# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1960844'
loop_
_audit_author_name
_audit_author_address
'Damir Safin'
;University of Tyumen
Russia
;
_audit_update_record             
;
2019-10-22 deposited with the CCDC.	2020-03-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H10 N6 O7 Pb'
_chemical_formula_sum            'C12 H10 N6 O7 Pb'
_chemical_formula_weight         557.45

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   17.2085(6)
_cell_length_b                   12.9123(5)
_cell_length_c                   7.4057(2)
_cell_angle_alpha                90
_cell_angle_beta                 98.710(2)
_cell_angle_gamma                90
_cell_volume                     1626.58(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    9895
_cell_measurement_theta_min      2.3947
_cell_measurement_theta_max      29.5991

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.276
_exptl_crystal_F_000             1048
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    10.424
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4765
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      223(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine focus sealed X-ray tube'
_diffrn_measurement_device_type  'Bruker AXS SMART APEX2 CCD diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            52795
_diffrn_reflns_av_unetI/netI     0.0154
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         1.980
_diffrn_reflns_theta_max         29.711
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4616
_reflns_number_gt                4053
_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       'APEX2 V2013.10.0 (Bruker, 2013)'
_computing_cell_refinement       'APEX2 V2013.10.0 (Bruker, 2013)'
_computing_data_reduction        'APEX2 V2013.10.0 (Bruker, 2013)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0182P)²+1.3523P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4616
_refine_ls_number_parameters     235
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0218
_refine_ls_R_factor_gt           0.0172
_refine_ls_wR_factor_ref         0.0395
_refine_ls_wR_factor_gt          0.0384
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_restrained_S_all      1.075
_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 0.26086(2) 0.58286(2) 0.35383(2) 0.02067(3) Uani 1 1 d . . . . .
O1 O 0.37809(11) 0.60972(15) 0.6370(2) 0.0283(4) Uani 1 1 d . . . . .
O2 O 0.32140(13) 0.39837(16) 0.3781(3) 0.0395(5) Uani 1 1 d . . . . .
O3 O 0.24745(11) 0.42391(15) 0.1187(2) 0.0305(4) Uani 1 1 d . . . . .
O4 O 0.2926(2) 0.2711(2) 0.1910(4) 0.0789(10) Uani 1 1 d . . . . .
N1 N 0.13639(12) 0.47534(17) 0.3814(3) 0.0255(4) Uani 1 1 d . . . . .
N2 N 0.24528(12) 0.51345(17) 0.6749(3) 0.0229(4) Uani 1 1 d . . . . .
N3 N 0.30084(12) 0.53494(18) 0.8211(3) 0.0248(4) Uani 1 1 d . . . . .
H3 H 0.294228 0.517117 0.931024 0.030 Uiso 1 1 calc R U . . .
N4 N 0.40596(13) 0.57964(17) 1.1205(3) 0.0271(4) Uani 1 1 d . . . . .
N5 N 0.28759(14) 0.36217(19) 0.2288(3) 0.0322(5) Uani 1 1 d . . . . .
C1 C 0.08150(16) 0.4548(2) 0.2375(4) 0.0333(6) Uani 1 1 d . . . . .
H1 H 0.087399 0.483698 0.123846 0.040 Uiso 1 1 calc R U . . .
C2 C 0.01659(17) 0.3932(2) 0.2476(4) 0.0378(7) Uani 1 1 d . . . . .
H2 H -0.020506 0.380589 0.143099 0.045 Uiso 1 1 calc R U . . .
C3 C 0.00724(18) 0.3509(3) 0.4121(4) 0.0421(7) Uani 1 1 d . . . . .
H3A H -0.036828 0.309625 0.422950 0.051 Uiso 1 1 calc R U . . .
C4 C 0.06388(18) 0.3698(3) 0.5629(4) 0.0400(7) Uani 1 1 d . . . . .
H4 H 0.059355 0.340431 0.676981 0.048 Uiso 1 1 calc R U . . .
C5 C 0.12756(15) 0.4331(2) 0.5424(3) 0.0266(5) Uani 1 1 d . . . . .
C6 C 0.18774(16) 0.4554(2) 0.6991(3) 0.0288(5) Uani 1 1 d . . . . .
H6 H 0.184100 0.427763 0.814967 0.035 Uiso 1 1 calc R U . . .
C7 C 0.36622(14) 0.58451(18) 0.7906(3) 0.0222(5) Uani 1 1 d . . . . .
C8 C 0.42588(15) 0.60455(18) 0.9574(3) 0.0222(5) Uani 1 1 d . . . . .
C9 C 0.49836(15) 0.64213(19) 0.9326(3) 0.0266(5) Uani 1 1 d . . . . .
H9 H 0.509150 0.657989 0.815015 0.032 Uiso 1 1 calc R U . . .
C10 C 0.55545(16) 0.6562(2) 1.0856(4) 0.0313(6) Uani 1 1 d . . . . .
H10 H 0.605450 0.682294 1.074074 0.038 Uiso 1 1 calc R U . . .
C11 C 0.53637(16) 0.6306(2) 1.2544(4) 0.0305(6) Uani 1 1 d . . . . .
H11 H 0.573499 0.638382 1.360463 0.037 Uiso 1 1 calc R U . . .
C12 C 0.46212(17) 0.5934(2) 1.2654(3) 0.0321(6) Uani 1 1 d . . . . .
H12 H 0.450087 0.576558 1.381523 0.039 Uiso 1 1 calc R U . . .
O5 O 0.24844(12) 0.75589(17) 0.5647(3) 0.0422(5) Uani 1 1 d . . . . .
O6 O 0.14215(12) 0.72807(16) 0.3769(3) 0.0389(5) Uani 1 1 d . . . . .
O7 O 0.16014(12) 0.87514(15) 0.5178(3) 0.0328(4) Uani 1 1 d . . . . .
N6 N 0.18297(12) 0.78658(16) 0.4856(3) 0.0244(4) 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 N1 2.586(2) . ?
Pb N2 2.5923(19) . ?
Pb O2 2.595(2) . ?
Pb O3 2.6790(19) . ?
Pb O1 2.7032(17) . ?
Pb O5 2.753(2) . ?
O1 C7 1.229(3) . ?
O2 N5 1.259(3) . ?
O3 N5 1.268(3) . ?
O4 N5 1.214(3) . ?
N1 C1 1.339(3) . ?
N1 C5 1.341(3) . ?
N2 C6 1.276(3) . ?
N2 N3 1.360(3) . ?
N3 C7 1.343(3) . ?
N3 H3 0.8700 . ?
N4 C12 1.343(3) . ?
N4 C8 1.344(3) . ?
C1 C2 1.383(4) . ?
C1 H1 0.9400 . ?
C2 C3 1.366(4) . ?
C2 H2 0.9400 . ?
C3 C4 1.388(4) . ?
C3 H3A 0.9400 . ?
C4 C5 1.393(4) . ?
C4 H4 0.9400 . ?
C5 C6 1.463(3) . ?
C6 H6 0.9400 . ?
C7 C8 1.505(3) . ?
C8 C9 1.376(4) . ?
C9 C10 1.395(4) . ?
C9 H9 0.9400 . ?
C10 C11 1.380(4) . ?
C10 H10 0.9400 . ?
C11 C12 1.379(4) . ?
C11 H11 0.9400 . ?
C12 H12 0.9400 . ?
O5 N6 1.253(3) . ?
O6 N6 1.241(3) . ?
O7 N6 1.244(3) . ?

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 Pb N2 62.63(6) . . ?
N1 Pb O2 80.24(7) . . ?
N2 Pb O2 73.47(7) . . ?
N1 Pb O3 69.47(6) . . ?
N2 Pb O3 108.70(6) . . ?
O2 Pb O3 48.39(6) . . ?
N1 Pb O1 122.50(6) . . ?
N2 Pb O1 60.10(6) . . ?
O2 Pb O1 79.60(6) . . ?
O3 Pb O1 125.69(6) . . ?
N1 Pb O5 104.75(7) . . ?
N2 Pb O5 74.49(7) . . ?
O2 Pb O5 140.41(6) . . ?
O3 Pb O5 169.80(6) . . ?
O1 Pb O5 64.44(6) . . ?
C7 O1 Pb 118.34(16) . . ?
N5 O2 Pb 98.79(15) . . ?
N5 O3 Pb 94.51(14) . . ?
C1 N1 C5 117.8(2) . . ?
C1 N1 Pb 122.44(17) . . ?
C5 N1 Pb 119.70(16) . . ?
C6 N2 N3 118.3(2) . . ?
C6 N2 Pb 121.50(15) . . ?
N3 N2 Pb 120.12(15) . . ?
C7 N3 N2 117.97(19) . . ?
C7 N3 H3 121.0 . . ?
N2 N3 H3 121.0 . . ?
C12 N4 C8 115.8(2) . . ?
O4 N5 O2 121.5(2) . . ?
O4 N5 O3 120.7(2) . . ?
O2 N5 O3 117.8(2) . . ?
N1 C1 C2 123.3(3) . . ?
N1 C1 H1 118.4 . . ?
C2 C1 H1 118.4 . . ?
C3 C2 C1 118.9(3) . . ?
C3 C2 H2 120.5 . . ?
C1 C2 H2 120.5 . . ?
C2 C3 C4 118.9(3) . . ?
C2 C3 H3A 120.5 . . ?
C4 C3 H3A 120.5 . . ?
C3 C4 C5 118.9(3) . . ?
C3 C4 H4 120.5 . . ?
C5 C4 H4 120.5 . . ?
N1 C5 C4 122.2(2) . . ?
N1 C5 C6 117.6(2) . . ?
C4 C5 C6 120.2(2) . . ?
N2 C6 C5 118.4(2) . . ?
N2 C6 H6 120.8 . . ?
C5 C6 H6 120.8 . . ?
O1 C7 N3 122.9(2) . . ?
O1 C7 C8 121.7(2) . . ?
N3 C7 C8 115.4(2) . . ?
N4 C8 C9 124.4(2) . . ?
N4 C8 C7 117.5(2) . . ?
C9 C8 C7 118.1(2) . . ?
C8 C9 C10 118.6(2) . . ?
C8 C9 H9 120.7 . . ?
C10 C9 H9 120.7 . . ?
C11 C10 C9 118.0(3) . . ?
C11 C10 H10 121.0 . . ?
C9 C10 H10 121.0 . . ?
C12 C11 C10 119.1(2) . . ?
C12 C11 H11 120.4 . . ?
C10 C11 H11 120.4 . . ?
N4 C12 C11 124.1(3) . . ?
N4 C12 H12 118.0 . . ?
C11 C12 H12 118.0 . . ?
N6 O5 Pb 97.64(14) . . ?
O6 N6 O7 121.3(2) . . ?
O6 N6 O5 119.4(2) . . ?
O7 N6 O5 119.3(2) . . ?

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 171.5(2) . . . . ?
Pb N2 N3 C7 -5.8(3) . . . . ?
Pb O2 N5 O4 -171.9(3) . . . . ?
Pb O2 N5 O3 7.6(3) . . . . ?
Pb O3 N5 O4 172.2(3) . . . . ?
Pb O3 N5 O2 -7.3(3) . . . . ?
C5 N1 C1 C2 0.4(4) . . . . ?
Pb N1 C1 C2 176.6(2) . . . . ?
N1 C1 C2 C3 0.1(5) . . . . ?
C1 C2 C3 C4 -1.0(5) . . . . ?
C2 C3 C4 C5 1.3(5) . . . . ?
C1 N1 C5 C4 -0.1(4) . . . . ?
Pb N1 C5 C4 -176.4(2) . . . . ?
C1 N1 C5 C6 179.8(3) . . . . ?
Pb N1 C5 C6 3.5(3) . . . . ?
C3 C4 C5 N1 -0.7(5) . . . . ?
C3 C4 C5 C6 179.3(3) . . . . ?
N3 N2 C6 C5 179.4(2) . . . . ?
Pb N2 C6 C5 -3.3(3) . . . . ?
N1 C5 C6 N2 -0.2(4) . . . . ?
C4 C5 C6 N2 179.8(3) . . . . ?
Pb O1 C7 N3 6.9(3) . . . . ?
Pb O1 C7 C8 -175.11(16) . . . . ?
N2 N3 C7 O1 -1.0(4) . . . . ?
N2 N3 C7 C8 -179.1(2) . . . . ?
C12 N4 C8 C9 0.0(4) . . . . ?
C12 N4 C8 C7 176.5(2) . . . . ?
O1 C7 C8 N4 176.3(2) . . . . ?
N3 C7 C8 N4 -5.5(3) . . . . ?
O1 C7 C8 C9 -6.9(4) . . . . ?
N3 C7 C8 C9 171.3(2) . . . . ?
N4 C8 C9 C10 -0.3(4) . . . . ?
C7 C8 C9 C10 -176.9(2) . . . . ?
C8 C9 C10 C11 0.6(4) . . . . ?
C9 C10 C11 C12 -0.6(4) . . . . ?
C8 N4 C12 C11 0.1(4) . . . . ?
C10 C11 C12 N4 0.2(4) . . . . ?
Pb O5 N6 O6 12.7(3) . . . . ?
Pb O5 N6 O7 -167.42(19) . . . . ?

_refine_diff_density_max         0.993
_refine_diff_density_min         -0.818
_refine_diff_density_rms         0.090

####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1960845'
loop_
_audit_author_name
_audit_author_address
'Damir Safin'
;University of Tyumen
Russia
;
_audit_update_record             
;
2019-10-22 deposited with the CCDC.	2020-03-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H9 N4 O Pb, Cl O4'
_chemical_formula_sum            'C12 H9 Cl N4 O5 Pb'
_chemical_formula_weight         531.87

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'

_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                   10.4298(16)
_cell_length_b                   9.4400(12)
_cell_length_c                   15.1770(18)
_cell_angle_alpha                90
_cell_angle_beta                 105.911(15)
_cell_angle_gamma                90
_cell_volume                     1437.0(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    985
_cell_measurement_theta_min      3.54
_cell_measurement_theta_max      24.80

_exptl_crystal_description       plate
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.458
_exptl_crystal_F_000             992
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.12
_exptl_absorpt_coefficient_mu    11.959
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.1605
_exptl_absorpt_correction_T_max  0.2143
_exptl_absorpt_process_details   'Bruker SADABS, 2010'

_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4988
_diffrn_reflns_av_unetI/netI     0.1610
_diffrn_reflns_av_R_equivalents  0.1217
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.529
_diffrn_reflns_theta_max         25.348
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             2626
_reflns_number_gt                1745
_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       'APEX2 v2011.4.0 (Bruker-AXS, 2011)'
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2011)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2011)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'WinGX (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)+(0.0782P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0022(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2626
_refine_ls_number_parameters     237
_refine_ls_number_restraints     63
_refine_ls_R_factor_all          0.1149
_refine_ls_R_factor_gt           0.0732
_refine_ls_wR_factor_ref         0.1901
_refine_ls_wR_factor_gt          0.1579
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_restrained_S_all      0.987
_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
Pb1 Pb 0.57636(7) 0.42535(7) 0.36003(4) 0.0268(4) Uani 1 1 d . . . . .
N1 N 0.6361(16) 0.1816(13) 0.4483(9) 0.028(4) Uani 1 1 d . . . . .
N2 N 0.4342(15) 0.3547(15) 0.4545(8) 0.026(3) Uani 1 1 d . . . . .
N3 N 0.3244(17) 0.4375(14) 0.4535(10) 0.033(4) Uani 1 1 d . . . . .
N4 N 0.0191(16) 0.7702(16) 0.2725(8) 0.033(4) Uani 1 1 d . . . . .
O1 O 0.3603(12) 0.5285(13) 0.3205(7) 0.033(3) Uani 1 1 d . . . . .
C1 C 0.7374(19) 0.098(2) 0.4450(15) 0.040(5) Uani 1 1 d . . . . .
H1 H 0.7719 0.1042 0.3948 0.049 Uiso 1 1 calc R U . . .
C2 C 0.793(2) 0.0036(19) 0.5134(13) 0.043(5) Uani 1 1 d . . . . .
H2 H 0.8635 -0.0539 0.5096 0.052 Uiso 1 1 calc R U . . .
C3 C 0.7409(19) -0.005(2) 0.5889(11) 0.037(5) Uani 1 1 d . . . . .
H3 H 0.7787 -0.0658 0.6371 0.044 Uiso 1 1 calc R U . . .
C4 C 0.6359(16) 0.0760(18) 0.5912(11) 0.026(4) Uani 1 1 d . . . . .
H4 H 0.5988 0.0701 0.6402 0.032 Uiso 1 1 calc R U . . .
C5 C 0.5830(16) 0.1698(18) 0.5181(10) 0.022(4) Uani 1 1 d . U . . .
C6 C 0.4710(16) 0.2561(17) 0.5180(10) 0.021(4) Uani 1 1 d . . . . .
H6 H 0.4248 0.2433 0.5618 0.025 Uiso 1 1 calc R U . . .
C7 C 0.2922(15) 0.5223(18) 0.3779(10) 0.019(3) Uani 1 1 d . U . . .
C8 C 0.1690(16) 0.6070(17) 0.3664(10) 0.020(4) Uani 1 1 d . U . . .
C9 C 0.088(2) 0.6068(18) 0.4271(11) 0.033(5) Uani 1 1 d . . . . .
H9 H 0.1111 0.5497 0.4790 0.039 Uiso 1 1 calc R U . . .
C10 C -0.019(2) 0.6865(18) 0.4111(12) 0.036(5) Uani 1 1 d . . . . .
H10 H -0.0696 0.6867 0.4527 0.043 Uiso 1 1 calc R U . . .
C11 C -0.0567(17) 0.770(2) 0.3337(11) 0.031(4) Uani 1 1 d . . . . .
H11 H -0.1330 0.8260 0.3230 0.037 Uiso 1 1 calc R U . . .
C12 C 0.1304(19) 0.6919(19) 0.2914(11) 0.033(4) Uani 1 1 d . U . . .
H12 H 0.1837 0.6958 0.2514 0.040 Uiso 1 1 calc R U . . .
Cl1 Cl 0.4359(5) 0.2300(6) 0.7881(3) 0.0439(13) Uani 1 1 d . . . . .
O2 O 0.3605(19) 0.1624(16) 0.8427(11) 0.076(5) Uani 1 1 d . . . . .
O3 O 0.433(3) 0.387(3) 0.801(2) 0.050(9) Uani 0.61(5) 1 d D U P A .
O4 O 0.372(3) 0.228(5) 0.690(2) 0.073(11) Uani 0.61(5) 1 d D U P A .
O5 O 0.569(3) 0.192(3) 0.797(3) 0.066(10) Uani 0.61(5) 1 d D U P A .
O3A O 0.373(5) 0.347(5) 0.755(4) 0.060(16) Uani 0.39(5) 1 d D U P A 2
O4A O 0.406(6) 0.143(6) 0.711(3) 0.072(17) Uani 0.39(5) 1 d D U P A 2
O5A O 0.557(5) 0.223(6) 0.850(3) 0.082(19) Uani 0.39(5) 1 d D U P A 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
Pb1 O1 2.376(11) . ?
Pb1 N2 2.422(15) . ?
Pb1 N4 2.467(13) 2_545 ?
Pb1 N1 2.649(13) . ?
N1 C5 1.33(2) . ?
N1 C1 1.33(2) . ?
N2 C6 1.319(19) . ?
N2 N3 1.38(2) . ?
N3 C7 1.36(2) . ?
N4 C12 1.34(2) . ?
N4 C11 1.38(2) . ?
N4 Pb1 2.467(13) 2 ?
O1 C7 1.268(18) . ?
C1 C2 1.37(3) . ?
C1 H1 0.9300 . ?
C2 C3 1.40(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.34(2) . ?
C3 H3 0.9300 . ?
C4 C5 1.41(2) . ?
C4 H4 0.9300 . ?
C5 C6 1.42(2) . ?
C6 H6 0.9300 . ?
C7 C8 1.48(2) . ?
C8 C12 1.36(2) . ?
C8 C9 1.41(2) . ?
C9 C10 1.31(2) . ?
C9 H9 0.9300 . ?
C10 C11 1.38(2) . ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
Cl1 O3A 1.31(4) . ?
Cl1 O5A 1.35(5) . ?
Cl1 O4A 1.39(5) . ?
Cl1 O5 1.40(3) . ?
Cl1 O2 1.439(16) . ?
Cl1 O4 1.46(3) . ?
Cl1 O3 1.50(3) . ?
O3 O3A 0.89(3) . ?
O4 O4A 0.90(3) . ?
O4 O3A 1.50(5) . ?
O5 O5A 0.89(3) . ?

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 N2 64.5(4) . . ?
O1 Pb1 N4 83.9(5) . 2_545 ?
N2 Pb1 N4 98.2(5) . 2_545 ?
O1 Pb1 N1 124.0(4) . . ?
N2 Pb1 N1 63.8(5) . . ?
N4 Pb1 N1 83.3(4) 2_545 . ?
C5 N1 C1 119.3(15) . . ?
C5 N1 Pb1 112.6(11) . . ?
C1 N1 Pb1 125.1(12) . . ?
C6 N2 N3 118.7(14) . . ?
C6 N2 Pb1 121.6(11) . . ?
N3 N2 Pb1 118.5(10) . . ?
C7 N3 N2 110.7(14) . . ?
C12 N4 C11 118.7(14) . . ?
C12 N4 Pb1 129.4(12) . 2 ?
C11 N4 Pb1 111.9(12) . 2 ?
C7 O1 Pb1 118.6(10) . . ?
N1 C1 C2 122(2) . . ?
N1 C1 H1 118.9 . . ?
C2 C1 H1 118.9 . . ?
C1 C2 C3 119(2) . . ?
C1 C2 H2 120.7 . . ?
C3 C2 H2 120.7 . . ?
C4 C3 C2 119.4(18) . . ?
C4 C3 H3 120.3 . . ?
C2 C3 H3 120.3 . . ?
C3 C4 C5 118.9(16) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 H4 120.6 . . ?
N1 C5 C4 121.5(15) . . ?
N1 C5 C6 118.2(14) . . ?
C4 C5 C6 120.3(14) . . ?
N2 C6 C5 118.6(14) . . ?
N2 C6 H6 120.7 . . ?
C5 C6 H6 120.7 . . ?
O1 C7 N3 123.4(15) . . ?
O1 C7 C8 121.6(14) . . ?
N3 C7 C8 115.0(14) . . ?
C12 C8 C9 117.1(16) . . ?
C12 C8 C7 117.8(15) . . ?
C9 C8 C7 125.2(15) . . ?
C10 C9 C8 120.6(16) . . ?
C10 C9 H9 119.7 . . ?
C8 C9 H9 119.7 . . ?
C9 C10 C11 121.2(17) . . ?
C9 C10 H10 119.4 . . ?
C11 C10 H10 119.4 . . ?
N4 C11 C10 119.3(16) . . ?
N4 C11 H11 120.3 . . ?
C10 C11 H11 120.3 . . ?
N4 C12 C8 123.1(17) . . ?
N4 C12 H12 118.5 . . ?
C8 C12 H12 118.5 . . ?
O3A Cl1 O5A 125(3) . . ?
O3A Cl1 O4A 102(2) . . ?
O5A Cl1 O4A 120(3) . . ?
O3A Cl1 O5 129(3) . . ?
O5A Cl1 O5 37.5(16) . . ?
O4A Cl1 O5 85(2) . . ?
O3A Cl1 O2 107(2) . . ?
O5A Cl1 O2 98(3) . . ?
O4A Cl1 O2 101(2) . . ?
O5 Cl1 O2 120.7(16) . . ?
O3A Cl1 O4 65(2) . . ?
O5A Cl1 O4 142(3) . . ?
O4A Cl1 O4 36.6(15) . . ?
O5 Cl1 O4 105.1(19) . . ?
O2 Cl1 O4 114.5(15) . . ?
O3A Cl1 O3 36.1(17) . . ?
O5A Cl1 O3 90(3) . . ?
O4A Cl1 O3 134(2) . . ?
O5 Cl1 O3 107.2(17) . . ?
O2 Cl1 O3 109.2(12) . . ?
O4 Cl1 O3 97.6(18) . . ?
O3A O3 Cl1 60(4) . . ?
O4A O4 Cl1 68(4) . . ?
O4A O4 O3A 120(5) . . ?
Cl1 O4 O3A 53(2) . . ?
O5A O5 Cl1 68(4) . . ?
O3 O3A Cl1 84(4) . . ?
O3 O3A O4 136(5) . . ?
Cl1 O3A O4 62(2) . . ?
O4 O4A Cl1 76(4) . . ?
O5 O5A Cl1 74(4) . . ?

_refine_diff_density_max         2.947
_refine_diff_density_min         -3.284
_refine_diff_density_rms         0.401

####################################################################### 
# 
# 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 1960846'
loop_
_audit_author_name
_audit_author_address
'Damir Safin'
;University of Tyumen
Russia
;
_audit_update_record             
;
2019-10-22 deposited with the CCDC.	2020-03-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H24 N12 O8 Pb2 S2'
_chemical_formula_sum            'C28 H24 N12 O8 Pb2 S2'
_chemical_formula_weight         1135.09

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'C c'
_space_group_name_Hall           'C -2yc'

_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, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   7.0192(4)
_cell_length_b                   16.1126(7)
_cell_length_c                   15.0998(8)
_cell_angle_alpha                90
_cell_angle_beta                 102.955(4)
_cell_angle_gamma                90
_cell_volume                     1664.28(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3749
_cell_measurement_theta_min      2.66
_cell_measurement_theta_max      28.37

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.265
_exptl_crystal_F_000             1072
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_exptl_absorpt_coefficient_mu    10.298
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.1605
_exptl_absorpt_correction_T_max  0.2143
_exptl_absorpt_process_details   'Bruker SADABS, 2010'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15951
_diffrn_reflns_av_unetI/netI     0.1005
_diffrn_reflns_av_R_equivalents  0.1257
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.528
_diffrn_reflns_theta_max         29.161
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4471
_reflns_number_gt                4246
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.995
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_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       'APEX2 v2011.4.0 (Bruker-AXS, 2011)'
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2011)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2011)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0536P)²+8.3600P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.257(17)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4471
_refine_ls_number_parameters     236
_refine_ls_number_restraints     35
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0423
_refine_ls_wR_factor_ref         0.1055
_refine_ls_wR_factor_gt          0.1043
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.056
_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 0.18615(6) 0.27980(2) 0.58793(5) 0.01214(13) Uani 1 1 d . . . . .
S1 S 0.7645(5) 0.1988(3) 0.5004(3) 0.0301(8) Uani 1 1 d . . . . .
O1 O 0.1830(17) 0.3957(7) 0.4644(6) 0.021(2) Uani 1 1 d . . . . .
N1 N 0.2077(15) 0.1228(6) 0.5514(7) 0.0122(18) Uani 1 1 d . . . . .
N2 N 0.2475(18) 0.2372(7) 0.4278(7) 0.0108(18) Uani 1 1 d . . . . .
N3 N 0.2650(15) 0.2995(7) 0.3692(7) 0.0134(18) Uani 1 1 d . . . . .
H3N H 0.2994 0.2891 0.3191 0.016 Uiso 1 1 calc R U . . .
N4 N 0.2590(19) 0.5729(8) 0.2017(8) 0.019(2) Uani 1 1 d . . . . .
N5 N 0.5423(16) 0.2789(8) 0.6076(10) 0.023(3) Uani 1 1 d . . . . .
N6 N 0.185(2) 0.1910(8) 0.7760(7) 0.019(2) Uani 1 1 d . . . . .
O2 O 0.3361(16) 0.2123(7) 0.7480(8) 0.024(2) Uani 1 1 d . . . . .
O3 O 0.026(2) 0.2241(7) 0.7417(9) 0.026(2) Uani 1 1 d . . . . .
O4 O 0.197(3) 0.1365(10) 0.8346(9) 0.045(4) Uani 1 1 d . . . . .
C1 C 0.172(2) 0.0655(9) 0.6082(8) 0.021(3) Uani 1 1 d . . . . .
H1 H 0.1389 0.0825 0.6618 0.025 Uiso 1 1 calc R U . . .
C2 C 0.181(5) -0.0212(7) 0.591(2) 0.022(2) Uani 1 1 d . U . . .
H2 H 0.1447 -0.0598 0.6296 0.027 Uiso 1 1 calc R U . . .
C3 C 0.246(2) -0.0471(8) 0.5153(9) 0.020(2) Uani 1 1 d . U . . .
H3 H 0.2662 -0.1031 0.5054 0.023 Uiso 1 1 calc R U . . .
C4 C 0.281(2) 0.0120(8) 0.4552(8) 0.018(2) Uani 1 1 d . . . . .
H4 H 0.3202 -0.0042 0.4030 0.021 Uiso 1 1 calc R U . . .
C5 C 0.2564(16) 0.0970(7) 0.4720(7) 0.0097(18) Uani 1 1 d . U . . .
C6 C 0.2708(19) 0.1616(9) 0.4040(7) 0.0120(19) Uani 1 1 d . U . . .
C7 C 0.298(2) 0.1362(9) 0.3126(8) 0.019(2) Uani 1 1 d . U . . .
H7A H 0.3120 0.0770 0.3110 0.029 Uiso 1 1 calc R U . . .
H7B H 0.1855 0.1528 0.2671 0.029 Uiso 1 1 calc R U . . .
H7C H 0.4124 0.1623 0.3011 0.029 Uiso 1 1 calc R U . . .
C8 C 0.2272(18) 0.3777(8) 0.3914(8) 0.013(2) Uani 1 1 d . . . . .
C9 C 0.2418(17) 0.4431(8) 0.3237(8) 0.014(2) Uani 1 1 d . . . . .
C10 C 0.2872(19) 0.5232(8) 0.3548(8) 0.017(2) Uani 1 1 d . . . . .
H10 H 0.3119 0.5349 0.4167 0.020 Uiso 1 1 calc R U . . .
C11 C 0.295(2) 0.5860(8) 0.2926(9) 0.018(2) Uani 1 1 d . . . . .
H11 H 0.3274 0.6394 0.3143 0.022 Uiso 1 1 calc R U . . .
C12 C 0.213(2) 0.4951(9) 0.1724(9) 0.021(3) Uani 1 1 d . . . . .
H12 H 0.1875 0.4851 0.1102 0.025 Uiso 1 1 calc R U . . .
C13 C 0.2024(19) 0.4289(9) 0.2298(8) 0.017(2) Uani 1 1 d . . . . .
H13 H 0.1695 0.3761 0.2065 0.021 Uiso 1 1 calc R U . . .
C15 C 0.6340(17) 0.2455(9) 0.5627(9) 0.016(2) 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 N5 2.451(11) . ?
Pb N1 2.602(10) . ?
Pb O1 2.635(10) . ?
Pb N2 2.640(11) . ?
Pb O2 2.645(11) . ?
Pb N4 2.907(12) 2_565 ?
S1 C15 1.636(14) . ?
O1 C8 1.244(15) . ?
N1 C1 1.322(16) . ?
N1 C5 1.382(13) . ?
N2 C6 1.291(17) . ?
N2 N3 1.362(15) . ?
N3 C8 1.346(17) . ?
N3 H3N 0.8600 . ?
N4 C12 1.344(19) . ?
N4 C11 1.355(18) . ?
N5 C15 1.166(19) . ?
N6 O4 1.234(18) . ?
N6 O3 1.242(19) . ?
N6 O2 1.276(18) . ?
C1 C2 1.427(19) . ?
C1 H1 0.9300 . ?
C2 C3 1.38(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.372(18) . ?
C3 H3 0.9300 . ?
C4 C5 1.411(17) . ?
C4 H4 0.9300 . ?
C5 C6 1.481(17) . ?
C6 C7 1.491(16) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 C9 1.488(17) . ?
C9 C10 1.386(18) . ?
C9 C13 1.401(17) . ?
C10 C11 1.390(18) . ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
C12 C13 1.388(18) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?

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
N5 Pb N1 85.1(4) . . ?
N5 Pb O1 86.4(4) . . ?
N1 Pb O1 122.0(3) . . ?
N5 Pb N2 74.8(4) . . ?
N1 Pb N2 61.6(3) . . ?
O1 Pb N2 60.9(3) . . ?
N5 Pb O2 72.6(4) . . ?
N1 Pb O2 76.3(3) . . ?
O1 Pb O2 151.2(4) . . ?
N2 Pb O2 128.1(3) . . ?
N5 Pb N4 83.9(4) . 2_565 ?
N1 Pb N4 155.3(3) . 2_565 ?
O1 Pb N4 79.2(4) . 2_565 ?
N2 Pb N4 135.3(4) . 2_565 ?
O2 Pb N4 79.3(4) . 2_565 ?
C8 O1 Pb 119.9(9) . . ?
C1 N1 C5 118.3(11) . . ?
C1 N1 Pb 120.8(8) . . ?
C5 N1 Pb 120.9(7) . . ?
C6 N2 N3 118.6(11) . . ?
C6 N2 Pb 123.8(8) . . ?
N3 N2 Pb 117.5(8) . . ?
C8 N3 N2 118.4(10) . . ?
C8 N3 H3N 120.8 . . ?
N2 N3 H3N 120.8 . . ?
C12 N4 C11 117.1(12) . . ?
C15 N5 Pb 127.8(10) . . ?
O4 N6 O3 121.0(15) . . ?
O4 N6 O2 120.0(14) . . ?
O3 N6 O2 118.9(13) . . ?
N6 O2 Pb 102.9(8) . . ?
N1 C1 C2 122.6(16) . . ?
N1 C1 H1 118.7 . . ?
C2 C1 H1 118.7 . . ?
C3 C2 C1 119.1(18) . . ?
C3 C2 H2 120.5 . . ?
C1 C2 H2 120.5 . . ?
C4 C3 C2 118.3(13) . . ?
C4 C3 H3 120.8 . . ?
C2 C3 H3 120.8 . . ?
C3 C4 C5 120.5(12) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?
N1 C5 C4 120.7(11) . . ?
N1 C5 C6 117.3(10) . . ?
C4 C5 C6 121.8(11) . . ?
N2 C6 C5 116.0(10) . . ?
N2 C6 C7 124.5(12) . . ?
C5 C6 C7 119.4(12) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O1 C8 N3 122.8(11) . . ?
O1 C8 C9 120.9(12) . . ?
N3 C8 C9 116.3(11) . . ?
C10 C9 C13 118.3(11) . . ?
C10 C9 C8 118.2(11) . . ?
C13 C9 C8 123.4(12) . . ?
C9 C10 C11 119.3(12) . . ?
C9 C10 H10 120.3 . . ?
C11 C10 H10 120.3 . . ?
N4 C11 C10 123.0(13) . . ?
N4 C11 H11 118.5 . . ?
C10 C11 H11 118.5 . . ?
N4 C12 C13 123.6(12) . . ?
N4 C12 H12 118.2 . . ?
C13 C12 H12 118.2 . . ?
C12 C13 C9 118.7(12) . . ?
C12 C13 H13 120.6 . . ?
C9 C13 H13 120.6 . . ?
N5 C15 S1 179.5(13) . . ?

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 C8 175.5(12) . . . . ?
Pb N2 N3 C8 -7.8(15) . . . . ?
O4 N6 O2 Pb 158.3(12) . . . . ?
O3 N6 O2 Pb -19.7(14) . . . . ?
C5 N1 C1 C2 0(3) . . . . ?
Pb N1 C1 C2 179.8(19) . . . . ?
N1 C1 C2 C3 5(4) . . . . ?
C1 C2 C3 C4 -6(3) . . . . ?
C2 C3 C4 C5 2(2) . . . . ?
C1 N1 C5 C4 -4.4(18) . . . . ?
Pb N1 C5 C4 175.8(9) . . . . ?
C1 N1 C5 C6 172.3(12) . . . . ?
Pb N1 C5 C6 -7.5(13) . . . . ?
C3 C4 C5 N1 3.4(19) . . . . ?
C3 C4 C5 C6 -173.1(12) . . . . ?
N3 N2 C6 C5 178.0(10) . . . . ?
Pb N2 C6 C5 1.5(16) . . . . ?
N3 N2 C6 C7 -6(2) . . . . ?
Pb N2 C6 C7 177.4(10) . . . . ?
N1 C5 C6 N2 3.9(17) . . . . ?
C4 C5 C6 N2 -179.4(12) . . . . ?
N1 C5 C6 C7 -172.2(11) . . . . ?
C4 C5 C6 C7 4.4(18) . . . . ?
Pb O1 C8 N3 4.6(17) . . . . ?
Pb O1 C8 C9 -175.1(8) . . . . ?
N2 N3 C8 O1 2.3(19) . . . . ?
N2 N3 C8 C9 -178.0(10) . . . . ?
O1 C8 C9 C10 26.7(18) . . . . ?
N3 C8 C9 C10 -153.0(12) . . . . ?
O1 C8 C9 C13 -149.9(13) . . . . ?
N3 C8 C9 C13 30.4(17) . . . . ?
C13 C9 C10 C11 -1.1(18) . . . . ?
C8 C9 C10 C11 -177.9(12) . . . . ?
C12 N4 C11 C10 0(2) . . . . ?
C9 C10 C11 N4 1(2) . . . . ?
C11 N4 C12 C13 0(2) . . . . ?
N4 C12 C13 C9 0(2) . . . . ?
C10 C9 C13 C12 1.0(18) . . . . ?
C8 C9 C13 C12 177.6(12) . . . . ?

_refine_diff_density_max         4.377
_refine_diff_density_min         -3.259
_refine_diff_density_rms         0.240

