(5) . . . . ?
Pb S1 C7 N4 170.6(3) . . . . ?
Pb S1 C7 N3 -10.1(3) . . . . ?

_refine_diff_density_max         5.112
_refine_diff_density_min         -0.752
_refine_diff_density_rms         0.153

####################################################################### 
# 
# 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_3_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2310954'
loop_
_audit_author_name
_audit_author_address
'Damir Safin'
;Tyumen State University
Russia
;
_audit_update_record             
;
2023-11-29 deposited with the CCDC.	2024-02-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H9 N6 Pb S2, C N S'
_chemical_formula_sum            'C9 H9 N7 Pb S3'
_chemical_formula_weight         518.60

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'
N N 0.0061 0.0033 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 2/a'
_space_group_name_Hall           '-I 2ya'

_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.
;

loop_
_space_group_symop_operation_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                   7.8039(4)
_cell_length_b                   11.1545(7)
_cell_length_c                   33.709(2)
_cell_angle_alpha                90
_cell_angle_beta                 90.944(2)
_cell_angle_gamma                90
_cell_volume                     2933.9(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9933
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      30.63

_exptl_crystal_description       prism
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.348
_exptl_crystal_F_000             1936
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    11.927
_shelx_estimated_absorpt_T_min   0.449
_shelx_estimated_absorpt_T_max   0.796
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.676
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON III-14'
_diffrn_measurement_method       'omega and phi'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            41141
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_theta_min         2.417
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4472
_reflns_number_gt                4017
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'APEX3 Software (Bruker, 2019)'
_computing_cell_refinement       'APEX3 Software (Bruker, 2019)'
_computing_data_reduction        'APEX3 Software (Bruker, 2019)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Diamond vers. 3.2k'
_computing_publication_material  'WinGX vers. 2018.3'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0078P)²+8.2400P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4472
_refine_ls_number_parameters     191
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0235
_refine_ls_R_factor_gt           0.0180
_refine_ls_wR_factor_ref         0.0351
_refine_ls_wR_factor_gt          0.0337
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Pb Pb 0.55117(2) 0.39464(2) 0.07580(2) 0.00938(3) Uani 0.9865(5) 1 d . . P B .
S1 S 0.40198(8) 0.57983(5) 0.12232(2) 0.01266(12) Uani 1 1 d . . . . .
N1 N 0.5559(3) 0.16607(18) 0.08366(6) 0.0134(4) Uani 1 1 d . . . . .
N2 N 0.4512(3) 0.31450(18) 0.14073(6) 0.0115(4) Uani 1 1 d . . . . .
N3 N 0.3917(3) 0.38786(18) 0.17096(6) 0.0128(4) Uani 1 1 d . . . . .
H3A H 0.398974 0.364535 0.194946 0.015 Uiso 1 1 d R U . . .
N4 N 0.3266(3) 0.5671(2) 0.19827(7) 0.0198(5) Uani 1 1 d . . . . .
H4A H 0.321765 0.536322 0.219561 0.024 Uiso 1 1 d R U . . .
H4B H 0.307435 0.635332 0.195061 0.024 Uiso 1 1 d R U . . .
N5 N 0.3498(3) 0.15323(19) 0.17879(6) 0.0159(4) Uani 1 1 d D . . . .
H5A H 0.336487 0.074641 0.182486 0.019 Uiso 1 1 d DR U . . .
H5B H 0.299487 0.198911 0.195886 0.019 Uiso 1 1 d DR U . . .
C1 C 0.6136(4) 0.0941(2) 0.05502(8) 0.0167(5) Uani 1 1 d . . . . .
H1 H 0.654745 0.129767 0.031419 0.020 Uiso 1 1 calc R U . A 2
C2 C 0.6163(4) -0.0287(2) 0.05805(8) 0.0195(6) Uani 1 1 d . . . . .
H2 H 0.657206 -0.076820 0.036974 0.023 Uiso 1 1 calc R U . . .
C3 C 0.5578(4) -0.0806(2) 0.09258(8) 0.0175(5) Uani 1 1 d . . . . .
H3 H 0.559961 -0.165207 0.095833 0.021 Uiso 1 1 calc R U . . .
C4 C 0.4962(3) -0.0074(2) 0.12235(8) 0.0158(5) Uani 1 1 d . . . . .
H4 H 0.454620 -0.041338 0.146186 0.019 Uiso 1 1 calc R U . . .
C5 C 0.4957(3) 0.1157(2) 0.11701(7) 0.0111(4) Uani 1 1 d . . . . .
C6 C 0.4275(3) 0.2002(2) 0.14723(7) 0.0114(5) Uani 1 1 d . . . . .
C7 C 0.3725(3) 0.5061(2) 0.16627(7) 0.0130(5) Uani 1 1 d . . . . .
S2 S -0.07291(8) 0.34146(6) 0.02236(2) 0.01607(13) Uani 1 1 d . . . . .
C8 C 0.1233(3) 0.3369(2) 0.04044(7) 0.0108(5) Uani 1 1 d . . . . .
N6 N 0.2594(3) 0.3357(2) 0.05493(7) 0.0170(5) Uani 1 1 d . . . . .
S3 S 0.76788(9) 0.13518(6) 0.20610(2) 0.01652(13) Uani 1 1 d . . . . .
C9 C 0.9548(4) 0.1460(2) 0.22956(8) 0.0161(5) Uani 1 1 d . . . . .
N7 N 1.0856(3) 0.1539(2) 0.24663(7) 0.0209(5) Uani 1 1 d . . . . .
Pb2 Pb 0.5815(8) 0.3177(7) 0.07036(19) 0.010(2) Uani 0.0135(5) 1 d . . P B 2


_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
Pb Pb2 0.910(7) . ?
Pb N6 2.461(2) . ?
Pb N2 2.501(2) . ?
Pb N1 2.563(2) . ?
Pb S1 2.8534(6) . ?
S1 C7 1.713(3) . ?
N1 C1 1.339(3) . ?
N1 C5 1.348(3) . ?
N1 Pb2 1.762(8) . ?
N2 C6 1.308(3) . ?
N2 N3 1.392(3) . ?
N2 Pb2 2.597(7) . ?
N3 C7 1.337(3) . ?
N3 H3A 0.8505 . ?
N4 C7 1.329(3) . ?
N4 H4A 0.7967 . ?
N4 H4B 0.7834 . ?
N5 C6 1.340(3) . ?
N5 H5A 0.8918 . ?
N5 H5B 0.8680 . ?
C1 C2 1.374(4) . ?
C1 Pb2 2.560(8) . ?
C1 H1 0.9500 . ?
C2 C3 1.384(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.386(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.385(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.492(3) . ?
C5 Pb2 2.834(7) . ?
S2 C8 1.639(3) . ?
C8 N6 1.162(3) . ?
N6 Pb2 2.566(7) . ?
S3 C9 1.652(3) . ?
C9 N7 1.167(4) . ?

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
Pb2 Pb N6 86.2(4) . . ?
Pb2 Pb N2 85.7(4) . . ?
N6 Pb N2 81.62(7) . . ?
Pb2 Pb N1 23.0(4) . . ?
N6 Pb N1 77.04(7) . . ?
N2 Pb N1 63.78(7) . . ?
Pb2 Pb S1 154.6(4) . . ?
N6 Pb S1 88.08(5) . . ?
N2 Pb S1 69.01(5) . . ?
N1 Pb S1 131.95(5) . . ?
C7 S1 Pb 100.93(9) . . ?
C1 N1 C5 118.5(2) . . ?
C1 N1 Pb2 110.5(3) . . ?
C5 N1 Pb2 130.9(3) . . ?
C1 N1 Pb 121.74(17) . . ?
C5 N1 Pb 119.74(16) . . ?
Pb2 N1 Pb 11.6(2) . . ?
C6 N2 N3 113.6(2) . . ?
C6 N2 Pb 122.84(16) . . ?
N3 N2 Pb 122.88(15) . . ?
C6 N2 Pb2 103.0(2) . . ?
N3 N2 Pb2 143.2(2) . . ?
Pb N2 Pb2 20.46(16) . . ?
C7 N3 N2 122.1(2) . . ?
C7 N3 H3A 114.8 . . ?
N2 N3 H3A 119.9 . . ?
C7 N4 H4A 121.9 . . ?
C7 N4 H4B 116.0 . . ?
H4A N4 H4B 122.1 . . ?
C6 N5 H5A 123.4 . . ?
C6 N5 H5B 120.9 . . ?
H5A N5 H5B 115.4 . . ?
N1 C1 C2 123.3(2) . . ?
N1 C1 Pb2 40.12(19) . . ?
C2 C1 Pb2 163.3(2) . . ?
N1 C1 H1 118.4 . . ?
C2 C1 H1 118.4 . . ?
Pb2 C1 H1 78.3 . . ?
C1 C2 C3 118.4(2) . . ?
C1 C2 H2 120.8 . . ?
C3 C2 H2 120.8 . . ?
C2 C3 C4 119.0(2) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
C5 C4 C3 119.3(2) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
N1 C5 C4 121.4(2) . . ?
N1 C5 C6 116.1(2) . . ?
C4 C5 C6 122.5(2) . . ?
N1 C5 Pb2 28.02(17) . . ?
C4 C5 Pb2 149.4(2) . . ?
C6 C5 Pb2 88.12(19) . . ?
N2 C6 N5 125.5(2) . . ?
N2 C6 C5 116.6(2) . . ?
N5 C6 C5 117.8(2) . . ?
N4 C7 N3 116.1(2) . . ?
N4 C7 S1 119.9(2) . . ?
N3 C7 S1 124.02(19) . . ?
N6 C8 S2 176.8(2) . . ?
C8 N6 Pb 162.2(2) . . ?
C8 N6 Pb2 166.3(2) . . ?
Pb N6 Pb2 20.72(16) . . ?
N7 C9 S3 179.0(3) . . ?
Pb Pb2 N1 145.4(6) . . ?
Pb Pb2 C1 170.5(6) . . ?
N1 Pb2 C1 29.33(15) . . ?
Pb Pb2 N6 73.1(4) . . ?
N1 Pb2 N6 90.7(3) . . ?
C1 Pb2 N6 97.7(2) . . ?
Pb Pb2 N2 73.8(4) . . ?
N1 Pb2 N2 72.9(2) . . ?
C1 Pb2 N2 102.3(2) . . ?
N6 Pb2 N2 77.82(19) . . ?
Pb Pb2 C5 125.0(5) . . ?
N1 Pb2 C5 21.07(13) . . ?
C1 Pb2 C5 50.39(15) . . ?
N6 Pb2 C5 86.3(2) . . ?
N2 Pb2 C5 51.87(14) . . ?

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
C6 N2 N3 C7 -166.1(2) . . . . ?
Pb N2 N3 C7 4.8(3) . . . . ?
Pb2 N2 N3 C7 8.1(5) . . . . ?
C5 N1 C1 C2 -0.7(4) . . . . ?
Pb2 N1 C1 C2 177.2(3) . . . . ?
Pb N1 C1 C2 -179.3(2) . . . . ?
C5 N1 C1 Pb2 -177.9(4) . . . . ?
Pb N1 C1 Pb2 3.5(2) . . . . ?
N1 C1 C2 C3 -0.6(4) . . . . ?
Pb2 C1 C2 C3 5.7(10) . . . . ?
C1 C2 C3 C4 1.2(4) . . . . ?
C2 C3 C4 C5 -0.5(4) . . . . ?
C1 N1 C5 C4 1.4(4) . . . . ?
Pb2 N1 C5 C4 -176.0(3) . . . . ?
Pb N1 C5 C4 -179.99(18) . . . . ?
C1 N1 C5 C6 -177.9(2) . . . . ?
Pb2 N1 C5 C6 4.7(4) . . . . ?
Pb N1 C5 C6 0.7(3) . . . . ?
C1 N1 C5 Pb2 177.4(5) . . . . ?
Pb N1 C5 Pb2 -4.0(3) . . . . ?
C3 C4 C5 N1 -0.8(4) . . . . ?
C3 C4 C5 C6 178.5(2) . . . . ?
C3 C4 C5 Pb2 -4.5(6) . . . . ?
N3 N2 C6 N5 2.0(4) . . . . ?
Pb N2 C6 N5 -169.04(19) . . . . ?
Pb2 N2 C6 N5 -174.5(3) . . . . ?
N3 N2 C6 C5 -177.1(2) . . . . ?
Pb N2 C6 C5 11.9(3) . . . . ?
Pb2 N2 C6 C5 6.4(3) . . . . ?
N1 C5 C6 N2 -7.9(3) . . . . ?
C4 C5 C6 N2 172.8(2) . . . . ?
Pb2 C5 C6 N2 -5.7(2) . . . . ?
N1 C5 C6 N5 172.9(2) . . . . ?
C4 C5 C6 N5 -6.4(4) . . . . ?
Pb2 C5 C6 N5 175.1(2) . . . . ?
N2 N3 C7 N4 -175.3(2) . . . . ?
N2 N3 C7 S1 5.2(3) . . . . ?
Pb S1 C7 N4 170.5(2) . . . . ?
Pb S1 C7 N3 -10.0(2) . . . . ?
N6 Pb Pb2 N1 -65.3(10) . . . . ?
N2 Pb Pb2 N1 16.6(10) . . . . ?
S1 Pb Pb2 N1 12.0(18) . . . . ?
N2 Pb Pb2 N6 81.86(8) . . . . ?
N1 Pb Pb2 N6 65.3(10) . . . . ?
S1 Pb Pb2 N6 77.3(9) . . . . ?
N6 Pb Pb2 N2 -81.86(8) . . . . ?
N1 Pb Pb2 N2 -16.6(10) . . . . ?
S1 Pb Pb2 N2 -4.6(9) . . . . ?
N6 Pb Pb2 C5 -72.9(5) . . . . ?
N2 Pb Pb2 C5 9.0(4) . . . . ?
N1 Pb Pb2 C5 -7.5(6) . . . . ?
S1 Pb Pb2 C5 4.4(13) . . . . ?
C1 N1 Pb2 Pb 165.0(10) . . . . ?
C5 N1 Pb2 Pb -17.4(13) . . . . ?
C5 N1 Pb2 C1 177.6(4) . . . . ?
Pb N1 Pb2 C1 -165.0(10) . . . . ?
C1 N1 Pb2 N6 104.6(2) . . . . ?
C5 N1 Pb2 N6 -77.8(3) . . . . ?
Pb N1 Pb2 N6 -60.4(10) . . . . ?
C1 N1 Pb2 N2 -178.3(2) . . . . ?
C5 N1 Pb2 N2 -0.8(3) . . . . ?
Pb N1 Pb2 N2 16.6(10) . . . . ?
C1 N1 Pb2 C5 -177.6(4) . . . . ?
Pb N1 Pb2 C5 17.4(13) . . . . ?

_refine_diff_density_max         0.641
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.128

