# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1992559'
loop_
_audit_author_name
_audit_author_address
'Damir Safin' 'University of Tyumen'
_audit_update_record             
;
2020-03-25 deposited with the CCDC.	2020-07-17 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 H10 I2 N4 O Pb'
_chemical_formula_sum            'C12 H10 I2 N4 O Pb'
_chemical_formula_weight         687.23

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'
I I -0.4742 1.8119 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   4.6530(15)
_cell_length_b                   11.365(2)
_cell_length_c                   16.636(4)
_cell_angle_alpha                70.590(18)
_cell_angle_beta                 88.62(2)
_cell_angle_gamma                86.101(19)
_cell_volume                     827.8(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    25
_cell_measurement_theta_min      6
_cell_measurement_theta_max      19

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.757
_exptl_crystal_F_000             612
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_exptl_absorpt_coefficient_mu    13.920
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   
;
        Walker, N. & Stuart, D (1983) Acta. Cryst. A39, 158-166
;
_exptl_absorpt_correction_T_min  0.4887
_exptl_absorpt_correction_T_max  0.5329

_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          X-ray
_diffrn_detector                 'scintillation LiI'
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled ω scans'
_diffrn_detector_area_resol_mean ?

_diffrn_orient_matrix_type       
;
  x-axis points to radiation source
  the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_ub_11      0.050146
_diffrn_orient_matrix_ub_12      0.061475
_diffrn_orient_matrix_ub_13      -0.056475
_diffrn_orient_matrix_ub_21      0.005791
_diffrn_orient_matrix_ub_22      0.066646
_diffrn_orient_matrix_ub_23      0.026749
_diffrn_orient_matrix_ub_31      0.209425
_diffrn_orient_matrix_ub_32      -0.022775
_diffrn_orient_matrix_ub_33      0.01273
_diffrn_standards_number         1
_diffrn_standards_interval_time  60
_diffrn_standards_decay_%        0
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
0 2 5

_diffrn_reflns_number            3581
_diffrn_reflns_av_unetI/netI     0.0711
_diffrn_reflns_av_R_equivalents  0.0667
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.298
_diffrn_reflns_theta_max         26.971
_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             3581
_reflns_number_gt                2280
_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       'CAD4 Express (Enraf Nonius, 1994)'
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND, K. Brandenburg, (1999)'
_computing_publication_material  'Wingx 2013.3 (Farrugia, 1999)'

_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)+(0.0724P)²+4.4243P] 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_number_reflns         3581
_refine_ls_number_parameters     181
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1093
_refine_ls_R_factor_gt           0.0554
_refine_ls_wR_factor_ref         0.1509
_refine_ls_wR_factor_gt          0.1281
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_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 -0.02122(13) 0.23361(6) -0.28383(4) 0.03100(19) Uani 1 1 d . . . . .
I1 I -0.5420(2) 0.43168(10) -0.35415(7) 0.0412(3) Uani 1 1 d . . . . .
I2 I -0.4871(2) 0.02531(10) -0.21123(8) 0.0455(3) Uani 1 1 d . . . . .
N1 N -0.020(3) 0.2877(14) -0.1366(9) 0.049(4) Uani 1 1 d . . . . .
C2 C 0.140(4) 0.3765(16) -0.1288(10) 0.052(5) Uani 1 1 d . . . . .
H2 H 0.2153 0.4330 -0.1776 0.062 Uiso 1 1 calc R U . . .
C3 C 0.196(4) 0.3869(17) -0.0506(11) 0.053(5) Uani 1 1 d . . . . .
H3 H 0.2992 0.4525 -0.0474 0.063 Uiso 1 1 calc R U . . .
C4 C 0.102(3) 0.3012(14) 0.0219(9) 0.029(3) Uani 1 1 d . . . . .
C5 C -0.056(4) 0.2076(15) 0.0130(10) 0.042(4) Uani 1 1 d . . . . .
H5 H -0.1294 0.1484 0.0608 0.051 Uiso 1 1 calc R U . . .
C6 C -0.103(4) 0.202(2) -0.0659(11) 0.058(5) Uani 1 1 d . . . . .
H6 H -0.1976 0.1353 -0.0704 0.070 Uiso 1 1 calc R U . . .
C7 C 0.184(3) 0.3088(13) 0.1066(8) 0.029(3) Uani 1 1 d . . . . .
O7 O 0.412(2) 0.3472(11) 0.1177(7) 0.040(3) Uani 1 1 d . . . . .
N8 N -0.012(3) 0.2709(12) 0.1679(8) 0.037(3) Uani 1 1 d . . . . .
H8 H -0.1766 0.2505 0.1560 0.045 Uiso 1 1 calc R U . . .
N9 N 0.048(3) 0.2640(12) 0.2512(8) 0.037(3) Uani 1 1 d . . . . .
C10 C -0.144(4) 0.2200(16) 0.3053(10) 0.043(4) Uani 1 1 d . . . . .
H10 H -0.3096 0.1920 0.2896 0.052 Uiso 1 1 calc R U . . .
C11 C -0.100(3) 0.2137(15) 0.3937(10) 0.037(4) Uani 1 1 d . . . . .
C12 C 0.089(5) 0.2855(19) 0.4141(11) 0.065(6) Uani 1 1 d . . . . .
H12 H 0.2094 0.3351 0.3732 0.078 Uiso 1 1 calc R U . . .
C13 C 0.096(5) 0.2818(18) 0.4970(11) 0.061(6) Uani 1 1 d . . . . .
H13 H 0.2030 0.3406 0.5083 0.073 Uiso 1 1 calc R U . . .
N14 N -0.034(3) 0.2031(12) 0.5630(8) 0.038(3) Uani 1 1 d . . . . .
C15 C -0.209(6) 0.133(2) 0.5424(12) 0.084(8) Uani 1 1 d . . . . .
H15 H -0.3138 0.0794 0.5861 0.100 Uiso 1 1 calc R U . . .
C16 C -0.251(4) 0.133(2) 0.4630(13) 0.078(8) Uani 1 1 d . . . . .
H16 H -0.3793 0.0796 0.4534 0.094 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 N14 2.685(13) 1_554 ?
Pb1 N1 2.716(14) . ?
Pb1 I1 3.1546(16) . ?
Pb1 I1 3.1961(16) 1_655 ?
Pb1 I2 3.2300(16) . ?
Pb1 I2 3.2687(16) 1_655 ?
I1 Pb1 3.1961(16) 1_455 ?
I2 Pb1 3.2687(16) 1_455 ?
N1 C6 1.32(2) . ?
N1 C2 1.34(2) . ?
C2 C3 1.38(2) . ?
C2 H2 0.9300 . ?
C3 C4 1.36(2) . ?
C3 H3 0.9300 . ?
C4 C5 1.38(2) . ?
C4 C7 1.500(18) . ?
C5 C6 1.36(2) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 O7 1.214(17) . ?
C7 N8 1.333(17) . ?
N8 N9 1.396(17) . ?
N8 H8 0.8600 . ?
N9 C10 1.26(2) . ?
C10 C11 1.47(2) . ?
C10 H10 0.9300 . ?
C11 C12 1.36(2) . ?
C11 C16 1.42(2) . ?
C12 C13 1.37(2) . ?
C12 H12 0.9300 . ?
C13 N14 1.33(2) . ?
C13 H13 0.9300 . ?
N14 C15 1.30(2) . ?
N14 Pb1 2.685(13) 1_556 ?
C15 C16 1.34(2) . ?
C15 H15 0.9300 . ?
C16 H16 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
N14 Pb1 N1 174.6(4) 1_554 . ?
N14 Pb1 I1 84.8(3) 1_554 . ?
N1 Pb1 I1 91.0(3) . . ?
N14 Pb1 I1 89.3(3) 1_554 1_655 ?
N1 Pb1 I1 87.7(3) . 1_655 ?
I1 Pb1 I1 94.22(4) . 1_655 ?
N14 Pb1 I2 90.5(3) 1_554 . ?
N1 Pb1 I2 92.7(3) . . ?
I1 Pb1 I2 87.84(4) . . ?
I1 Pb1 I2 177.90(4) 1_655 . ?
N14 Pb1 I2 94.8(3) 1_554 1_655 ?
N1 Pb1 I2 89.4(3) . 1_655 ?
I1 Pb1 I2 179.20(4) . 1_655 ?
I1 Pb1 I2 86.49(4) 1_655 1_655 ?
I2 Pb1 I2 91.45(4) . 1_655 ?
Pb1 I1 Pb1 94.22(4) . 1_455 ?
Pb1 I2 Pb1 91.45(4) . 1_455 ?
C6 N1 C2 117.6(15) . . ?
C6 N1 Pb1 118.2(12) . . ?
C2 N1 Pb1 121.0(11) . . ?
N1 C2 C3 122.0(16) . . ?
N1 C2 H2 119.0 . . ?
C3 C2 H2 119.0 . . ?
C4 C3 C2 120.1(17) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C3 C4 C5 117.3(14) . . ?
C3 C4 C7 119.1(14) . . ?
C5 C4 C7 123.5(13) . . ?
C6 C5 C4 119.7(15) . . ?
C6 C5 H5 120.1 . . ?
C4 C5 H5 120.1 . . ?
N1 C6 C5 123.1(17) . . ?
N1 C6 H6 118.4 . . ?
C5 C6 H6 118.4 . . ?
O7 C7 N8 123.1(13) . . ?
O7 C7 C4 122.2(13) . . ?
N8 C7 C4 114.8(13) . . ?
C7 N8 N9 120.3(12) . . ?
C7 N8 H8 119.8 . . ?
N9 N8 H8 119.8 . . ?
C10 N9 N8 115.6(13) . . ?
N9 C10 C11 118.8(15) . . ?
N9 C10 H10 120.6 . . ?
C11 C10 H10 120.6 . . ?
C12 C11 C16 115.8(15) . . ?
C12 C11 C10 121.7(16) . . ?
C16 C11 C10 122.5(15) . . ?
C11 C12 C13 117.5(17) . . ?
C11 C12 H12 121.2 . . ?
C13 C12 H12 121.2 . . ?
N14 C13 C12 126.9(17) . . ?
N14 C13 H13 116.5 . . ?
C12 C13 H13 116.5 . . ?
C15 N14 C13 114.0(15) . . ?
C15 N14 Pb1 124.5(12) . 1_556 ?
C13 N14 Pb1 119.8(11) . 1_556 ?
N14 C15 C16 125.0(17) . . ?
N14 C15 H15 117.5 . . ?
C16 C15 H15 117.5 . . ?
C15 C16 C11 120.1(16) . . ?
C15 C16 H16 120.0 . . ?
C11 C16 H16 120.0 . . ?

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 N1 C2 C3 -6(3) . . . . ?
Pb1 N1 C2 C3 -165.0(15) . . . . ?
N1 C2 C3 C4 4(3) . . . . ?
C2 C3 C4 C5 -2(3) . . . . ?
C2 C3 C4 C7 175.5(17) . . . . ?
C3 C4 C5 C6 2(3) . . . . ?
C7 C4 C5 C6 -175.0(17) . . . . ?
C2 N1 C6 C5 6(3) . . . . ?
Pb1 N1 C6 C5 166.0(16) . . . . ?
C4 C5 C6 N1 -4(3) . . . . ?
C3 C4 C7 O7 -32(2) . . . . ?
C5 C4 C7 O7 144.9(16) . . . . ?
C3 C4 C7 N8 147.7(16) . . . . ?
C5 C4 C7 N8 -35(2) . . . . ?
O7 C7 N8 N9 -5(2) . . . . ?
C4 C7 N8 N9 174.9(13) . . . . ?
C7 N8 N9 C10 -175.8(15) . . . . ?
N8 N9 C10 C11 -178.0(14) . . . . ?
N9 C10 C11 C12 20(3) . . . . ?
N9 C10 C11 C16 -159.8(19) . . . . ?
C16 C11 C12 C13 -6(3) . . . . ?
C10 C11 C12 C13 174.2(19) . . . . ?
C11 C12 C13 N14 10(4) . . . . ?
C12 C13 N14 C15 -8(4) . . . . ?
C12 C13 N14 Pb1 -174.1(19) . . . 1_556 ?
C13 N14 C15 C16 3(4) . . . . ?
Pb1 N14 C15 C16 168(2) 1_556 . . . ?
N14 C15 C16 C11 -1(4) . . . . ?
C12 C11 C16 C15 2(4) . . . . ?
C10 C11 C16 C15 -178(2) . . . . ?

_refine_diff_density_max         2.057
_refine_diff_density_min         -2.241
_refine_diff_density_rms         0.312

####################################################################### 
# 
# 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 1992562'
loop_
_audit_author_name
_audit_author_address
'Damir Safin' 'University of Tyumen'
_audit_update_record             
;
2020-03-25 deposited with the CCDC.	2020-07-17 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         'C18 H15 N6 O7 Pb, C H4 O'
_chemical_formula_sum            'C19 H18 N6 O8 Pb'
_chemical_formula_weight         665.58

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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   9.1144(18)
_cell_length_b                   11.331(2)
_cell_length_c                   12.168(2)
_cell_angle_alpha                81.869(3)
_cell_angle_beta                 74.622(4)
_cell_angle_gamma                71.200(3)
_cell_volume                     1144.9(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    3638
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      23.78

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.931
_exptl_crystal_F_000             640
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.270
_exptl_crystal_size_min          0.130
_exptl_absorpt_coefficient_mu    7.426
_shelx_estimated_absorpt_T_min   0.175
_shelx_estimated_absorpt_T_max   0.445
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1752
_exptl_absorpt_correction_T_max  0.4452
_exptl_absorpt_process_details   'SADABS-2008/1, Bruker'

_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      193(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 SMART1000 CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6161
_diffrn_reflns_av_unetI/netI     0.0448
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.739
_diffrn_reflns_theta_max         24.985
_diffrn_reflns_theta_full        24.985
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.988
_reflns_number_total             3980
_reflns_number_gt                3596
_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       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND, K. Brandenburg, (1999)'
_computing_publication_material  'Wingx 2013.3 (Farrugia, 1999)'

_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)+(0.0389P)²+2.6661P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3980
_refine_ls_number_parameters     314
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0301
_refine_ls_wR_factor_ref         0.0785
_refine_ls_wR_factor_gt          0.0752
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_restrained_S_all      1.077
_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 0.63810(2) -0.24295(2) 0.10321(2) 0.01739(9) Uani 1 1 d . . . . .
O1 O 0.6761(5) -0.4258(4) -0.0157(4) 0.0251(10) Uani 1 1 d . . . . .
O11 O 0.7845(5) -0.4199(4) 0.2236(4) 0.0267(10) Uani 1 1 d . . . . .
O12 O 0.6168(5) -0.2707(4) 0.3275(4) 0.0261(10) Uani 1 1 d . . . . .
O13 O 0.7594(6) -0.4356(5) 0.4070(4) 0.0432(13) Uani 1 1 d . . . . .
O21 O 0.4540(6) -0.0266(4) 0.2057(4) 0.0363(12) Uani 1 1 d . . . . .
O22 O 0.3171(6) 0.1451(5) 0.1322(4) 0.0400(13) Uani 1 1 d . . . . .
O23 O 0.5680(6) 0.0667(6) 0.0583(4) 0.0457(14) Uani 1 1 d . . . . .
N1 N 0.6222(6) -0.6585(5) -0.2159(4) 0.0218(11) Uani 1 1 d . . . . .
N2 N 0.9143(6) -0.4117(5) -0.1229(4) 0.0176(11) Uani 1 1 d . . . . .
H20 H 0.991(7) -0.439(5) -0.177(5) 0.010(15) Uiso 1 1 d . . . . .
N3 N 0.9162(6) -0.3369(4) -0.0437(4) 0.0158(10) Uani 1 1 d . . . . .
N4 N 0.8833(6) -0.1840(5) 0.1123(4) 0.0228(11) Uani 1 1 d . . . . .
N11 N 0.7204(6) -0.3765(5) 0.3223(5) 0.0257(12) Uani 1 1 d . . . . .
N21 N 0.4473(6) 0.0631(5) 0.1317(5) 0.0262(12) Uani 1 1 d . . . . .
C1 C 0.6547(7) -0.5896(5) -0.1496(5) 0.0195(13) Uani 1 1 d . . . . .
H1 H 0.5924 -0.5798 -0.0734 0.023 Uiso 1 1 calc R U . . .
C2 C 0.7745(6) -0.5318(5) -0.1860(5) 0.0147(12) Uani 1 1 d . . . . .
C3 C 0.8639(7) -0.5444(6) -0.2975(5) 0.0231(14) Uani 1 1 d . . . . .
H3 H 0.9452 -0.5050 -0.3259 0.028 Uiso 1 1 calc R U . . .
C4 C 0.8324(8) -0.6156(7) -0.3665(5) 0.0295(15) Uani 1 1 d . . . . .
H4 H 0.8927 -0.6274 -0.4430 0.035 Uiso 1 1 calc R U . . .
C5 C 0.7106(8) -0.6694(6) -0.3217(6) 0.0281(15) Uani 1 1 d . . . . .
H5 H 0.6890 -0.7173 -0.3702 0.034 Uiso 1 1 calc R U . . .
C6 C 0.7850(7) -0.4534(5) -0.1010(5) 0.0167(12) Uani 1 1 d . . . . .
C7 C 1.0247(7) -0.2810(5) -0.0660(5) 0.0169(12) Uani 1 1 d . . . . .
C8 C 1.0156(7) -0.2028(5) 0.0258(5) 0.0176(12) Uani 1 1 d . . . . .
C9 C 1.1348(7) -0.1522(6) 0.0234(5) 0.0222(13) Uani 1 1 d . . . . .
H9 H 1.2240 -0.1620 -0.0401 0.027 Uiso 1 1 calc R U . . .
C10 C 1.1231(8) -0.0861(6) 0.1156(6) 0.0267(14) Uani 1 1 d . . . . .
H10 H 1.2055 -0.0522 0.1164 0.032 Uiso 1 1 calc R U . . .
C11 C 0.9915(8) -0.0708(6) 0.2048(5) 0.0273(15) Uani 1 1 d . . . . .
H11 H 0.9825 -0.0285 0.2695 0.033 Uiso 1 1 calc R U . . .
C12 C 0.8727(8) -0.1180(6) 0.1986(5) 0.0256(14) Uani 1 1 d . . . . .
H12 H 0.7787 -0.1031 0.2584 0.031 Uiso 1 1 calc R U . . .
C13 C 1.1441(7) -0.2835(5) -0.1771(5) 0.0170(12) Uani 1 1 d . . . . .
C14 C 1.3082(7) -0.3356(6) -0.1869(5) 0.0239(14) Uani 1 1 d . . . . .
H14 H 1.3478 -0.3733 -0.1215 0.029 Uiso 1 1 calc R U . . .
C15 C 1.4121(8) -0.3319(6) -0.2915(6) 0.0291(15) Uani 1 1 d . . . . .
H15 H 1.5235 -0.3673 -0.2981 0.035 Uiso 1 1 calc R U . . .
C16 C 1.3556(8) -0.2767(6) -0.3882(6) 0.0312(16) Uani 1 1 d . . . . .
H16 H 1.4276 -0.2746 -0.4605 0.037 Uiso 1 1 calc R U . . .
C17 C 1.1931(8) -0.2250(7) -0.3770(6) 0.0302(16) Uani 1 1 d . . . . .
H17 H 1.1540 -0.1857 -0.4422 0.036 Uiso 1 1 calc R U . . .
C18 C 1.0873(7) -0.2293(6) -0.2738(5) 0.0219(13) Uani 1 1 d . . . . .
H18 H 0.9759 -0.1954 -0.2683 0.026 Uiso 1 1 calc R U . . .
O31 O 0.1850(7) 0.0007(6) 0.3935(5) 0.0505(14) Uani 1 1 d D . . A 1
H31 H 0.2676 -0.0248 0.3418 0.076 Uiso 1 1 calc R U . A 1
C31 C 0.2106(14) 0.0859(13) 0.4633(9) 0.108(5) Uani 1 1 d D U . A 1
H31A H 0.2137 0.1644 0.4185 0.162 Uiso 1 1 calc R U . A 1
H31B H 0.3120 0.0468 0.4858 0.162 Uiso 1 1 calc R U . A 1
H31C H 0.1232 0.1029 0.5318 0.162 Uiso 1 1 calc R U . A 1


_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 O11 2.536(4) . ?
Pb N4 2.562(5) . ?
Pb O1 2.574(4) . ?
Pb O12 2.665(4) . ?
Pb N3 2.674(5) . ?
Pb O21 2.736(4) . ?
Pb O22 2.894(5) 2_655 ?
O1 C6 1.227(7) . ?
O11 N11 1.279(7) . ?
O12 N11 1.261(7) . ?
O13 N11 1.218(7) . ?
O21 N21 1.256(7) . ?
O22 N21 1.248(7) . ?
O23 N21 1.228(7) . ?
N1 C5 1.324(8) . ?
N1 C1 1.342(8) . ?
N2 C6 1.357(8) . ?
N2 N3 1.377(7) . ?
N2 H20 0.83(6) . ?
N3 C7 1.291(8) . ?
N4 C12 1.340(8) . ?
N4 C8 1.353(8) . ?
C1 C2 1.393(8) . ?
C1 H1 0.9500 . ?
C2 C3 1.385(8) . ?
C2 C6 1.495(8) . ?
C3 C4 1.381(9) . ?
C3 H3 0.9500 . ?
C4 C5 1.387(10) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C7 C13 1.491(8) . ?
C7 C8 1.492(8) . ?
C8 C9 1.375(9) . ?
C9 C10 1.397(9) . ?
C9 H9 0.9500 . ?
C10 C11 1.369(9) . ?
C10 H10 0.9500 . ?
C11 C12 1.376(9) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C18 1.395(8) . ?
C13 C14 1.399(8) . ?
C14 C15 1.375(9) . ?
C14 H14 0.9500 . ?
C15 C16 1.394(9) . ?
C15 H15 0.9500 . ?
C16 C17 1.383(10) . ?
C16 H16 0.9500 . ?
C17 C18 1.371(9) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
O31 C31 1.480(11) . ?
O31 H31 0.8400 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O11 Pb N4 75.18(16) . . ?
O11 Pb O1 81.32(14) . . ?
N4 Pb O1 119.06(14) . . ?
O11 Pb O12 49.23(13) . . ?
N4 Pb O12 79.43(15) . . ?
O1 Pb O12 122.45(14) . . ?
O11 Pb N3 77.71(14) . . ?
N4 Pb N3 60.59(15) . . ?
O1 Pb N3 59.79(14) . . ?
O12 Pb N3 120.62(13) . . ?
O11 Pb O21 117.90(14) . . ?
N4 Pb O21 87.76(16) . . ?
O1 Pb O21 151.33(15) . . ?
O12 Pb O21 69.22(13) . . ?
N3 Pb O21 141.05(16) . . ?
O11 Pb O22 138.25(13) . 2_655 ?
N4 Pb O22 87.79(16) . 2_655 ?
O1 Pb O22 74.16(15) . 2_655 ?
O12 Pb O22 162.59(15) . 2_655 ?
N3 Pb O22 60.83(13) . 2_655 ?
O21 Pb O22 98.75(14) . 2_655 ?
C6 O1 Pb 122.3(4) . . ?
N11 O11 Pb 99.6(3) . . ?
N11 O12 Pb 93.9(3) . . ?
N21 O21 Pb 109.0(3) . . ?
C5 N1 C1 116.4(6) . . ?
C6 N2 N3 116.1(5) . . ?
C6 N2 H20 120(4) . . ?
N3 N2 H20 124(4) . . ?
C7 N3 N2 119.3(5) . . ?
C7 N3 Pb 120.0(4) . . ?
N2 N3 Pb 116.0(3) . . ?
C12 N4 C8 118.4(5) . . ?
C12 N4 Pb 118.7(4) . . ?
C8 N4 Pb 122.3(4) . . ?
O13 N11 O12 122.0(5) . . ?
O13 N11 O11 120.7(5) . . ?
O12 N11 O11 117.3(5) . . ?
O23 N21 O22 121.2(6) . . ?
O23 N21 O21 119.3(6) . . ?
O22 N21 O21 119.4(6) . . ?
N1 C1 C2 123.8(6) . . ?
N1 C1 H1 118.1 . . ?
C2 C1 H1 118.1 . . ?
C3 C2 C1 118.2(5) . . ?
C3 C2 C6 126.3(5) . . ?
C1 C2 C6 115.3(5) . . ?
C4 C3 C2 118.6(6) . . ?
C4 C3 H3 120.7 . . ?
C2 C3 H3 120.7 . . ?
C3 C4 C5 118.5(6) . . ?
C3 C4 H4 120.8 . . ?
C5 C4 H4 120.8 . . ?
N1 C5 C4 124.5(6) . . ?
N1 C5 H5 117.8 . . ?
C4 C5 H5 117.8 . . ?
O1 C6 N2 121.9(5) . . ?
O1 C6 C2 119.8(5) . . ?
N2 C6 C2 118.3(5) . . ?
N3 C7 C13 124.4(5) . . ?
N3 C7 C8 114.8(5) . . ?
C13 C7 C8 120.7(5) . . ?
N4 C8 C9 121.5(5) . . ?
N4 C8 C7 116.4(5) . . ?
C9 C8 C7 122.1(5) . . ?
C8 C9 C10 119.1(6) . . ?
C8 C9 H9 120.5 . . ?
C10 C9 H9 120.5 . . ?
C11 C10 C9 119.3(6) . . ?
C11 C10 H10 120.3 . . ?
C9 C10 H10 120.3 . . ?
C10 C11 C12 118.5(6) . . ?
C10 C11 H11 120.8 . . ?
C12 C11 H11 120.8 . . ?
N4 C12 C11 123.1(6) . . ?
N4 C12 H12 118.4 . . ?
C11 C12 H12 118.4 . . ?
C18 C13 C14 119.6(6) . . ?
C18 C13 C7 117.6(5) . . ?
C14 C13 C7 122.8(5) . . ?
C15 C14 C13 119.7(6) . . ?
C15 C14 H14 120.1 . . ?
C13 C14 H14 120.1 . . ?
C14 C15 C16 120.7(6) . . ?
C14 C15 H15 119.6 . . ?
C16 C15 H15 119.6 . . ?
C17 C16 C15 118.9(6) . . ?
C17 C16 H16 120.6 . . ?
C15 C16 H16 120.6 . . ?
C18 C17 C16 121.3(6) . . ?
C18 C17 H17 119.3 . . ?
C16 C17 H17 119.3 . . ?
C17 C18 C13 119.7(6) . . ?
C17 C18 H18 120.2 . . ?
C13 C18 H18 120.2 . . ?
C31 O31 H31 109.5 . . ?
O31 C31 H31A 109.5 . . ?
O31 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
O31 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 N2 N3 C7 -171.1(5) . . . . ?
C6 N2 N3 Pb -15.4(6) . . . . ?
Pb O12 N11 O13 180.0(6) . . . . ?
Pb O12 N11 O11 0.4(5) . . . . ?
Pb O11 N11 O13 180.0(5) . . . . ?
Pb O11 N11 O12 -0.4(6) . . . . ?
Pb O21 N21 O23 -40.8(7) . . . . ?
Pb O21 N21 O22 137.1(5) . . . . ?
C5 N1 C1 C2 -0.5(8) . . . . ?
N1 C1 C2 C3 1.0(9) . . . . ?
N1 C1 C2 C6 176.7(5) . . . . ?
C1 C2 C3 C4 -1.3(8) . . . . ?
C6 C2 C3 C4 -176.4(6) . . . . ?
C2 C3 C4 C5 1.1(9) . . . . ?
C1 N1 C5 C4 0.4(9) . . . . ?
C3 C4 C5 N1 -0.7(10) . . . . ?
Pb O1 C6 N2 16.7(8) . . . . ?
Pb O1 C6 C2 -161.3(4) . . . . ?
N3 N2 C6 O1 0.2(8) . . . . ?
N3 N2 C6 C2 178.2(5) . . . . ?
C3 C2 C6 O1 162.4(6) . . . . ?
C1 C2 C6 O1 -12.9(8) . . . . ?
C3 C2 C6 N2 -15.6(8) . . . . ?
C1 C2 C6 N2 169.1(5) . . . . ?
N2 N3 C7 C13 4.7(8) . . . . ?
Pb N3 C7 C13 -150.1(4) . . . . ?
N2 N3 C7 C8 -179.8(5) . . . . ?
Pb N3 C7 C8 25.4(6) . . . . ?
C12 N4 C8 C9 -2.4(9) . . . . ?
Pb N4 C8 C9 168.9(4) . . . . ?
C12 N4 C8 C7 177.7(5) . . . . ?
Pb N4 C8 C7 -11.0(7) . . . . ?
N3 C7 C8 N4 -10.0(7) . . . . ?
C13 C7 C8 N4 165.7(5) . . . . ?
N3 C7 C8 C9 170.1(5) . . . . ?
C13 C7 C8 C9 -14.2(8) . . . . ?
N4 C8 C9 C10 3.9(9) . . . . ?
C7 C8 C9 C10 -176.2(5) . . . . ?
C8 C9 C10 C11 -1.6(9) . . . . ?
C9 C10 C11 C12 -2.0(10) . . . . ?
C8 N4 C12 C11 -1.4(9) . . . . ?
Pb N4 C12 C11 -173.1(5) . . . . ?
C10 C11 C12 N4 3.6(10) . . . . ?
N3 C7 C13 C18 63.8(8) . . . . ?
C8 C7 C13 C18 -111.4(6) . . . . ?
N3 C7 C13 C14 -117.4(7) . . . . ?
C8 C7 C13 C14 67.4(8) . . . . ?
C18 C13 C14 C15 0.5(9) . . . . ?
C7 C13 C14 C15 -178.3(6) . . . . ?
C13 C14 C15 C16 0.0(10) . . . . ?
C14 C15 C16 C17 0.3(11) . . . . ?
C15 C16 C17 C18 -1.3(11) . . . . ?
C16 C17 C18 C13 1.9(10) . . . . ?
C14 C13 C18 C17 -1.5(9) . . . . ?
C7 C13 C18 C17 177.4(6) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H20 O11 0.83(6) 2.14(6) 2.860(7) 144(5) 2_745
O31 H31 O21 0.84 2.03 2.840(8) 161.6 .

_refine_diff_density_max         2.766
_refine_diff_density_min         -1.209
_refine_diff_density_rms         0.155

####################################################################### 
# 
# 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 1992561'
loop_
_audit_author_name
_audit_author_address
'Damir Safin' 'University of Tyumen'
_audit_update_record             
;
2020-03-25 deposited with the CCDC.	2020-07-17 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         'C13 H11 I N4 O Pb'
_chemical_formula_sum            'C13 H11 I N4 O Pb'
_chemical_formula_weight         573.35

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_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                   6.8225(2)
_cell_length_b                   18.6186(5)
_cell_length_c                   11.9818(3)
_cell_angle_alpha                90
_cell_angle_beta                 104.108(3)
_cell_angle_gamma                90
_cell_volume                     1476.09(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    4200
_cell_measurement_theta_min      2.7979
_cell_measurement_theta_max      30.3838


_exptl_crystal_description       plate
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.580
_exptl_crystal_F_000             1040
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    13.522

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
1 2 -3 0.0996 1.0000 2.0000 -3.0000 -0.1004 0.0452 -0.1709
-2 -4 8 0.0735 -2.0000 -4.0000 8.0000 0.2631 -0.1821 0.3933
0 -1 0 0.1251 0.0000 -1.0000 0.0000 -0.0225 0.0020 0.0308
0 1 0 0.1157 -0.0000 1.0000 -0.0000 0.0225 -0.0020 -0.0308
-8 10 -4 0.0498 -8.0000 10.0000 -4.0000 0.5153 0.8681 -0.1537
8 -10 4 0.0116 8.0000 -10.0000 4.0000 -0.5153 -0.8681 0.1537
4 23 -7 0.1005 4.0000 23.0000 -7.0000 0.0912 -0.0782 -1.0160
_exptl_absorpt_correction_T_min  0.062
_exptl_absorpt_correction_T_max  0.459
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;

_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  
;
Oxford Diffraction Xcalibur E
;
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            8732
_diffrn_reflns_av_unetI/netI     0.0500
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.507
_diffrn_reflns_theta_max         27.994
_diffrn_reflns_theta_full        27.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3549
_reflns_number_gt                3073
_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       CrysalisPro
_computing_cell_refinement       CrysalisPro
_computing_data_reduction        CrysalisPro
_computing_structure_solution    SIR92
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND, K. Brandenburg, (1999)'
_computing_publication_material  SHELXL-2014

_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)+(0.0106P)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     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3549
_refine_ls_number_parameters     182
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0297
_refine_ls_wR_factor_ref         0.0526
_refine_ls_wR_factor_gt          0.0496
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_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
Pb1 Pb 1.09850(3) 0.03628(2) 0.82960(2) 0.01798(6) Uani 1 1 d . . . . .
I1 I 0.68955(5) 0.04909(2) 0.88047(3) 0.02395(9) Uani 1 1 d . . . . .
O1 O 1.0455(5) 0.14086(18) 0.7151(3) 0.0213(8) Uani 1 1 d . . . . .
N1 N 0.8827(6) 0.0198(2) 0.6278(3) 0.0169(9) Uani 1 1 d . . . . .
N2 N 0.8091(6) 0.0820(2) 0.5694(3) 0.0192(9) Uani 1 1 d . . . . .
N3 N 1.0061(6) -0.0992(2) 0.7524(3) 0.0193(9) Uani 1 1 d . . . . .
N4 N 0.6886(6) 0.3430(2) 0.4739(3) 0.0241(10) Uani 1 1 d . . . . .
C1 C 0.6927(8) -0.0461(3) 0.4574(4) 0.0212(11) Uani 1 1 d . . . . .
H1A H 0.5595 -0.0640 0.4614 0.032 Uiso 1 1 calc R U . . .
H1B H 0.7530 -0.0794 0.4117 0.032 Uiso 1 1 calc R U . . .
H1C H 0.6781 0.0014 0.4210 0.032 Uiso 1 1 calc R U . . .
C2 C 0.8258(7) -0.0407(3) 0.5757(4) 0.0171(10) Uani 1 1 d . . . . .
C3 C 0.8987(7) -0.1074(3) 0.6417(4) 0.0177(11) Uani 1 1 d . . . . .
C4 C 0.8586(8) -0.1745(3) 0.5928(4) 0.0226(11) Uani 1 1 d . . . . .
H4 H 0.7817 -0.1791 0.5156 0.027 Uiso 1 1 calc R U . . .
C5 C 0.9316(8) -0.2357(3) 0.6573(4) 0.0245(12) Uani 1 1 d . . . . .
H5 H 0.9066 -0.2822 0.6245 0.029 Uiso 1 1 calc R U . . .
C6 C 1.0393(8) -0.2269(3) 0.7682(4) 0.0250(12) Uani 1 1 d . . . . .
H6 H 1.0900 -0.2674 0.8145 0.030 Uiso 1 1 calc R U . . .
C7 C 1.0734(8) -0.1586(3) 0.8121(4) 0.0244(12) Uani 1 1 d . . . . .
H7 H 1.1493 -0.1533 0.8894 0.029 Uiso 1 1 calc R U . . .
C8 C 0.8988(8) 0.1390(3) 0.6238(4) 0.0192(11) Uani 1 1 d . . . . .
C9 C 0.8218(7) 0.2095(3) 0.5709(4) 0.0170(10) Uani 1 1 d . . . . .
C10 C 0.6564(7) 0.2144(3) 0.4768(4) 0.0219(11) Uani 1 1 d . . . . .
H10 H 0.5870 0.1725 0.4431 0.026 Uiso 1 1 calc R U . . .
C11 C 0.5956(8) 0.2818(3) 0.4334(4) 0.0238(12) Uani 1 1 d . . . . .
H11 H 0.4800 0.2848 0.3706 0.029 Uiso 1 1 calc R U . . .
C12 C 0.8451(8) 0.3376(3) 0.5645(4) 0.0224(11) Uani 1 1 d . . . . .
H12 H 0.9129 0.3804 0.5954 0.027 Uiso 1 1 calc R U . . .
C13 C 0.9149(7) 0.2732(3) 0.6164(4) 0.0198(11) Uani 1 1 d . . . . .
H13 H 1.0252 0.2724 0.6825 0.024 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 O1 2.359(3) . ?
Pb1 N1 2.525(4) . ?
Pb1 N3 2.708(4) . ?
Pb1 I1 3.0070(4) . ?
O1 C8 1.290(6) . ?
N1 C2 1.300(6) . ?
N1 N2 1.383(5) . ?
N2 C8 1.315(6) . ?
N3 C7 1.335(6) . ?
N3 C3 1.359(6) . ?
N4 C12 1.329(6) . ?
N4 C11 1.336(6) . ?
C1 C2 1.490(7) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.492(7) . ?
C3 C4 1.378(7) . ?
C4 C5 1.398(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.362(7) . ?
C5 H5 0.9500 . ?
C6 C7 1.375(7) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C9 1.496(7) . ?
C9 C10 1.390(7) . ?
C9 C13 1.392(7) . ?
C10 C11 1.383(7) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 C13 1.380(7) . ?
C12 H12 0.9500 . ?
C13 H13 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
O1 Pb1 N1 64.66(12) . . ?
O1 Pb1 N3 125.48(11) . . ?
N1 Pb1 N3 61.76(13) . . ?
O1 Pb1 I1 91.96(8) . . ?
N1 Pb1 I1 81.40(8) . . ?
N3 Pb1 I1 89.60(8) . . ?
C8 O1 Pb1 116.7(3) . . ?
C2 N1 N2 117.0(4) . . ?
C2 N1 Pb1 127.0(3) . . ?
N2 N1 Pb1 115.9(3) . . ?
C8 N2 N1 111.0(4) . . ?
C7 N3 C3 117.6(4) . . ?
C7 N3 Pb1 124.6(3) . . ?
C3 N3 Pb1 117.6(3) . . ?
C12 N4 C11 116.6(5) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C1 123.9(4) . . ?
N1 C2 C3 116.4(4) . . ?
C1 C2 C3 119.6(4) . . ?
N3 C3 C4 121.4(5) . . ?
N3 C3 C2 117.1(4) . . ?
C4 C3 C2 121.6(4) . . ?
C3 C4 C5 119.8(5) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
C6 C5 C4 118.4(5) . . ?
C6 C5 H5 120.8 . . ?
C4 C5 H5 120.8 . . ?
C5 C6 C7 119.0(5) . . ?
C5 C6 H6 120.5 . . ?
C7 C6 H6 120.5 . . ?
N3 C7 C6 123.9(5) . . ?
N3 C7 H7 118.1 . . ?
C6 C7 H7 118.1 . . ?
O1 C8 N2 127.7(5) . . ?
O1 C8 C9 117.1(4) . . ?
N2 C8 C9 115.2(4) . . ?
C10 C9 C13 117.7(5) . . ?
C10 C9 C8 122.2(5) . . ?
C13 C9 C8 120.1(4) . . ?
C11 C10 C9 118.2(5) . . ?
C11 C10 H10 120.9 . . ?
C9 C10 H10 120.9 . . ?
N4 C11 C10 124.4(5) . . ?
N4 C11 H11 117.8 . . ?
C10 C11 H11 117.8 . . ?
N4 C12 C13 123.7(5) . . ?
N4 C12 H12 118.2 . . ?
C13 C12 H12 118.2 . . ?
C12 C13 C9 119.2(5) . . ?
C12 C13 H13 120.4 . . ?
C9 C13 H13 120.4 . . ?

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
C2 N1 N2 C8 -171.3(4) . . . . ?
Pb1 N1 N2 C8 12.1(4) . . . . ?
N2 N1 C2 C1 1.8(6) . . . . ?
Pb1 N1 C2 C1 178.0(3) . . . . ?
N2 N1 C2 C3 -177.3(3) . . . . ?
Pb1 N1 C2 C3 -1.0(6) . . . . ?
C7 N3 C3 C4 0.6(7) . . . . ?
Pb1 N3 C3 C4 175.0(3) . . . . ?
C7 N3 C3 C2 -179.5(4) . . . . ?
Pb1 N3 C3 C2 -5.2(5) . . . . ?
N1 C2 C3 N3 4.2(6) . . . . ?
C1 C2 C3 N3 -174.9(4) . . . . ?
N1 C2 C3 C4 -175.9(4) . . . . ?
C1 C2 C3 C4 5.0(7) . . . . ?
N3 C3 C4 C5 -0.8(7) . . . . ?
C2 C3 C4 C5 179.3(4) . . . . ?
C3 C4 C5 C6 0.8(7) . . . . ?
C4 C5 C6 C7 -0.5(7) . . . . ?
C3 N3 C7 C6 -0.3(7) . . . . ?
Pb1 N3 C7 C6 -174.3(4) . . . . ?
C5 C6 C7 N3 0.3(8) . . . . ?
Pb1 O1 C8 N2 -19.7(6) . . . . ?
Pb1 O1 C8 C9 161.5(3) . . . . ?
N1 N2 C8 O1 4.4(6) . . . . ?
N1 N2 C8 C9 -176.8(3) . . . . ?
O1 C8 C9 C10 -175.9(4) . . . . ?
N2 C8 C9 C10 5.1(6) . . . . ?
O1 C8 C9 C13 3.5(6) . . . . ?
N2 C8 C9 C13 -175.5(4) . . . . ?
C13 C9 C10 C11 0.6(6) . . . . ?
C8 C9 C10 C11 -180.0(4) . . . . ?
C12 N4 C11 C10 -2.6(7) . . . . ?
C9 C10 C11 N4 1.9(7) . . . . ?
C11 N4 C12 C13 0.6(7) . . . . ?
N4 C12 C13 C9 1.8(7) . . . . ?
C10 C9 C13 C12 -2.3(6) . . . . ?
C8 C9 C13 C12 178.2(4) . . . . ?

_refine_diff_density_max         1.428
_refine_diff_density_min         -1.048
_refine_diff_density_rms         0.189

####################################################################### 
# 
# 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 1992560'
loop_
_audit_author_name
_audit_author_address
'Damir Safin' 'University of Tyumen'
_audit_update_record             
;
2020-03-25 deposited with the CCDC.	2020-07-17 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         'C8 H5 N4 Pb S2'
_chemical_formula_sum            'C8 H5 N4 Pb S2'
_chemical_formula_weight         428.48

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'
S S 0.1246 0.1234 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   6.7965(5)
_cell_length_b                   7.1870(6)
_cell_length_c                   11.8200(9)
_cell_angle_alpha                75.4600(10)
_cell_angle_beta                 82.1480(10)
_cell_angle_gamma                77.4340(10)
_cell_volume                     543.43(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2274
_cell_measurement_theta_min      2.01
_cell_measurement_theta_max      26.55

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.619
_exptl_crystal_F_000             390
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.300
_exptl_absorpt_coefficient_mu    15.876
_shelx_estimated_absorpt_T_min   0.061
_shelx_estimated_absorpt_T_max   0.087
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0752
_exptl_absorpt_correction_T_max  0.1152
_exptl_absorpt_process_details   'SADABS-2008/1, Bruker'

_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 SMART1000 CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            5450
_diffrn_reflns_av_unetI/netI     0.0485
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.787
_diffrn_reflns_theta_max         28.359
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             2662
_reflns_number_gt                2442
_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       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0546P)²+0.1990P] 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_number_reflns         2662
_refine_ls_number_parameters     136
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0318
_refine_ls_wR_factor_ref         0.0928
_refine_ls_wR_factor_gt          0.0897
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_restrained_S_all      1.104
_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
Pb1 Pb 1.19809(3) -0.23309(3) 0.91938(2) 0.02329(10) Uani 1 1 d . . . . .
S1 S 1.9310(3) -0.4551(3) 0.82629(17) 0.0304(4) Uani 1 1 d . . . . .
S2 S 1.4561(3) 0.3502(2) 0.89052(16) 0.0294(4) Uani 1 1 d . . . . .
N1 N 1.5535(10) -0.2039(10) 0.8070(6) 0.0401(15) Uani 1 1 d . . . . .
N2 N 1.1893(10) 0.0900(9) 0.9831(7) 0.0375(15) Uani 1 1 d . . . . .
N3 N 1.1056(9) 0.0069(9) 0.7231(5) 0.0300(12) Uani 1 1 d . . . . .
N4 N 0.6017(11) 0.4542(11) 0.4954(6) 0.0436(17) Uani 1 1 d . . . . .
C1 C 1.7108(10) -0.3050(10) 0.8143(6) 0.0262(13) Uani 1 1 d . . . . .
C2 C 1.3033(10) 0.1974(9) 0.9440(6) 0.0265(14) Uani 1 1 d . . . . .
C3 C 1.2427(12) 0.0246(13) 0.6297(8) 0.0418(19) Uani 1 1 d . . . . .
H3 H 1.3732 -0.0475 0.6385 0.050 Uiso 1 1 calc R U . . .
C4 C 1.1999(14) 0.1438(14) 0.5219(8) 0.049(2) Uani 1 1 d . . . . .
H4 H 1.3007 0.1531 0.4602 0.059 Uiso 1 1 calc R U . . .
C5 C 1.0075(13) 0.2489(12) 0.5058(7) 0.0390(17) Uani 1 1 d . . . . .
H5 H 0.9743 0.3278 0.4330 0.047 Uiso 1 1 calc R U . . .
C6 C 0.8632(11) 0.2337(10) 0.6022(6) 0.0285(14) Uani 1 1 d . . . . .
C7 C 0.9172(11) 0.1103(9) 0.7084(6) 0.0283(14) Uani 1 1 d . . . . .
H7 H 0.8195 0.0988 0.7717 0.034 Uiso 1 1 calc R U . . .
C8 C 0.6531(12) 0.3405(12) 0.5908(7) 0.0365(17) Uani 1 1 d . . . . .
H8 H 0.5574 0.3236 0.6548 0.044 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 N3 2.582(6) . ?
Pb1 N2 2.602(6) . ?
Pb1 N1 2.617(7) . ?
Pb1 N2 2.812(6) 2_757 ?
Pb1 S1 3.1206(19) 1_455 ?
Pb1 S2 3.1980(17) 1_545 ?
Pb1 S2 3.3034(19) 2_857 ?
Pb1 S1 3.403(2) 2_847 ?
S1 C1 1.643(7) . ?
S1 Pb1 3.1206(18) 1_655 ?
S2 C2 1.629(7) . ?
N1 C1 1.155(10) . ?
N2 C2 1.180(9) . ?
N3 C7 1.343(9) . ?
N3 C3 1.343(11) . ?
N4 C8 1.258(10) . ?
N4 N4 1.399(14) 2_666 ?
C3 C4 1.374(12) . ?
C3 H3 0.9300 . ?
C4 C5 1.372(12) . ?
C4 H4 0.9300 . ?
C5 C6 1.397(10) . ?
C5 H5 0.9300 . ?
C6 C7 1.386(9) . ?
C6 C8 1.473(10) . ?
C7 H7 0.9300 . ?
C8 H8 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
N3 Pb1 N2 82.4(2) . . ?
N3 Pb1 N1 77.6(2) . . ?
N2 Pb1 N1 89.3(2) . . ?
N3 Pb1 N2 87.9(2) . 2_757 ?
N2 Pb1 N2 68.7(2) . 2_757 ?
N1 Pb1 N2 155.2(2) . 2_757 ?
N3 Pb1 S1 78.54(14) . 1_455 ?
N2 Pb1 S1 142.51(15) . 1_455 ?
N1 Pb1 S1 117.24(17) . 1_455 ?
N2 Pb1 S1 78.54(14) 2_757 1_455 ?
N3 Pb1 S2 113.85(14) . 1_545 ?
N2 Pb1 S2 146.95(15) . 1_545 ?
N1 Pb1 S2 68.13(16) . 1_545 ?
N2 Pb1 S2 136.65(13) 2_757 1_545 ?
S1 Pb1 S2 70.51(5) 1_455 1_545 ?
N3 Pb1 S2 140.88(14) . 2_857 ?
N2 Pb1 S2 75.36(16) . 2_857 ?
N1 Pb1 S2 70.45(16) . 2_857 ?
N2 Pb1 S2 112.52(16) 2_757 2_857 ?
S1 Pb1 S2 136.34(4) 1_455 2_857 ?
S2 Pb1 S2 74.44(5) 1_545 2_857 ?
N3 Pb1 S1 150.95(14) . 2_847 ?
N2 Pb1 S1 103.64(17) . 2_847 ?
N1 Pb1 S1 130.17(15) . 2_847 ?
N2 Pb1 S1 68.77(15) 2_757 2_847 ?
S1 Pb1 S1 79.96(5) 1_455 2_847 ?
S2 Pb1 S1 76.40(4) 1_545 2_847 ?
S2 Pb1 S1 67.02(4) 2_857 2_847 ?
C1 S1 Pb1 104.3(3) . 1_655 ?
C1 N1 Pb1 133.0(5) . . ?
C2 N2 Pb1 124.5(5) . . ?
C7 N3 C3 117.4(6) . . ?
C7 N3 Pb1 121.7(5) . . ?
C3 N3 Pb1 120.8(5) . . ?
C8 N4 N4 111.5(8) . 2_666 ?
N1 C1 S1 178.1(7) . . ?
N2 C2 S2 178.5(6) . . ?
N3 C3 C4 123.4(7) . . ?
N3 C3 H3 118.3 . . ?
C4 C3 H3 118.3 . . ?
C5 C4 C3 119.6(8) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C4 C5 C6 117.9(7) . . ?
C4 C5 H5 121.1 . . ?
C6 C5 H5 121.1 . . ?
C7 C6 C5 119.3(7) . . ?
C7 C6 C8 119.9(6) . . ?
C5 C6 C8 120.8(7) . . ?
N3 C7 C6 122.4(7) . . ?
N3 C7 H7 118.8 . . ?
C6 C7 H7 118.8 . . ?
N4 C8 C6 120.7(7) . . ?
N4 C8 H8 119.6 . . ?
C6 C8 H8 119.6 . . ?

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 N3 C3 C4 0.8(13) . . . . ?
Pb1 N3 C3 C4 177.3(7) . . . . ?
N3 C3 C4 C5 -1.3(15) . . . . ?
C3 C4 C5 C6 1.7(14) . . . . ?
C4 C5 C6 C7 -1.8(12) . . . . ?
C4 C5 C6 C8 -179.2(8) . . . . ?
C3 N3 C7 C6 -0.9(11) . . . . ?
Pb1 N3 C7 C6 -177.3(5) . . . . ?
C5 C6 C7 N3 1.4(11) . . . . ?
C8 C6 C7 N3 178.8(7) . . . . ?
N4 N4 C8 C6 -177.9(9) 2_666 . . . ?
C7 C6 C8 N4 179.4(8) . . . . ?
C5 C6 C8 N4 -3.2(12) . . . . ?

_refine_diff_density_max         1.652
_refine_diff_density_min         -2.625
_refine_diff_density_rms         0.261

