# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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 1474988'
_audit_update_record             
;
2016-04-19 deposited with the CCDC.
2016-05-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C13 H12 Cl2 N4 O Pb'
_chemical_formula_sum            'C13 H12 Cl2 N4 O Pb'
_chemical_formula_weight         518.36

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   10.4863(14)
_cell_length_b                   14.790(2)
_cell_length_c                   10.8544(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 116.161(2)
_cell_angle_gamma                90.00
_cell_volume                     1511.0(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9951
_cell_measurement_theta_min      2.50
_cell_measurement_theta_max      29.16

_exptl_crystal_description       Block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.279
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             968
_exptl_absorpt_coefficient_mu    11.522
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.2163
_exptl_absorpt_correction_T_max  0.3074
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008a)'

_exptl_special_details           
; 
 The diffraction data were obtained from 3 sets of 400 frames,
 each of width 0.5 deg. in omega, colllected at phi = 0.00,
 90.00 and 180.00 deg. and 2 sets of 800 frames, each of
 width 0.45 deg in phi, collected at omega = -30.00 and 210.00
 deg. The scan time was 10 sec/frame.
;

_diffrn_ambient_temperature      100(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 CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26047
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_sigmaI/netI    0.0264
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.16
_diffrn_reflns_theta_max         29.18
_reflns_number_total             3940
_reflns_number_gt                3567
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2 (Bruker-AXS, 2010)'
_computing_cell_refinement       'Bruker SAINT (Bruker-AXS 2009)'
_computing_data_reduction        'Bruker SAINT (Bruker-AXS 2009)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL(Bruker-AXS 2008)'
_computing_publication_material  'Bruker SHELXTL(Bruker-AXS 2008)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. H-atoms attached to carbon
 were placed in calculated positions (C---H = 0.95 - 0.98 Å) while that
 attached to nitrogen was placed in a location derived from a difference
 map. All were included as riding contributions with isotropic displacement
 parameters 1.2 - 1.5 times those of the attached atoms.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0177P)²+1.0606P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     heavy
_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         3940
_refine_ls_number_parameters     191
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0223
_refine_ls_R_factor_gt           0.0183
_refine_ls_wR_factor_ref         0.0418
_refine_ls_wR_factor_gt          0.0403
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.002
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.742187(9) 0.768755(6) 0.557266(9) 0.01168(4) Uani 1 1 d . . .
Cl1 Cl 1.04286(7) 0.75470(4) 0.61876(7) 0.01659(13) Uani 1 1 d . . .
Cl2 Cl 0.68986(7) 0.80948(5) 0.29652(7) 0.01981(13) Uani 1 1 d . . .
O1 O 0.5127(2) 0.85923(13) 0.5037(2) 0.0228(4) Uani 1 1 d . . .
N1 N 0.7206(2) 0.59763(15) 0.4813(2) 0.0136(4) Uani 1 1 d . . .
N2 N 0.4808(2) 0.69216(15) 0.4074(2) 0.0135(4) Uani 1 1 d . . .
N3 N 0.3648(2) 0.74840(15) 0.3728(2) 0.0141(4) Uani 1 1 d . . .
H3N H 0.2775 0.7368 0.3046 0.017 Uiso 1 1 d R . .
N4 N 0.1882(2) 1.04615(15) 0.3777(2) 0.0161(5) Uani 1 1 d . . .
C1 C 0.8388(3) 0.54732(19) 0.5295(3) 0.0169(5) Uani 1 1 d . . .
H1 H 0.9270 0.5762 0.5833 0.020 Uiso 1 1 calc R . .
C2 C 0.8394(3) 0.45519(19) 0.5049(3) 0.0192(6) Uani 1 1 d . . .
H2 H 0.9254 0.4217 0.5424 0.023 Uiso 1 1 calc R . .
C3 C 0.7115(3) 0.41371(19) 0.4247(3) 0.0171(5) Uani 1 1 d . . .
H3 H 0.7082 0.3509 0.4053 0.021 Uiso 1 1 calc R . .
C4 C 0.5873(3) 0.46495(18) 0.3726(3) 0.0166(5) Uani 1 1 d . . .
H4 H 0.4983 0.4376 0.3166 0.020 Uiso 1 1 calc R . .
C5 C 0.5953(3) 0.55641(18) 0.4035(3) 0.0133(5) Uani 1 1 d . . .
C6 C 0.4636(3) 0.61282(17) 0.3545(3) 0.0121(5) Uani 1 1 d . . .
C7 C 0.3268(3) 0.57224(19) 0.2532(3) 0.0178(5) Uani 1 1 d . . .
H7A H 0.2943 0.5273 0.2995 0.027 Uiso 1 1 calc R . .
H7B H 0.3413 0.5430 0.1795 0.027 Uiso 1 1 calc R . .
H7C H 0.2550 0.6199 0.2145 0.027 Uiso 1 1 calc R . .
C8 C 0.3916(3) 0.83230(18) 0.4295(3) 0.0144(5) Uani 1 1 d . . .
C9 C 0.2670(3) 0.89173(18) 0.4005(3) 0.0131(5) Uani 1 1 d . . .
C10 C 0.1382(3) 0.86133(18) 0.3927(3) 0.0140(5) Uani 1 1 d . . .
H10 H 0.1213 0.7986 0.3975 0.017 Uiso 1 1 calc R . .
C11 C 0.0354(3) 0.92465(18) 0.3777(3) 0.0162(5) Uani 1 1 d . . .
H11 H -0.0537 0.9062 0.3723 0.019 Uiso 1 1 calc R . .
C12 C 0.0643(3) 1.01542(19) 0.3706(3) 0.0172(5) Uani 1 1 d . . .
H12 H -0.0072 1.0583 0.3602 0.021 Uiso 1 1 calc R . .
C13 C 0.2870(3) 0.98433(18) 0.3923(3) 0.0154(5) Uani 1 1 d . . .
H13 H 0.3752 1.0045 0.3974 0.018 Uiso 1 1 calc R . .


_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 2.5857(19) . ?
Pb1 N1 2.641(2) . ?
Pb1 Cl2 2.7027(8) . ?
Pb1 N2 2.740(2) . ?
Pb1 Cl1 2.9282(8) . ?
O1 C8 1.232(3) . ?
N1 C1 1.338(3) . ?
N1 C5 1.354(3) . ?
N2 C6 1.284(3) . ?
N2 N3 1.383(3) . ?
N3 C8 1.358(3) . ?
N3 H3N 0.9042 . ?
N4 C13 1.338(3) . ?
N4 C12 1.346(3) . ?
C1 C2 1.389(4) . ?
C1 H1 0.9500 . ?
C2 C3 1.379(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.394(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.387(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.497(3) . ?
C6 C7 1.495(3) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.489(4) . ?
C9 C10 1.390(3) . ?
C9 C13 1.394(4) . ?
C10 C11 1.382(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.386(4) . ?
C11 H11 0.9500 . ?
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 118.87(6) . . ?
O1 Pb1 Cl2 84.83(5) . . ?
N1 Pb1 Cl2 86.36(5) . . ?
O1 Pb1 N2 59.49(6) . . ?
N1 Pb1 N2 59.53(7) . . ?
Cl2 Pb1 N2 77.44(5) . . ?
O1 Pb1 Cl1 152.85(5) . . ?
N1 Pb1 Cl1 86.47(5) . . ?
Cl2 Pb1 Cl1 87.45(2) . . ?
N2 Pb1 Cl1 143.18(5) . . ?
C8 O1 Pb1 124.66(18) . . ?
C1 N1 C5 118.1(2) . . ?
C1 N1 Pb1 118.28(17) . . ?
C5 N1 Pb1 123.52(17) . . ?
C6 N2 N3 119.6(2) . . ?
C6 N2 Pb1 123.40(17) . . ?
N3 N2 Pb1 116.29(15) . . ?
C8 N3 N2 116.4(2) . . ?
C8 N3 H3N 118.5 . . ?
N2 N3 H3N 124.1 . . ?
C13 N4 C12 117.0(2) . . ?
N1 C1 C2 123.5(3) . . ?
N1 C1 H1 118.3 . . ?
C2 C1 H1 118.3 . . ?
C3 C2 C1 118.2(3) . . ?
C3 C2 H2 120.9 . . ?
C1 C2 H2 120.9 . . ?
C2 C3 C4 119.3(3) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C5 C4 C3 119.1(3) . . ?
C5 C4 H4 120.5 . . ?
C3 C4 H4 120.5 . . ?
N1 C5 C4 121.9(2) . . ?
N1 C5 C6 117.4(2) . . ?
C4 C5 C6 120.6(2) . . ?
N2 C6 C7 126.6(2) . . ?
N2 C6 C5 115.1(2) . . ?
C7 C6 C5 118.3(2) . . ?
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 122.6(2) . . ?
O1 C8 C9 120.2(2) . . ?
N3 C8 C9 117.2(2) . . ?
C10 C9 C13 118.9(2) . . ?
C10 C9 C8 124.1(2) . . ?
C13 C9 C8 116.8(2) . . ?
C11 C10 C9 118.3(2) . . ?
C11 C10 H10 120.8 . . ?
C9 C10 H10 120.8 . . ?
C10 C11 C12 119.0(2) . . ?
C10 C11 H11 120.5 . . ?
C12 C11 H11 120.5 . . ?
N4 C12 C11 123.6(3) . . ?
N4 C12 H12 118.2 . . ?
C11 C12 H12 118.2 . . ?
N4 C13 C9 123.2(2) . . ?
N4 C13 H13 118.4 . . ?
C9 C13 H13 118.4 . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.420
_refine_diff_density_min         -0.802
_refine_diff_density_rms         0.111

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
N3 H3N Cl1 0.90 2.40 3.285(2) 166 4_475
####################################################################### 
# 
# 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_jtm318_0m
_database_code_depnum_ccdc_archive 'CCDC 1474989'
_audit_update_record             
;
2016-05-16 deposited with the CCDC.
2016-05-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
Tetranitratobis(2-acetylpyridylnicotinylhydrozone)dilead(II))
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C13 H12 N6 O7 Pb'
_chemical_formula_sum            'C13 H12 N6 O7 Pb'
_chemical_formula_weight         571.48

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'
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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.0862(4)
_cell_length_b                   9.3122(4)
_cell_length_c                   11.5175(5)
_cell_angle_alpha                84.905(1)
_cell_angle_beta                 72.809(1)
_cell_angle_gamma                62.775(1)
_cell_volume                     826.61(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9984
_cell_measurement_theta_min      2.46
_cell_measurement_theta_max      29.14

_exptl_crystal_description       Parallelepiped
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.227
_exptl_crystal_size_mid          0.168
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.296
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             540
_exptl_absorpt_coefficient_mu    10.259
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.0924
_exptl_absorpt_correction_T_max  0.3290
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008a)'

_exptl_special_details           
; 
 The diffraction data were obtained from 3 sets of 400 frames,
 each of width 0.5 deg. in omega, colllected at phi = 0.00,
 90.00 and 180.00 deg. and 2 sets of 800 frames, each of
 width 0.45 deg in phi, collected at omega = -30.00 and 210.00
 deg. The scan time was 10 sec/frame.
;

_diffrn_ambient_temperature      100(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 CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14331
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_sigmaI/netI    0.0270
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.46
_diffrn_reflns_theta_max         28.10
_reflns_number_total             3973
_reflns_number_gt                3878
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2 (Bruker-AXS, 2009)'
_computing_cell_refinement       'Bruker SAINT (Bruker-AXS 2009a)'
_computing_data_reduction        'Bruker SAINT (Bruker-AXS 2009a)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL(Bruker-AXS 2008)'
_computing_publication_material  'Bruker SHELXTL(Bruker-AXS 2008)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. H-atoms attached to carbon
 were placed in calculated positions (C---H = 0.95 - 0.98 Å) while those
 attached to nitrogen were placed in locations derived from a difference
 map.All were included as riding contributions with isotropic displacement
 parameters 1.2 - 1.5 times those of the attached atoms.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0279P)²+0.4758P] 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         3973
_refine_ls_number_parameters     245
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0198
_refine_ls_R_factor_gt           0.0192
_refine_ls_wR_factor_ref         0.0487
_refine_ls_wR_factor_gt          0.0484
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_restrained_S_all      1.079
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.905011(11) 0.367710(10) 0.215748(8) 0.01206(4) Uani 1 1 d . . .
O1 O 0.7987(3) 0.2197(3) 0.38761(19) 0.0195(4) Uani 1 1 d . . .
O2 O 1.0009(3) 0.0428(3) 0.2442(2) 0.0229(5) Uani 1 1 d . . .
O3 O 0.8871(3) -0.0369(3) 0.4157(3) 0.0345(6) Uani 1 1 d . . .
O4 O 0.8518(3) 0.8106(3) 0.0059(2) 0.0235(5) Uani 1 1 d . . .
O5 O 1.0395(3) 0.5975(3) 0.0676(2) 0.0238(5) Uani 1 1 d . . .
O6 O 0.7644(3) 0.6787(3) 0.15292(19) 0.0191(4) Uani 1 1 d . . .
O7 O 0.8306(3) 0.5405(3) 0.39989(19) 0.0205(4) Uani 1 1 d . . .
N1 N 0.6775(3) 0.3377(3) 0.1503(2) 0.0157(5) Uani 1 1 d . . .
N2 N 0.5768(3) 0.5493(3) 0.3306(2) 0.0129(4) Uani 1 1 d . . .
N3 N 0.5425(3) 0.6536(3) 0.4245(2) 0.0138(4) Uani 1 1 d . . .
H3N H 0.4397 0.6998 0.4720 0.017 Uiso 1 1 d R . .
N4 N 0.7986(4) 0.7860(3) 0.6866(2) 0.0201(5) Uani 1 1 d . . .
N5 N 0.8983(3) 0.0708(3) 0.3495(3) 0.0205(5) Uani 1 1 d . . .
N6 N 0.8851(3) 0.6963(3) 0.0758(2) 0.0156(5) Uani 1 1 d . . .
C1 C 0.7316(4) 0.2248(3) 0.0630(3) 0.0183(6) Uani 1 1 d . . .
H1 H 0.8489 0.1538 0.0361 0.022 Uiso 1 1 calc R . .
C2 C 0.6201(4) 0.2090(4) 0.0109(3) 0.0216(6) Uani 1 1 d . . .
H2 H 0.6611 0.1277 -0.0486 0.026 Uiso 1 1 calc R . .
C3 C 0.4461(4) 0.3171(4) 0.0495(3) 0.0213(6) Uani 1 1 d . . .
H3 H 0.3686 0.3109 0.0150 0.026 Uiso 1 1 calc R . .
C4 C 0.3888(4) 0.4351(4) 0.1404(3) 0.0180(6) Uani 1 1 d . . .
H4 H 0.2723 0.5082 0.1679 0.022 Uiso 1 1 calc R . .
C5 C 0.5076(4) 0.4426(3) 0.1898(2) 0.0145(5) Uani 1 1 d . . .
C6 C 0.4542(4) 0.5639(3) 0.2888(2) 0.0143(5) Uani 1 1 d . . .
C7 C 0.2696(4) 0.6911(4) 0.3306(3) 0.0208(6) Uani 1 1 d . . .
H7A H 0.2001 0.6442 0.3817 0.031 Uiso 1 1 calc R . .
H7B H 0.2283 0.7332 0.2612 0.031 Uiso 1 1 calc R . .
H7C H 0.2624 0.7771 0.3757 0.031 Uiso 1 1 calc R . .
C8 C 0.6821(4) 0.6391(3) 0.4541(2) 0.0147(5) Uani 1 1 d . . .
C9 C 0.6559(4) 0.7447(3) 0.5557(2) 0.0143(5) Uani 1 1 d . . .
C10 C 0.7990(4) 0.7039(3) 0.5968(3) 0.0170(5) Uani 1 1 d . . .
H10 H 0.9012 0.6139 0.5595 0.020 Uiso 1 1 calc R . .
C11 C 0.6495(4) 0.9158(4) 0.7371(3) 0.0226(6) Uani 1 1 d . . .
H11 H 0.6459 0.9747 0.7999 0.027 Uiso 1 1 calc R . .
C12 C 0.5010(4) 0.9680(4) 0.7023(3) 0.0216(6) Uani 1 1 d . . .
H12 H 0.4012 1.0595 0.7405 0.026 Uiso 1 1 calc R . .
C13 C 0.5034(4) 0.8812(3) 0.6093(3) 0.0164(5) Uani 1 1 d . . .
H13 H 0.4057 0.9134 0.5834 0.020 Uiso 1 1 calc R . .


_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 O7 2.512(2) . ?
Pb1 O1 2.521(2) . ?
Pb1 N1 2.531(2) . ?
Pb1 N2 2.637(2) . ?
Pb1 O6 2.707(2) . ?
Pb1 O2 2.757(2) . ?
O1 N5 1.288(3) . ?
O2 N5 1.254(4) . ?
O3 N5 1.229(4) . ?
O4 N6 1.253(3) . ?
O5 N6 1.256(3) . ?
O6 N6 1.258(3) . ?
O7 C8 1.234(3) . ?
N1 C1 1.335(4) . ?
N1 C5 1.352(4) . ?
N2 C6 1.288(4) . ?
N2 N3 1.385(3) . ?
N3 C8 1.355(4) . ?
N3 H3N 0.8537 . ?
N4 C10 1.338(4) . ?
N4 C11 1.340(4) . ?
C1 C2 1.386(4) . ?
C1 H1 0.9300 . ?
C2 C3 1.385(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.391(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.390(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.487(4) . ?
C6 C7 1.501(4) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 C9 1.490(4) . ?
C9 C10 1.392(4) . ?
C9 C13 1.393(4) . ?
C10 H10 0.9300 . ?
C11 C12 1.380(5) . ?
C11 H11 0.9300 . ?
C12 C13 1.387(4) . ?
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
O7 Pb1 O1 77.50(7) . . ?
O7 Pb1 N1 122.24(7) . . ?
O1 Pb1 N1 77.64(7) . . ?
O7 Pb1 N2 61.12(7) . . ?
O1 Pb1 N2 69.62(7) . . ?
N1 Pb1 N2 61.48(7) . . ?
O7 Pb1 O6 73.44(7) . . ?
O1 Pb1 O6 132.45(6) . . ?
N1 Pb1 O6 87.03(7) . . ?
N2 Pb1 O6 63.55(7) . . ?
O7 Pb1 O2 117.78(7) . . ?
O1 Pb1 O2 48.45(7) . . ?
N1 Pb1 O2 78.88(8) . . ?
N2 Pb1 O2 112.08(7) . . ?
O6 Pb1 O2 165.29(8) . . ?
N5 O1 Pb1 101.99(17) . . ?
N5 O2 Pb1 91.54(17) . . ?
N6 O6 Pb1 105.94(16) . . ?
C8 O7 Pb1 123.89(19) . . ?
C1 N1 C5 119.4(3) . . ?
C1 N1 Pb1 117.63(19) . . ?
C5 N1 Pb1 122.51(19) . . ?
C6 N2 N3 120.1(2) . . ?
C6 N2 Pb1 121.99(18) . . ?
N3 N2 Pb1 116.65(16) . . ?
C8 N3 N2 115.7(2) . . ?
C8 N3 H3N 123.0 . . ?
N2 N3 H3N 118.5 . . ?
C10 N4 C11 116.1(3) . . ?
O3 N5 O2 122.9(3) . . ?
O3 N5 O1 119.3(3) . . ?
O2 N5 O1 117.8(3) . . ?
O4 N6 O5 119.9(2) . . ?
O4 N6 O6 120.2(2) . . ?
O5 N6 O6 119.9(3) . . ?
N1 C1 C2 122.6(3) . . ?
N1 C1 H1 118.7 . . ?
C2 C1 H1 118.7 . . ?
C3 C2 C1 118.5(3) . . ?
C3 C2 H2 120.8 . . ?
C1 C2 H2 120.8 . . ?
C2 C3 C4 119.2(3) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C5 C4 C3 119.2(3) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
N1 C5 C4 121.1(3) . . ?
N1 C5 C6 117.1(2) . . ?
C4 C5 C6 121.9(3) . . ?
N2 C6 C5 114.8(2) . . ?
N2 C6 C7 125.6(3) . . ?
C5 C6 C7 119.6(3) . . ?
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 . . ?
O7 C8 N3 122.1(3) . . ?
O7 C8 C9 118.9(3) . . ?
N3 C8 C9 119.1(2) . . ?
C10 C9 C13 118.3(3) . . ?
C10 C9 C8 116.2(2) . . ?
C13 C9 C8 125.5(3) . . ?
N4 C10 C9 124.1(3) . . ?
N4 C10 H10 118.0 . . ?
C9 C10 H10 118.0 . . ?
N4 C11 C12 124.5(3) . . ?
N4 C11 H11 117.7 . . ?
C12 C11 H11 117.7 . . ?
C11 C12 C13 118.6(3) . . ?
C11 C12 H12 120.7 . . ?
C13 C12 H12 120.7 . . ?
C12 C13 C9 118.3(3) . . ?
C12 C13 H13 120.8 . . ?
C9 C13 H13 120.8 . . ?

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
O7 Pb1 O1 N5 -143.79(19) . . . . ?
N1 Pb1 O1 N5 88.77(18) . . . . ?
N2 Pb1 O1 N5 152.66(19) . . . . ?
O6 Pb1 O1 N5 162.97(16) . . . . ?
O2 Pb1 O1 N5 2.77(16) . . . . ?
O7 Pb1 O2 N5 34.7(2) . . . . ?
O1 Pb1 O2 N5 -2.78(16) . . . . ?
N1 Pb1 O2 N5 -86.05(18) . . . . ?
N2 Pb1 O2 N5 -33.3(2) . . . . ?
O6 Pb1 O2 N5 -102.9(3) . . . . ?
O7 Pb1 O6 N6 111.80(18) . . . . ?
O1 Pb1 O6 N6 166.48(16) . . . . ?
N1 Pb1 O6 N6 -123.26(18) . . . . ?
N2 Pb1 O6 N6 177.3(2) . . . . ?
O2 Pb1 O6 N6 -106.7(3) . . . . ?
O1 Pb1 O7 C8 -79.4(2) . . . . ?
N1 Pb1 O7 C8 -13.0(3) . . . . ?
N2 Pb1 O7 C8 -6.0(2) . . . . ?
O6 Pb1 O7 C8 62.5(2) . . . . ?
O2 Pb1 O7 C8 -107.2(2) . . . . ?
O7 Pb1 N1 C1 -170.0(2) . . . . ?
O1 Pb1 N1 C1 -103.5(2) . . . . ?
N2 Pb1 N1 C1 -176.9(2) . . . . ?
O6 Pb1 N1 C1 121.8(2) . . . . ?
O2 Pb1 N1 C1 -54.0(2) . . . . ?
O7 Pb1 N1 C5 17.9(2) . . . . ?
O1 Pb1 N1 C5 84.3(2) . . . . ?
N2 Pb1 N1 C5 11.0(2) . . . . ?
O6 Pb1 N1 C5 -50.4(2) . . . . ?
O2 Pb1 N1 C5 133.9(2) . . . . ?
O7 Pb1 N2 C6 173.2(2) . . . . ?
O1 Pb1 N2 C6 -100.1(2) . . . . ?
N1 Pb1 N2 C6 -13.5(2) . . . . ?
O6 Pb1 N2 C6 88.3(2) . . . . ?
O2 Pb1 N2 C6 -76.2(2) . . . . ?
O7 Pb1 N2 N3 5.87(16) . . . . ?
O1 Pb1 N2 N3 92.50(18) . . . . ?
N1 Pb1 N2 N3 179.2(2) . . . . ?
O6 Pb1 N2 N3 -79.01(18) . . . . ?
O2 Pb1 N2 N3 116.40(17) . . . . ?
C6 N2 N3 C8 -173.7(2) . . . . ?
Pb1 N2 N3 C8 -6.1(3) . . . . ?
Pb1 O2 N5 O3 -176.9(3) . . . . ?
Pb1 O2 N5 O1 4.6(3) . . . . ?
Pb1 O1 N5 O3 176.3(3) . . . . ?
Pb1 O1 N5 O2 -5.2(3) . . . . ?
Pb1 O6 N6 O4 160.2(2) . . . . ?
Pb1 O6 N6 O5 -18.6(3) . . . . ?
C5 N1 C1 C2 -0.5(4) . . . . ?
Pb1 N1 C1 C2 -172.9(2) . . . . ?
N1 C1 C2 C3 1.3(5) . . . . ?
C1 C2 C3 C4 -1.3(4) . . . . ?
C2 C3 C4 C5 0.5(4) . . . . ?
C1 N1 C5 C4 -0.3(4) . . . . ?
Pb1 N1 C5 C4 171.7(2) . . . . ?
C1 N1 C5 C6 178.9(3) . . . . ?
Pb1 N1 C5 C6 -9.1(3) . . . . ?
C3 C4 C5 N1 0.3(4) . . . . ?
C3 C4 C5 C6 -178.9(3) . . . . ?
N3 N2 C6 C5 -178.9(2) . . . . ?
Pb1 N2 C6 C5 14.2(3) . . . . ?
N3 N2 C6 C7 1.8(4) . . . . ?
Pb1 N2 C6 C7 -165.1(2) . . . . ?
N1 C5 C6 N2 -3.6(4) . . . . ?
C4 C5 C6 N2 175.7(3) . . . . ?
N1 C5 C6 C7 175.8(3) . . . . ?
C4 C5 C6 C7 -5.0(4) . . . . ?
Pb1 O7 C8 N3 5.5(4) . . . . ?
Pb1 O7 C8 C9 -174.76(18) . . . . ?
N2 N3 C8 O7 0.9(4) . . . . ?
N2 N3 C8 C9 -178.9(2) . . . . ?
O7 C8 C9 C10 -11.5(4) . . . . ?
N3 C8 C9 C10 168.2(3) . . . . ?
O7 C8 C9 C13 166.7(3) . . . . ?
N3 C8 C9 C13 -13.6(4) . . . . ?
C11 N4 C10 C9 -0.7(5) . . . . ?
C13 C9 C10 N4 1.3(4) . . . . ?
C8 C9 C10 N4 179.6(3) . . . . ?
C10 N4 C11 C12 -0.2(5) . . . . ?
N4 C11 C12 C13 0.3(5) . . . . ?
C11 C12 C13 C9 0.3(4) . . . . ?
C10 C9 C13 C12 -1.1(4) . . . . ?
C8 C9 C13 C12 -179.2(3) . . . . ?

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
N3 H3N O1 0.85 2.13 2.971(3) 169 2_666

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        28.10
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         2.220
_refine_diff_density_min         -1.173
_refine_diff_density_rms         0.131
####################################################################### 
# 
# 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 1474990'
_audit_update_record             
;
2016-04-19 deposited with the CCDC.
2016-05-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H24 N12 O2 Pb2 S4'
_chemical_formula_weight         1127.23

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'
S S 0.1246 0.1234 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.5527(2)
_cell_length_b                   14.5337(5)
_cell_length_c                   16.8369(4)
_cell_angle_alpha                102.817(2)
_cell_angle_beta                 94.897(2)
_cell_angle_gamma                98.141(2)
_cell_volume                     1770.85(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    13480
_cell_measurement_theta_min      3.13
_cell_measurement_theta_max      30.24

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.114
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1064
_exptl_absorpt_coefficient_mu    9.779
_exptl_absorpt_correction_T_min  0.042
_exptl_absorpt_correction_T_max  0.322
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
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_special_details           
;
 ?
;

_diffrn_ambient_temperature      123(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  'Oxford Diffraction Xcalibur E'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            25546
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_sigmaI/netI    0.0426
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.29
_diffrn_reflns_theta_max         28.00
_reflns_number_total             8516
_reflns_number_gt                7285
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0105P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8516
_refine_ls_number_parameters     461
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0248
_refine_ls_wR_factor_ref         0.0454
_refine_ls_wR_factor_gt          0.0425
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.005
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.255707(18) 0.354298(10) 1.559743(8) 0.01383(4) Uani 1 1 d . . .
Pb2 Pb 0.195122(18) 0.159371(9) 1.983085(8) 0.01420(4) Uani 1 1 d . . .
S1 S 0.47300(13) 0.19518(7) 1.52659(6) 0.0251(2) Uani 1 1 d . . .
S2 S -0.34619(14) 0.42276(8) 1.46227(7) 0.0289(2) Uani 1 1 d . . .
S3 S 0.04855(13) 0.32668(7) 2.04345(6) 0.0206(2) Uani 1 1 d . . .
S4 S -0.34727(15) 0.01568(8) 2.12938(7) 0.0326(3) Uani 1 1 d . . .
O1 O 0.1187(3) 0.28069(18) 1.66748(14) 0.0213(6) Uani 1 1 d . . .
O2 O 0.3637(3) 0.24620(18) 1.89143(14) 0.0181(6) Uani 1 1 d . . .
N1 N 0.0046(4) 0.2077(2) 1.51022(17) 0.0148(6) Uani 1 1 d . . .
N2 N -0.0579(4) 0.1637(2) 1.56884(17) 0.0147(7) Uani 1 1 d . . .
N3 N 0.1352(4) 0.3072(2) 1.40765(17) 0.0139(6) Uani 1 1 d . . .
N4 N -0.0506(4) 0.1470(2) 1.84824(18) 0.0190(7) Uani 1 1 d . . .
N5 N 0.4959(4) 0.2891(2) 2.04708(17) 0.0145(6) Uani 1 1 d . . .
N6 N 0.5661(4) 0.3409(2) 1.99502(18) 0.0142(7) Uani 1 1 d . . .
N7 N 0.3312(4) 0.1817(2) 2.13684(18) 0.0167(7) Uani 1 1 d . . .
C25 C 0.7167(5) 0.4119(3) 1.7250(2) 0.0241(9) Uani 1 1 d . . .
H25 H 0.7653 0.4302 1.6796 0.029 Uiso 1 1 calc R . .
N9 N 0.2452(4) 0.0252(2) 1.4428(2) 0.0276(8) Uani 1 1 d . . .
N10 N -0.0374(4) 0.4163(2) 1.5634(2) 0.0247(8) Uani 1 1 d . . .
N11 N 0.2326(4) 0.4650(2) 1.9728(2) 0.0249(8) Uani 1 1 d . . .
N12 N -0.1138(4) 0.1062(3) 2.0389(2) 0.0309(9) Uani 1 1 d . . .
C1 C -0.1809(5) 0.0781(3) 1.4022(2) 0.0233(9) Uani 1 1 d . . .
H1A H -0.1394 0.0293 1.4276 0.035 Uiso 1 1 calc R . .
H1B H -0.1838 0.0578 1.3425 0.035 Uiso 1 1 calc R . .
H1C H -0.3020 0.0865 1.4158 0.035 Uiso 1 1 calc R . .
C2 C -0.0548(5) 0.1706(3) 1.4335(2) 0.0163(8) Uani 1 1 d . . .
C3 C 0.0096(5) 0.2293(3) 1.3763(2) 0.0147(8) Uani 1 1 d . . .
C4 C -0.0632(5) 0.2061(3) 1.2944(2) 0.0171(8) Uani 1 1 d . . .
H4 H -0.1514 0.1505 1.2731 0.021 Uiso 1 1 calc R . .
C5 C -0.0060(5) 0.2648(3) 1.2442(2) 0.0196(9) Uani 1 1 d . . .
H5 H -0.0542 0.2500 1.1880 0.024 Uiso 1 1 calc R . .
C6 C 0.1210(5) 0.3445(3) 1.2762(2) 0.0183(8) Uani 1 1 d . . .
H6 H 0.1616 0.3860 1.2428 0.022 Uiso 1 1 calc R . .
C7 C 0.1898(5) 0.3637(3) 1.3588(2) 0.0171(8) Uani 1 1 d . . .
H7 H 0.2785 0.4188 1.3811 0.021 Uiso 1 1 calc R . .
C8 C -0.0001(5) 0.2097(3) 1.6477(2) 0.0154(8) Uani 1 1 d . . .
C9 C -0.0903(5) 0.1715(3) 1.7118(2) 0.0160(8) Uani 1 1 d . . .
C10 C 0.0165(5) 0.1704(3) 1.7827(2) 0.0192(8) Uani 1 1 d . . .
H10 H 0.1435 0.1869 1.7850 0.023 Uiso 1 1 calc R . .
C11 C -0.2284(5) 0.1267(3) 1.8449(2) 0.0184(8) Uani 1 1 d . . .
H11 H -0.2781 0.1130 1.8918 0.022 Uiso 1 1 calc R . .
C12 C -0.3447(5) 0.1245(3) 1.7761(2) 0.0193(8) Uani 1 1 d . . .
H12 H -0.4711 0.1080 1.7758 0.023 Uiso 1 1 calc R . .
C13 C -0.2760(5) 0.1466(3) 1.7081(2) 0.0176(8) Uani 1 1 d . . .
H13 H -0.3534 0.1447 1.6600 0.021 Uiso 1 1 calc R . .
C14 C 0.6683(5) 0.4089(3) 2.1655(2) 0.0225(9) Uani 1 1 d . . .
H14A H 0.7927 0.3966 2.1686 0.034 Uiso 1 1 calc R . .
H14B H 0.6380 0.4328 2.2210 0.034 Uiso 1 1 calc R . .
H14C H 0.6561 0.4567 2.1334 0.034 Uiso 1 1 calc R . .
C15 C 0.5438(4) 0.3184(3) 2.1252(2) 0.0141(8) Uani 1 1 d . . .
C16 C 0.4658(5) 0.2538(3) 2.1751(2) 0.0151(8) Uani 1 1 d . . .
C17 C 0.5297(5) 0.2659(3) 2.2573(2) 0.0176(8) Uani 1 1 d . . .
H17 H 0.6216 0.3180 2.2837 0.021 Uiso 1 1 calc R . .
C18 C 0.4587(5) 0.2018(3) 2.3003(2) 0.0205(9) Uani 1 1 d . . .
H18 H 0.5010 0.2094 2.3565 0.025 Uiso 1 1 calc R . .
C19 C 0.3265(5) 0.1271(3) 2.2610(2) 0.0221(9) Uani 1 1 d . . .
H19 H 0.2772 0.0814 2.2891 0.027 Uiso 1 1 calc R . .
C20 C 0.2658(5) 0.1195(3) 2.1789(2) 0.0194(8) Uani 1 1 d . . .
H20 H 0.1739 0.0678 2.1518 0.023 Uiso 1 1 calc R . .
C21 C 0.4947(5) 0.3103(3) 1.9152(2) 0.0137(7) Uani 1 1 d . . .
C22 C 0.5838(5) 0.3553(2) 1.8542(2) 0.0138(8) Uani 1 1 d . . .
C23 C 0.7681(5) 0.3814(3) 1.8580(2) 0.0176(8) Uani 1 1 d . . .
H23 H 0.8464 0.3798 1.9047 0.021 Uiso 1 1 calc R . .
C24 C 0.8353(5) 0.4099(3) 1.7918(2) 0.0225(9) Uani 1 1 d . . .
H24 H 0.9614 0.4279 1.7921 0.027 Uiso 1 1 calc R . .
N8 N 0.5380(4) 0.3897(2) 1.72081(18) 0.0223(7) Uani 1 1 d . . .
C26 C 0.4739(5) 0.3610(3) 1.7850(2) 0.0187(8) Uani 1 1 d . . .
H26 H 0.3472 0.3437 1.7832 0.022 Uiso 1 1 calc R . .
C27 C 0.3370(5) 0.0948(3) 1.4776(2) 0.0181(8) Uani 1 1 d . . .
C28 C -0.1627(5) 0.4185(3) 1.5199(2) 0.0196(8) Uani 1 1 d . . .
C29 C 0.1597(5) 0.4078(3) 2.0024(2) 0.0162(8) Uani 1 1 d . . .
C30 C -0.2114(5) 0.0694(3) 2.0765(2) 0.0194(8) Uani 1 1 d . . .
H2N H 0.632(5) 0.392(3) 2.010(2) 0.014(11) Uiso 1 1 d . . .
H1N H -0.121(5) 0.109(3) 1.555(2) 0.022(11) Uiso 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
Pb1 N10 2.506(3) . ?
Pb1 O1 2.525(3) . ?
Pb1 N3 2.550(3) . ?
Pb1 N1 2.575(3) . ?
Pb1 S1 3.0019(10) . ?
Pb2 O2 2.518(3) . ?
Pb2 N7 2.635(3) . ?
Pb2 N12 2.667(3) . ?
Pb2 N5 2.710(3) . ?
Pb2 N4 2.763(3) . ?
Pb2 S3 2.8335(9) . ?
S1 C27 1.662(4) . ?
S2 C28 1.639(4) . ?
S3 C29 1.660(4) . ?
S4 C30 1.640(4) . ?
O1 C8 1.231(4) . ?
O2 C21 1.230(4) . ?
N1 C2 1.297(4) . ?
N1 N2 1.371(4) . ?
N2 C8 1.351(4) . ?
N2 H1N 0.85(4) . ?
N3 C7 1.335(5) . ?
N3 C3 1.344(4) . ?
N4 C11 1.328(4) . ?
N4 C10 1.343(4) . ?
N5 C15 1.291(4) . ?
N5 N6 1.369(4) . ?
N6 C21 1.356(4) . ?
N6 H2N 0.80(4) . ?
N7 C20 1.335(5) . ?
N7 C16 1.353(5) . ?
C25 N8 1.334(5) . ?
C25 C24 1.385(5) . ?
C25 H25 0.9500 . ?
N9 C27 1.147(5) . ?
N10 C28 1.155(4) . ?
N11 C29 1.158(5) . ?
N12 C30 1.161(5) . ?
C1 C2 1.493(5) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.490(5) . ?
C3 C4 1.389(5) . ?
C4 C5 1.381(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.368(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.395(5) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C9 1.490(5) . ?
C9 C10 1.387(5) . ?
C9 C13 1.390(5) . ?
C10 H10 0.9500 . ?
C11 C12 1.384(5) . ?
C11 H11 0.9500 . ?
C12 C13 1.379(5) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C15 1.489(5) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.488(5) . ?
C16 C17 1.391(5) . ?
C17 C18 1.381(5) . ?
C17 H17 0.9500 . ?
C18 C19 1.369(5) . ?
C18 H18 0.9500 . ?
C19 C20 1.393(5) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 C22 1.491(5) . ?
C22 C23 1.382(5) . ?
C22 C26 1.397(5) . ?
C23 C24 1.383(5) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
N8 C26 1.345(5) . ?
C26 H26 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
N10 Pb1 O1 78.73(10) . . ?
N10 Pb1 N3 79.33(9) . . ?
O1 Pb1 N3 124.29(9) . . ?
N10 Pb1 N1 73.34(10) . . ?
O1 Pb1 N1 62.42(8) . . ?
N3 Pb1 N1 62.36(10) . . ?
N10 Pb1 S1 152.23(8) . . ?
O1 Pb1 S1 88.73(6) . . ?
N3 Pb1 S1 87.78(6) . . ?
N1 Pb1 S1 78.90(7) . . ?
O2 Pb2 N7 119.61(9) . . ?
O2 Pb2 N12 149.38(9) . . ?
N7 Pb2 N12 83.35(10) . . ?
O2 Pb2 N5 60.22(8) . . ?
N7 Pb2 N5 59.72(9) . . ?
N12 Pb2 N5 134.33(10) . . ?
O2 Pb2 N4 74.55(8) . . ?
N7 Pb2 N4 160.33(9) . . ?
N12 Pb2 N4 78.91(10) . . ?
N5 Pb2 N4 130.31(9) . . ?
O2 Pb2 S3 88.86(6) . . ?
N7 Pb2 S3 84.88(7) . . ?
N12 Pb2 S3 72.29(8) . . ?
N5 Pb2 S3 78.14(6) . . ?
N4 Pb2 S3 81.70(6) . . ?
C27 S1 Pb1 108.89(13) . . ?
C29 S3 Pb2 103.54(12) . . ?
C8 O1 Pb1 120.7(2) . . ?
C21 O2 Pb2 124.8(2) . . ?
C2 N1 N2 119.4(3) . . ?
C2 N1 Pb1 123.5(3) . . ?
N2 N1 Pb1 116.8(2) . . ?
C8 N2 N1 116.4(3) . . ?
C8 N2 H1N 124(3) . . ?
N1 N2 H1N 120(3) . . ?
C7 N3 C3 119.0(3) . . ?
C7 N3 Pb1 119.6(2) . . ?
C3 N3 Pb1 121.3(2) . . ?
C11 N4 C10 117.6(3) . . ?
C11 N4 Pb2 125.7(2) . . ?
C10 N4 Pb2 116.5(2) . . ?
C15 N5 N6 119.8(3) . . ?
C15 N5 Pb2 122.3(2) . . ?
N6 N5 Pb2 115.6(2) . . ?
C21 N6 N5 115.8(3) . . ?
C21 N6 H2N 119(3) . . ?
N5 N6 H2N 124(3) . . ?
C20 N7 C16 118.4(3) . . ?
C20 N7 Pb2 119.0(3) . . ?
C16 N7 Pb2 122.6(2) . . ?
N8 C25 C24 123.9(4) . . ?
N8 C25 H25 118.1 . . ?
C24 C25 H25 118.1 . . ?
C28 N10 Pb1 140.1(3) . . ?
C30 N12 Pb2 158.3(3) . . ?
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 C3 114.6(3) . . ?
N1 C2 C1 124.7(4) . . ?
C3 C2 C1 120.7(3) . . ?
N3 C3 C4 121.5(3) . . ?
N3 C3 C2 117.5(3) . . ?
C4 C3 C2 121.0(3) . . ?
C5 C4 C3 119.2(4) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
C6 C5 C4 119.3(3) . . ?
C6 C5 H5 120.3 . . ?
C4 C5 H5 120.3 . . ?
C5 C6 C7 118.8(4) . . ?
C5 C6 H6 120.6 . . ?
C7 C6 H6 120.6 . . ?
N3 C7 C6 122.2(4) . . ?
N3 C7 H7 118.9 . . ?
C6 C7 H7 118.9 . . ?
O1 C8 N2 123.0(3) . . ?
O1 C8 C9 120.3(3) . . ?
N2 C8 C9 116.7(3) . . ?
C10 C9 C13 118.5(3) . . ?
C10 C9 C8 117.5(3) . . ?
C13 C9 C8 123.7(3) . . ?
N4 C10 C9 123.2(4) . . ?
N4 C10 H10 118.4 . . ?
C9 C10 H10 118.4 . . ?
N4 C11 C12 122.9(3) . . ?
N4 C11 H11 118.5 . . ?
C12 C11 H11 118.5 . . ?
C13 C12 C11 119.6(4) . . ?
C13 C12 H12 120.2 . . ?
C11 C12 H12 120.2 . . ?
C12 C13 C9 118.1(3) . . ?
C12 C13 H13 120.9 . . ?
C9 C13 H13 120.9 . . ?
C15 C14 H14A 109.5 . . ?
C15 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C15 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N5 C15 C16 114.9(3) . . ?
N5 C15 C14 124.7(3) . . ?
C16 C15 C14 120.4(3) . . ?
N7 C16 C17 121.2(3) . . ?
N7 C16 C15 117.2(3) . . ?
C17 C16 C15 121.5(3) . . ?
C18 C17 C16 119.6(4) . . ?
C18 C17 H17 120.2 . . ?
C16 C17 H17 120.2 . . ?
C19 C18 C17 119.2(4) . . ?
C19 C18 H18 120.4 . . ?
C17 C18 H18 120.4 . . ?
C18 C19 C20 118.6(4) . . ?
C18 C19 H19 120.7 . . ?
C20 C19 H19 120.7 . . ?
N7 C20 C19 122.9(4) . . ?
N7 C20 H20 118.5 . . ?
C19 C20 H20 118.5 . . ?
O2 C21 N6 122.7(3) . . ?
O2 C21 C22 119.5(3) . . ?
N6 C21 C22 117.8(3) . . ?
C23 C22 C26 118.8(3) . . ?
C23 C22 C21 123.9(3) . . ?
C26 C22 C21 116.9(3) . . ?
C22 C23 C24 118.2(4) . . ?
C22 C23 H23 120.9 . . ?
C24 C23 H23 120.9 . . ?
C23 C24 C25 119.2(4) . . ?
C23 C24 H24 120.4 . . ?
C25 C24 H24 120.4 . . ?
C25 N8 C26 116.6(3) . . ?
N8 C26 C22 123.4(4) . . ?
N8 C26 H26 118.3 . . ?
C22 C26 H26 118.3 . . ?
N9 C27 S1 178.9(4) . . ?
N10 C28 S2 177.0(3) . . ?
N11 C29 S3 178.0(4) . . ?
N12 C30 S4 178.9(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
N10 Pb1 S1 C27 9.8(2) . . . . ?
O1 Pb1 S1 C27 72.32(15) . . . . ?
N3 Pb1 S1 C27 -52.06(15) . . . . ?
N1 Pb1 S1 C27 10.20(15) . . . . ?
O2 Pb2 S3 C29 -7.70(14) . . . . ?
N7 Pb2 S3 C29 112.17(15) . . . . ?
N12 Pb2 S3 C29 -163.19(16) . . . . ?
N5 Pb2 S3 C29 52.07(15) . . . . ?
N4 Pb2 S3 C29 -82.25(15) . . . . ?
N10 Pb1 O1 C8 78.0(3) . . . . ?
N3 Pb1 O1 C8 9.4(3) . . . . ?
N1 Pb1 O1 C8 1.0(2) . . . . ?
S1 Pb1 O1 C8 -77.1(3) . . . . ?
N7 Pb2 O2 C21 -11.1(3) . . . . ?
N12 Pb2 O2 C21 123.2(3) . . . . ?
N5 Pb2 O2 C21 -4.7(3) . . . . ?
N4 Pb2 O2 C21 154.0(3) . . . . ?
S3 Pb2 O2 C21 72.3(3) . . . . ?
N10 Pb1 N1 C2 93.9(3) . . . . ?
O1 Pb1 N1 C2 179.6(3) . . . . ?
N3 Pb1 N1 C2 7.4(3) . . . . ?
S1 Pb1 N1 C2 -85.9(3) . . . . ?
N10 Pb1 N1 N2 -91.1(2) . . . . ?
O1 Pb1 N1 N2 -5.3(2) . . . . ?
N3 Pb1 N1 N2 -177.5(3) . . . . ?
S1 Pb1 N1 N2 89.1(2) . . . . ?
C2 N1 N2 C8 -175.5(3) . . . . ?
Pb1 N1 N2 C8 9.2(4) . . . . ?
N10 Pb1 N3 C7 96.6(3) . . . . ?
O1 Pb1 N3 C7 165.0(2) . . . . ?
N1 Pb1 N3 C7 173.3(3) . . . . ?
S1 Pb1 N3 C7 -108.1(2) . . . . ?
N10 Pb1 N3 C3 -79.5(3) . . . . ?
O1 Pb1 N3 C3 -11.2(3) . . . . ?
N1 Pb1 N3 C3 -2.9(2) . . . . ?
S1 Pb1 N3 C3 75.8(2) . . . . ?
O2 Pb2 N4 C11 -161.4(3) . . . . ?
N7 Pb2 N4 C11 -22.8(5) . . . . ?
N12 Pb2 N4 C11 3.2(3) . . . . ?
N5 Pb2 N4 C11 -136.9(3) . . . . ?
S3 Pb2 N4 C11 -70.3(3) . . . . ?
O2 Pb2 N4 C10 13.5(3) . . . . ?
N7 Pb2 N4 C10 152.1(3) . . . . ?
N12 Pb2 N4 C10 178.1(3) . . . . ?
N5 Pb2 N4 C10 38.0(3) . . . . ?
S3 Pb2 N4 C10 104.6(3) . . . . ?
O2 Pb2 N5 C15 170.3(3) . . . . ?
N7 Pb2 N5 C15 -16.3(2) . . . . ?
N12 Pb2 N5 C15 24.5(3) . . . . ?
N4 Pb2 N5 C15 142.9(3) . . . . ?
S3 Pb2 N5 C15 74.7(3) . . . . ?
O2 Pb2 N5 N6 7.5(2) . . . . ?
N7 Pb2 N5 N6 -179.1(3) . . . . ?
N12 Pb2 N5 N6 -138.3(2) . . . . ?
N4 Pb2 N5 N6 -19.9(3) . . . . ?
S3 Pb2 N5 N6 -88.1(2) . . . . ?
C15 N5 N6 C21 -173.5(3) . . . . ?
Pb2 N5 N6 C21 -10.2(4) . . . . ?
O2 Pb2 N7 C20 -164.1(2) . . . . ?
N12 Pb2 N7 C20 37.4(3) . . . . ?
N5 Pb2 N7 C20 -170.6(3) . . . . ?
N4 Pb2 N7 C20 63.1(4) . . . . ?
S3 Pb2 N7 C20 110.2(3) . . . . ?
O2 Pb2 N7 C16 15.6(3) . . . . ?
N12 Pb2 N7 C16 -142.8(3) . . . . ?
N5 Pb2 N7 C16 9.1(2) . . . . ?
N4 Pb2 N7 C16 -117.2(3) . . . . ?
S3 Pb2 N7 C16 -70.1(2) . . . . ?
O1 Pb1 N10 C28 -125.5(5) . . . . ?
N3 Pb1 N10 C28 3.0(5) . . . . ?
N1 Pb1 N10 C28 -61.2(5) . . . . ?
S1 Pb1 N10 C28 -60.8(6) . . . . ?
O2 Pb2 N12 C30 178.6(8) . . . . ?
N7 Pb2 N12 C30 -40.2(9) . . . . ?
N5 Pb2 N12 C30 -74.7(9) . . . . ?
N4 Pb2 N12 C30 148.4(9) . . . . ?
S3 Pb2 N12 C30 -126.9(9) . . . . ?
N2 N1 C2 C3 174.6(3) . . . . ?
Pb1 N1 C2 C3 -10.4(4) . . . . ?
N2 N1 C2 C1 -4.0(5) . . . . ?
Pb1 N1 C2 C1 170.9(3) . . . . ?
C7 N3 C3 C4 0.4(5) . . . . ?
Pb1 N3 C3 C4 176.6(2) . . . . ?
C7 N3 C3 C2 -177.0(3) . . . . ?
Pb1 N3 C3 C2 -0.8(4) . . . . ?
N1 C2 C3 N3 7.1(5) . . . . ?
C1 C2 C3 N3 -174.2(3) . . . . ?
N1 C2 C3 C4 -170.3(3) . . . . ?
C1 C2 C3 C4 8.5(5) . . . . ?
N3 C3 C4 C5 -0.3(5) . . . . ?
C2 C3 C4 C5 176.9(3) . . . . ?
C3 C4 C5 C6 -0.1(5) . . . . ?
C4 C5 C6 C7 0.4(5) . . . . ?
C3 N3 C7 C6 -0.1(5) . . . . ?
Pb1 N3 C7 C6 -176.3(2) . . . . ?
C5 C6 C7 N3 -0.4(5) . . . . ?
Pb1 O1 C8 N2 3.6(5) . . . . ?
Pb1 O1 C8 C9 -175.0(2) . . . . ?
N1 N2 C8 O1 -8.8(5) . . . . ?
N1 N2 C8 C9 169.9(3) . . . . ?
O1 C8 C9 C10 -40.3(5) . . . . ?
N2 C8 C9 C10 141.0(3) . . . . ?
O1 C8 C9 C13 133.0(4) . . . . ?
N2 C8 C9 C13 -45.8(5) . . . . ?
C11 N4 C10 C9 -1.9(6) . . . . ?
Pb2 N4 C10 C9 -177.2(3) . . . . ?
C13 C9 C10 N4 -0.5(6) . . . . ?
C8 C9 C10 N4 173.1(3) . . . . ?
C10 N4 C11 C12 3.0(5) . . . . ?
Pb2 N4 C11 C12 177.9(3) . . . . ?
N4 C11 C12 C13 -1.7(6) . . . . ?
C11 C12 C13 C9 -0.8(5) . . . . ?
C10 C9 C13 C12 1.9(5) . . . . ?
C8 C9 C13 C12 -171.3(3) . . . . ?
N6 N5 C15 C16 -177.0(3) . . . . ?
Pb2 N5 C15 C16 20.9(4) . . . . ?
N6 N5 C15 C14 2.5(5) . . . . ?
Pb2 N5 C15 C14 -159.6(3) . . . . ?
C20 N7 C16 C17 -2.9(5) . . . . ?
Pb2 N7 C16 C17 177.3(2) . . . . ?
C20 N7 C16 C15 176.3(3) . . . . ?
Pb2 N7 C16 C15 -3.4(4) . . . . ?
N5 C15 C16 N7 -11.4(5) . . . . ?
C14 C15 C16 N7 169.1(3) . . . . ?
N5 C15 C16 C17 167.8(3) . . . . ?
C14 C15 C16 C17 -11.7(5) . . . . ?
N7 C16 C17 C18 2.0(5) . . . . ?
C15 C16 C17 C18 -177.2(3) . . . . ?
C16 C17 C18 C19 0.1(5) . . . . ?
C17 C18 C19 C20 -1.2(5) . . . . ?
C16 N7 C20 C19 1.9(5) . . . . ?
Pb2 N7 C20 C19 -178.4(3) . . . . ?
C18 C19 C20 N7 0.2(5) . . . . ?
Pb2 O2 C21 N6 1.2(5) . . . . ?
Pb2 O2 C21 C22 179.4(2) . . . . ?
N5 N6 C21 O2 6.7(5) . . . . ?
N5 N6 C21 C22 -171.5(3) . . . . ?
O2 C21 C22 C23 -140.9(4) . . . . ?
N6 C21 C22 C23 37.4(5) . . . . ?
O2 C21 C22 C26 31.7(5) . . . . ?
N6 C21 C22 C26 -150.0(3) . . . . ?
C26 C22 C23 C24 -1.5(5) . . . . ?
C21 C22 C23 C24 171.0(3) . . . . ?
C22 C23 C24 C25 0.4(5) . . . . ?
N8 C25 C24 C23 1.5(6) . . . . ?
C24 C25 N8 C26 -2.2(6) . . . . ?
C25 N8 C26 C22 1.0(5) . . . . ?
C23 C22 C26 N8 0.8(5) . . . . ?
C21 C22 C26 N8 -172.2(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        28.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.691
_refine_diff_density_min         -0.716
_refine_diff_density_rms         0.139?
####################################################################### 
# 
# 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 1474991'
_audit_update_record             
;
2016-04-19 deposited with the CCDC.
2016-05-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C13 H12 Cl2 N4 O Pb'
_chemical_formula_sum            'C13 H12 Cl2 N4 O Pb'
_chemical_formula_weight         518.36

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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.8658(7)
_cell_length_b                   8.6864(7)
_cell_length_c                   11.0020(9)
_cell_angle_alpha                100.321(4)
_cell_angle_beta                 92.891(5)
_cell_angle_gamma                95.189(4)
_cell_volume                     734.82(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9922
_cell_measurement_theta_min      37.99
_cell_measurement_theta_max      2.61

_exptl_crystal_description       plates
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.343
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             484
_exptl_absorpt_coefficient_mu    11.846
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2283
_exptl_absorpt_correction_T_max  0.4868
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(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 APEX II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18736
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_sigmaI/netI    0.0250
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.40
_diffrn_reflns_theta_max         28.28
_reflns_number_total             3653
_reflns_number_gt                3524
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0250P)²+0.5894P] 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     SHELXL
_refine_ls_extinction_coef       0.0013(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3653
_refine_ls_number_parameters     192
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0182
_refine_ls_R_factor_gt           0.0172
_refine_ls_wR_factor_ref         0.0439
_refine_ls_wR_factor_gt          0.0434
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.002
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C17 C 0.0653(4) 0.8567(3) 0.3425(3) 0.0172(5) Uani 1 1 d . . .
H17 H 0.1804 0.8481 0.3222 0.021 Uiso 1 1 calc R . .
C16 C 0.0056(3) 0.7833(3) 0.4371(2) 0.0147(5) Uani 1 1 d . . .
C15 C -0.1637(4) 0.7989(3) 0.4662(3) 0.0174(5) Uani 1 1 d . . .
H15 H -0.2095 0.7524 0.5309 0.021 Uiso 1 1 calc R . .
C14 C -0.2641(4) 0.8825(3) 0.4001(3) 0.0195(5) Uani 1 1 d . . .
H14 H -0.3797 0.8932 0.4182 0.023 Uiso 1 1 calc R . .
C13 C -0.1932(4) 0.9507(3) 0.3067(3) 0.0179(5) Uani 1 1 d . . .
H13 H -0.2625 1.0076 0.2611 0.022 Uiso 1 1 calc R . .
N3 N -0.0310(3) 0.9389(3) 0.2787(2) 0.0183(5) Uani 1 1 d . . .
Pb1 Pb 0.123191(11) 0.154650(10) 1.158861(8) 0.01335(5) Uani 1 1 d . . .
Cl1 Cl 0.18937(9) -0.11471(8) 1.00360(7) 0.02072(14) Uani 1 1 d . . .
Cl3 Cl 0.44384(9) 0.19037(10) 1.28796(7) 0.02732(16) Uani 1 1 d . . .
O1 O -0.0287(2) 0.5389(2) 0.80024(18) 0.0178(4) Uani 1 1 d . . .
N1 N 0.2655(3) 0.2843(3) 0.9902(2) 0.0174(5) Uani 1 1 d . . .
N5 N 0.0736(3) 0.6780(3) 0.6137(2) 0.0158(4) Uani 1 1 d . . .
N6 N 0.1843(3) 0.6022(3) 0.6801(2) 0.0167(5) Uani 1 1 d . . .
H6 H 0.2893 0.6108 0.6685 0.020 Uiso 1 1 d R . .
C1 C 0.4283(4) 0.2691(3) 0.9630(3) 0.0179(5) Uani 1 1 d . . .
H1 H 0.4925 0.2044 1.0048 0.022 Uiso 1 1 calc R . .
C2 C 0.5065(4) 0.3444(3) 0.8760(3) 0.0187(5) Uani 1 1 d . . .
H2 H 0.6225 0.3326 0.8598 0.022 Uiso 1 1 calc R . .
C3 C 0.2420(3) 0.4515(3) 0.8397(2) 0.0133(5) Uani 1 1 d . . .
C4 C 0.1755(3) 0.3729(3) 0.9286(2) 0.0147(5) Uani 1 1 d . . .
H4 H 0.0597 0.3824 0.9468 0.018 Uiso 1 1 calc R . .
C5 C 0.4127(4) 0.4369(3) 0.8135(3) 0.0170(5) Uani 1 1 d . . .
H5 H 0.4635 0.4896 0.7538 0.020 Uiso 1 1 calc R . .
C6 C 0.1213(3) 0.5370(3) 0.7743(2) 0.0131(5) Uani 1 1 d . . .
C23 C 0.1197(3) 0.6977(3) 0.5060(2) 0.0149(5) Uani 1 1 d . . .
C24 C 0.2761(4) 0.6394(4) 0.4473(3) 0.0211(6) Uani 1 1 d . . .
H24A H 0.3728 0.7209 0.4691 0.032 Uiso 1 1 calc R . .
H24B H 0.2540 0.6148 0.3571 0.032 Uiso 1 1 calc R . .
H24C H 0.3035 0.5444 0.4776 0.032 Uiso 1 1 calc R . .


_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
C17 N3 1.341(4) . ?
C17 C16 1.394(4) . ?
C17 H17 0.9500 . ?
C16 C15 1.398(4) . ?
C16 C23 1.479(4) . ?
C15 C14 1.384(4) . ?
C15 H15 0.9500 . ?
C14 C13 1.391(4) . ?
C14 H14 0.9500 . ?
C13 N3 1.336(4) . ?
C13 H13 0.9500 . ?
N3 Pb1 2.712(2) 1_564 ?
Pb1 N1 2.588(2) . ?
Pb1 N3 2.712(2) 1_546 ?
Pb1 Cl1 2.7461(7) . ?
Pb1 Cl3 2.7954(8) . ?
Pb1 Cl1 2.9223(7) 2_557 ?
Cl1 Pb1 2.9223(7) 2_557 ?
O1 C6 1.229(3) . ?
N1 C4 1.337(3) . ?
N1 C1 1.342(4) . ?
N5 C23 1.292(4) . ?
N5 N6 1.391(3) . ?
N6 C6 1.361(3) . ?
N6 H6 0.8409 . ?
C1 C2 1.390(4) . ?
C1 H1 0.9500 . ?
C2 C5 1.384(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.387(4) . ?
C3 C5 1.400(4) . ?
C3 C6 1.489(4) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C23 C24 1.504(4) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 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
N3 C17 C16 123.6(3) . . ?
N3 C17 H17 118.2 . . ?
C16 C17 H17 118.2 . . ?
C17 C16 C15 117.2(2) . . ?
C17 C16 C23 120.9(2) . . ?
C15 C16 C23 121.9(2) . . ?
C14 C15 C16 119.5(3) . . ?
C14 C15 H15 120.2 . . ?
C16 C15 H15 120.2 . . ?
C15 C14 C13 119.0(3) . . ?
C15 C14 H14 120.5 . . ?
C13 C14 H14 120.5 . . ?
N3 C13 C14 122.3(3) . . ?
N3 C13 H13 118.9 . . ?
C14 C13 H13 118.9 . . ?
C13 N3 C17 118.4(3) . . ?
C13 N3 Pb1 118.65(18) . 1_564 ?
C17 N3 Pb1 119.53(19) . 1_564 ?
N1 Pb1 N3 162.10(8) . 1_546 ?
N1 Pb1 Cl1 81.80(5) . . ?
N3 Pb1 Cl1 80.93(5) 1_546 . ?
N1 Pb1 Cl3 88.25(6) . . ?
N3 Pb1 Cl3 97.45(6) 1_546 . ?
Cl1 Pb1 Cl3 93.36(2) . . ?
N1 Pb1 Cl1 85.63(6) . 2_557 ?
N3 Pb1 Cl1 87.43(6) 1_546 2_557 ?
Cl1 Pb1 Cl1 82.40(2) . 2_557 ?
Cl3 Pb1 Cl1 172.99(2) . 2_557 ?
Pb1 Cl1 Pb1 97.60(2) . 2_557 ?
C4 N1 C1 118.1(2) . . ?
C4 N1 Pb1 119.22(18) . . ?
C1 N1 Pb1 122.70(18) . . ?
C23 N5 N6 115.7(2) . . ?
C6 N6 N5 117.8(2) . . ?
C6 N6 H6 122.2 . . ?
N5 N6 H6 119.2 . . ?
N1 C1 C2 122.5(3) . . ?
N1 C1 H1 118.7 . . ?
C2 C1 H1 118.7 . . ?
C5 C2 C1 119.0(3) . . ?
C5 C2 H2 120.5 . . ?
C1 C2 H2 120.5 . . ?
C4 C3 C5 117.8(2) . . ?
C4 C3 C6 116.7(2) . . ?
C5 C3 C6 125.3(2) . . ?
N1 C4 C3 123.6(2) . . ?
N1 C4 H4 118.2 . . ?
C3 C4 H4 118.2 . . ?
C2 C5 C3 119.0(3) . . ?
C2 C5 H5 120.5 . . ?
C3 C5 H5 120.5 . . ?
O1 C6 N6 122.8(2) . . ?
O1 C6 C3 121.0(2) . . ?
N6 C6 C3 116.1(2) . . ?
N5 C23 C16 115.8(2) . . ?
N5 C23 C24 125.1(3) . . ?
C16 C23 C24 119.1(2) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 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
N3 C17 C16 C15 -0.6(4) . . . . ?
N3 C17 C16 C23 -178.5(2) . . . . ?
C17 C16 C15 C14 1.0(4) . . . . ?
C23 C16 C15 C14 178.9(2) . . . . ?
C16 C15 C14 C13 -0.6(4) . . . . ?
C15 C14 C13 N3 -0.3(4) . . . . ?
C14 C13 N3 C17 0.8(4) . . . . ?
C14 C13 N3 Pb1 -158.3(2) . . . 1_564 ?
C16 C17 N3 C13 -0.3(4) . . . . ?
C16 C17 N3 Pb1 158.6(2) . . . 1_564 ?
N1 Pb1 Cl1 Pb1 -86.65(6) . . . 2_557 ?
N3 Pb1 Cl1 Pb1 88.59(6) 1_546 . . 2_557 ?
Cl3 Pb1 Cl1 Pb1 -174.39(2) . . . 2_557 ?
Cl1 Pb1 Cl1 Pb1 0.0 2_557 . . 2_557 ?
N3 Pb1 N1 C4 103.7(3) 1_546 . . . ?
Cl1 Pb1 N1 C4 119.1(2) . . . . ?
Cl3 Pb1 N1 C4 -147.2(2) . . . . ?
Cl1 Pb1 N1 C4 36.20(19) 2_557 . . . ?
N3 Pb1 N1 C1 -77.6(3) 1_546 . . . ?
Cl1 Pb1 N1 C1 -62.2(2) . . . . ?
Cl3 Pb1 N1 C1 31.5(2) . . . . ?
Cl1 Pb1 N1 C1 -145.1(2) 2_557 . . . ?
C23 N5 N6 C6 -160.8(2) . . . . ?
C4 N1 C1 C2 1.5(4) . . . . ?
Pb1 N1 C1 C2 -177.2(2) . . . . ?
N1 C1 C2 C5 -1.0(4) . . . . ?
C1 N1 C4 C3 -1.0(4) . . . . ?
Pb1 N1 C4 C3 177.8(2) . . . . ?
C5 C3 C4 N1 -0.1(4) . . . . ?
C6 C3 C4 N1 176.3(2) . . . . ?
C1 C2 C5 C3 -0.1(4) . . . . ?
C4 C3 C5 C2 0.6(4) . . . . ?
C6 C3 C5 C2 -175.4(2) . . . . ?
N5 N6 C6 O1 1.9(4) . . . . ?
N5 N6 C6 C3 177.6(2) . . . . ?
C4 C3 C6 O1 1.2(4) . . . . ?
C5 C3 C6 O1 177.2(3) . . . . ?
C4 C3 C6 N6 -174.6(2) . . . . ?
C5 C3 C6 N6 1.5(4) . . . . ?
N6 N5 C23 C16 -177.8(2) . . . . ?
N6 N5 C23 C24 2.9(4) . . . . ?
C17 C16 C23 N5 158.7(3) . . . . ?
C15 C16 C23 N5 -19.1(4) . . . . ?
C17 C16 C23 C24 -22.0(4) . . . . ?
C15 C16 C23 C24 160.2(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        28.28
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.119
_refine_diff_density_min         -1.624
_refine_diff_density_rms         0.127
####################################################################### 
# 
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 1474992'
_audit_update_record             
;
2016-04-19 deposited with the CCDC.
2016-05-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C13 H12 N6 O7 Pb'
_chemical_formula_weight         571.48

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'
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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   9.0537(3)
_cell_length_b                   23.1055(8)
_cell_length_c                   7.8698(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.4580(10)
_cell_angle_gamma                90.00
_cell_volume                     1628.38(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8349
_cell_measurement_theta_min      2.44
_cell_measurement_theta_max      32.59

_exptl_crystal_description       rod
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.331
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1080
_exptl_absorpt_coefficient_mu    10.416
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2865
_exptl_absorpt_correction_T_max  0.6240
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(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 APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            29363
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_sigmaI/netI    0.0445
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.76
_diffrn_reflns_theta_max         33.17
_reflns_number_total             6193
_reflns_number_gt                4981
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0195P)²+1.3056P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6193
_refine_ls_number_parameters     249
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0290
_refine_ls_wR_factor_ref         0.0538
_refine_ls_wR_factor_gt          0.0507
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.027
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.209579(12) 0.157539(5) 0.056512(14) 0.01198(3) Uani 1 1 d . . .
N1 N 0.4676(3) 0.28102(12) -0.3253(3) 0.0165(5) Uani 1 1 d . . .
N2 N 0.3729(3) 0.11237(11) -0.2179(3) 0.0126(5) Uani 1 1 d . . .
N3 N 0.3339(3) 0.05464(11) -0.2409(3) 0.0132(5) Uani 1 1 d . . .
H3B H 0.385(4) 0.0355(16) -0.290(4) 0.018(10) Uiso 1 1 d . . .
N4 N -0.0058(3) -0.10205(11) -0.2208(3) 0.0167(6) Uani 1 1 d . . .
N5 N 0.4107(3) 0.07583(12) 0.2989(3) 0.0159(5) Uani 1 1 d . . .
N6 N 0.0565(3) 0.23542(11) -0.2572(3) 0.0137(5) Uani 1 1 d . . .
O1 O 0.1251(2) 0.06735(9) -0.1180(3) 0.0158(4) Uani 1 1 d . . .
O2 O 0.3319(3) 0.11241(11) 0.3614(3) 0.0266(6) Uani 1 1 d . . .
O3 O 0.4053(3) 0.07358(11) 0.1385(3) 0.0266(6) Uani 1 1 d . . .
O4 O 0.4965(3) 0.04381(11) 0.3934(3) 0.0290(6) Uani 1 1 d . . .
O5 O 0.0114(2) 0.18614(10) -0.2222(3) 0.0172(5) Uani 1 1 d . . .
O6 O 0.1731(2) 0.25598(10) -0.1692(3) 0.0191(5) Uani 1 1 d . . .
O7 O -0.0099(3) 0.26399(11) -0.3783(3) 0.0233(5) Uani 1 1 d . . .
C1 C 0.1465(3) -0.02009(13) -0.2672(4) 0.0119(6) Uani 1 1 d . . .
C2 C 0.0636(3) -0.05329(13) -0.1671(4) 0.0148(6) Uani 1 1 d . . .
H2A H 0.0564 -0.0403 -0.0541 0.018 Uiso 1 1 calc R . .
C3 C 0.0067(3) -0.12010(14) -0.3809(4) 0.0163(6) Uani 1 1 d . . .
H3A H -0.0431 -0.1546 -0.4221 0.020 Uiso 1 1 calc R . .
C4 C 0.0886(3) -0.09061(14) -0.4875(4) 0.0156(6) Uani 1 1 d . . .
H4A H 0.0965 -0.1053 -0.5986 0.019 Uiso 1 1 calc R . .
C5 C 0.1590(3) -0.03951(14) -0.4314(4) 0.0141(6) Uani 1 1 d . . .
H5A H 0.2147 -0.0182 -0.5035 0.017 Uiso 1 1 calc R . .
C6 C 0.2018(3) 0.03734(13) -0.2008(4) 0.0131(6) Uani 1 1 d . . .
C7 C 0.5125(3) 0.12431(13) -0.2125(3) 0.0116(6) Uani 1 1 d . . .
C8 C 0.6340(4) 0.08029(14) -0.2060(4) 0.0180(6) Uani 1 1 d . . .
H8A H 0.6218 0.0512 -0.1187 0.027 Uiso 1 1 calc R . .
H8B H 0.7311 0.0993 -0.1768 0.027 Uiso 1 1 calc R . .
H8C H 0.6288 0.0615 -0.3184 0.027 Uiso 1 1 calc R . .
C9 C 0.5475(3) 0.18659(13) -0.2188(4) 0.0127(6) Uani 1 1 d . . .
C10 C 0.4476(3) 0.22375(13) -0.3162(4) 0.0147(6) Uani 1 1 d . . .
H10A H 0.3602 0.2075 -0.3800 0.018 Uiso 1 1 calc R . .
C11 C 0.5918(3) 0.30336(14) -0.2360(4) 0.0174(6) Uani 1 1 d . . .
H11A H 0.6065 0.3440 -0.2397 0.021 Uiso 1 1 calc R . .
C12 C 0.6992(4) 0.27009(14) -0.1391(4) 0.0181(7) Uani 1 1 d . . .
H12A H 0.7866 0.2876 -0.0791 0.022 Uiso 1 1 calc R . .
C13 C 0.6783(3) 0.21091(14) -0.1302(4) 0.0158(6) Uani 1 1 d . . .
H13A H 0.7515 0.1872 -0.0650 0.019 Uiso 1 1 calc R . .


_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 2.550(2) . ?
Pb1 O3 2.643(2) . ?
Pb1 O2 2.700(2) . ?
Pb1 O5 2.704(2) . ?
Pb1 N4 2.724(3) 3 ?
Pb1 N1 2.775(3) 4_566 ?
N1 C11 1.338(4) . ?
N1 C10 1.339(4) . ?
N1 Pb1 2.775(3) 4_565 ?
N2 C7 1.288(4) . ?
N2 N3 1.385(4) . ?
N3 C6 1.342(4) . ?
N3 H3B 0.79(4) . ?
N4 C2 1.328(4) . ?
N4 C3 1.348(4) . ?
N4 Pb1 2.725(3) 3 ?
N5 O4 1.239(3) . ?
N5 O2 1.252(3) . ?
N5 O3 1.257(3) . ?
N6 O7 1.240(3) . ?
N6 O5 1.254(3) . ?
N6 O6 1.267(3) . ?
O1 C6 1.234(3) . ?
C1 C5 1.388(4) . ?
C1 C2 1.395(4) . ?
C1 C6 1.486(4) . ?
C2 H2A 0.9500 . ?
C3 C4 1.379(4) . ?
C3 H3A 0.9500 . ?
C4 C5 1.383(4) . ?
C4 H4A 0.9500 . ?
C5 H5A 0.9500 . ?
C7 C9 1.476(4) . ?
C7 C8 1.494(4) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.392(4) . ?
C9 C13 1.401(4) . ?
C10 H10A 0.9500 . ?
C11 C12 1.379(4) . ?
C11 H11A 0.9500 . ?
C12 C13 1.384(4) . ?
C12 H12A 0.9500 . ?
C13 H13A 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 O3 70.67(7) . . ?
O1 Pb1 O2 102.37(8) . . ?
O3 Pb1 O2 47.69(7) . . ?
O1 Pb1 O5 69.64(7) . . ?
O3 Pb1 O5 135.95(7) . . ?
O2 Pb1 O5 162.16(7) . . ?
O1 Pb1 N4 72.58(7) . 3 ?
O3 Pb1 N4 90.88(8) . 3 ?
O2 Pb1 N4 67.32(8) . 3 ?
O5 Pb1 N4 94.88(7) . 3 ?
O1 Pb1 N1 140.32(7) . 4_566 ?
O3 Pb1 N1 78.02(8) . 4_566 ?
O2 Pb1 N1 71.61(8) . 4_566 ?
O5 Pb1 N1 124.93(7) . 4_566 ?
N4 Pb1 N1 132.63(8) 3 4_566 ?
C11 N1 C10 117.6(3) . . ?
C11 N1 Pb1 125.4(2) . 4_565 ?
C10 N1 Pb1 114.2(2) . 4_565 ?
C7 N2 N3 116.2(3) . . ?
C6 N3 N2 118.4(3) . . ?
C6 N3 H3B 124(3) . . ?
N2 N3 H3B 117(3) . . ?
C2 N4 C3 117.3(3) . . ?
C2 N4 Pb1 124.73(19) . 3 ?
C3 N4 Pb1 117.0(2) . 3 ?
O4 N5 O2 120.7(3) . . ?
O4 N5 O3 120.5(3) . . ?
O2 N5 O3 118.8(3) . . ?
O7 N6 O5 121.0(3) . . ?
O7 N6 O6 119.5(3) . . ?
O5 N6 O6 119.5(3) . . ?
C6 O1 Pb1 126.6(2) . . ?
N5 O2 Pb1 95.42(17) . . ?
N5 O3 Pb1 98.06(18) . . ?
N6 O5 Pb1 101.61(17) . . ?
C5 C1 C2 118.2(3) . . ?
C5 C1 C6 123.1(3) . . ?
C2 C1 C6 118.3(3) . . ?
N4 C2 C1 123.7(3) . . ?
N4 C2 H2A 118.1 . . ?
C1 C2 H2A 118.1 . . ?
N4 C3 C4 122.9(3) . . ?
N4 C3 H3A 118.6 . . ?
C4 C3 H3A 118.6 . . ?
C3 C4 C5 119.4(3) . . ?
C3 C4 H4A 120.3 . . ?
C5 C4 H4A 120.3 . . ?
C4 C5 C1 118.4(3) . . ?
C4 C5 H5A 120.8 . . ?
C1 C5 H5A 120.8 . . ?
O1 C6 N3 123.2(3) . . ?
O1 C6 C1 120.1(3) . . ?
N3 C6 C1 116.7(3) . . ?
N2 C7 C9 115.0(3) . . ?
N2 C7 C8 124.7(3) . . ?
C9 C7 C8 120.3(3) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 C13 117.4(3) . . ?
C10 C9 C7 119.6(3) . . ?
C13 C9 C7 123.0(3) . . ?
N1 C10 C9 123.8(3) . . ?
N1 C10 H10A 118.1 . . ?
C9 C10 H10A 118.1 . . ?
N1 C11 C12 123.0(3) . . ?
N1 C11 H11A 118.5 . . ?
C12 C11 H11A 118.5 . . ?
C11 C12 C13 119.2(3) . . ?
C11 C12 H12A 120.4 . . ?
C13 C12 H12A 120.4 . . ?
C12 C13 C9 118.9(3) . . ?
C12 C13 H13A 120.6 . . ?
C9 C13 H13A 120.6 . . ?


_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        33.17
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.627
_refine_diff_density_min         -2.003
_refine_diff_density_rms         0.188
####################################################################### 
# 
# 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_6
_database_code_depnum_ccdc_archive 'CCDC 1474993'
_audit_update_record             
;
2016-04-19 deposited with the CCDC.
2016-05-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97

_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C15 H12 N6 O Pb S2'
_chemical_formula_weight         563.62

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'
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'
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.6135(4)
_cell_length_b                   9.3532(7)
_cell_length_c                   11.1952(10)
_cell_angle_alpha                87.356(7)
_cell_angle_beta                 87.566(5)
_cell_angle_gamma                82.906(5)
_cell_volume                     893.46(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8887
_cell_measurement_theta_min      28.60
_cell_measurement_theta_max      2.61

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.095
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             532
_exptl_absorpt_coefficient_mu    9.691
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
Interpolation using  Int.Tab. Vol. C (1992) p. 523,Tab. 6.3.3.3
for values of muR in the range 0-2.5, and Int.Tab. Vol.II (1959)
p.302; Table 5.3.6 B for muR in the range 2.6-10.0.
The interpolation procedure of C.W.Dwiggins Jr (Acta Cryst.(1975)
A31,146-148) is used with some modification.
;
_exptl_absorpt_correction_T_min  0.1872
_exptl_absorpt_correction_T_max  0.2090

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8887
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_sigmaI/netI    0.0432
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.91
_diffrn_reflns_theta_max         28.60
_reflns_number_total             4459
_reflns_number_gt                4115
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_structure_solution    "SIR92, J. Appl. Cryst. 26, 343-350, (1993)')"
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0305P)²+1.6668P] 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         4459
_refine_ls_number_parameters     227
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0319
_refine_ls_wR_factor_ref         0.0793
_refine_ls_wR_factor_gt          0.0773
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_restrained_S_all      1.147
_refine_ls_shift/su_max          0.002
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.87038(2) 0.20284(2) 0.799039(15) 0.02611(7) Uani 1 1 d . . .
O1 O 1.0111(5) 0.1834(5) 0.5944(4) 0.0499(12) Uani 1 1 d . . .
S1 S 0.68239(19) 0.0982(2) 1.01529(16) 0.0498(4) Uani 1 1 d . . .
S2 S 0.5139(2) 0.3466(3) 0.7783(2) 0.0733(6) Uani 1 1 d . . .
N1 N 1.2478(5) 0.0107(5) 0.3019(4) 0.0366(11) Uani 1 1 d . . .
N2 N 1.1443(5) 0.3774(5) 0.5888(4) 0.0296(9) Uani 1 1 d . . .
H2N H 1.2143 0.4242 0.5537 0.036 Uiso 1 1 calc R . .
N3 N 1.0544(5) 0.4316(5) 0.6856(4) 0.0277(9) Uani 1 1 d . . .
N4 N 0.9689(5) 0.7048(5) 1.0216(4) 0.0316(10) Uani 1 1 d . . .
N5 N 0.9023(12) -0.0068(7) 1.1781(7) 0.108(4) Uani 1 1 d . . .
N6 N 0.6641(8) 0.4600(8) 0.5784(6) 0.0628(17) Uani 1 1 d . . .
C1 C 1.3979(7) 0.0331(8) 0.2836(6) 0.0474(16) Uani 1 1 d . . .
H1 H 1.4580 -0.0169 0.2244 0.057 Uiso 1 1 calc R . .
C2 C 1.4661(7) 0.1279(9) 0.3496(7) 0.058(2) Uani 1 1 d . . .
H2 H 1.5709 0.1400 0.3352 0.069 Uiso 1 1 calc R . .
C3 C 1.3800(7) 0.2041(7) 0.4362(6) 0.0426(14) Uani 1 1 d . . .
H3 H 1.4245 0.2691 0.4805 0.051 Uiso 1 1 calc R . .
C4 C 1.2235(6) 0.1818(6) 0.4562(4) 0.0275(10) Uani 1 1 d . . .
C5 C 1.1646(6) 0.0837(6) 0.3866(5) 0.0310(11) Uani 1 1 d . . .
H5 H 1.0607 0.0680 0.4001 0.037 Uiso 1 1 calc R . .
C6 C 1.1172(6) 0.2485(6) 0.5521(4) 0.0286(11) Uani 1 1 d . . .
C7 C 1.0822(6) 0.5525(6) 0.7246(4) 0.0270(10) Uani 1 1 d . . .
C8 C 1.2045(7) 0.6424(7) 0.6771(6) 0.0441(15) Uani 1 1 d . . .
H8A H 1.3054 0.5857 0.6784 0.066 Uiso 1 1 calc R . .
H8B H 1.2046 0.7241 0.7259 0.066 Uiso 1 1 calc R . .
H8C H 1.1824 0.6751 0.5963 0.066 Uiso 1 1 calc R . .
C9 C 0.9820(6) 0.6053(5) 0.8274(4) 0.0252(10) Uani 1 1 d . . .
C10 C 1.0502(6) 0.6565(5) 0.9243(4) 0.0274(10) Uani 1 1 d . . .
H10 H 1.1581 0.6572 0.9214 0.033 Uiso 1 1 calc R . .
C11 C 0.8205(6) 0.6047(6) 0.8327(5) 0.0343(12) Uani 1 1 d . . .
H11 H 0.7698 0.5710 0.7699 0.041 Uiso 1 1 calc R . .
C12 C 0.7368(7) 0.6555(7) 0.9338(6) 0.0401(13) Uani 1 1 d . . .
H12 H 0.6287 0.6562 0.9396 0.048 Uiso 1 1 calc R . .
C13 C 0.8135(6) 0.7042(6) 1.0243(5) 0.0356(12) Uani 1 1 d . . .
H13 H 0.7555 0.7388 1.0912 0.043 Uiso 1 1 calc R . .
C14 C 0.8219(7) 0.0366(6) 1.1009(6) 0.0412(14) Uani 1 1 d . . .
C15 C 0.5996(7) 0.4104(7) 0.6582(6) 0.0387(13) 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
Pb1 N5 2.525(7) 2_757 ?
Pb1 O1 2.549(4) . ?
Pb1 N1 2.666(4) 2_756 ?
Pb1 N4 2.718(4) 2_767 ?
Pb1 S1 3.0464(17) . ?
Pb1 S2 3.209(2) . ?
O1 C6 1.227(6) . ?
S1 C14 1.603(7) . ?
S2 C15 1.631(7) . ?
N1 C5 1.327(7) . ?
N1 C1 1.341(7) . ?
N1 Pb1 2.666(4) 2_756 ?
N2 C6 1.341(6) . ?
N2 N3 1.384(6) . ?
N3 C7 1.283(6) . ?
N4 C10 1.335(6) . ?
N4 C13 1.338(7) . ?
N4 Pb1 2.718(4) 2_767 ?
N5 C14 1.158(8) . ?
N5 Pb1 2.525(7) 2_757 ?
N6 C15 1.143(8) . ?
C1 C2 1.380(9) . ?
C2 C3 1.367(9) . ?
C3 C4 1.397(7) . ?
C4 C5 1.386(7) . ?
C4 C6 1.489(7) . ?
C7 C9 1.475(7) . ?
C7 C8 1.494(7) . ?
C9 C10 1.386(7) . ?
C9 C11 1.391(7) . ?
C11 C12 1.386(8) . ?
C12 C13 1.359(8) . ?

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 Pb1 O1 73.6(2) 2_757 . ?
N5 Pb1 N1 80.63(19) 2_757 2_756 ?
O1 Pb1 N1 75.49(13) . 2_756 ?
N5 Pb1 N4 76.89(16) 2_757 2_767 ?
O1 Pb1 N4 116.78(14) . 2_767 ?
N1 Pb1 N4 149.38(15) 2_756 2_767 ?
N5 Pb1 S1 94.9(3) 2_757 . ?
O1 Pb1 S1 155.66(10) . . ?
N1 Pb1 S1 81.57(10) 2_756 . ?
N4 Pb1 S1 79.95(10) 2_767 . ?
N5 Pb1 S2 158.4(2) 2_757 . ?
O1 Pb1 S2 111.65(13) . . ?
N1 Pb1 S2 80.59(12) 2_756 . ?
N4 Pb1 S2 115.91(11) 2_767 . ?
S1 Pb1 S2 71.77(5) . . ?
C6 O1 Pb1 129.3(4) . . ?
C14 S1 Pb1 100.1(2) . . ?
C15 S2 Pb1 77.0(2) . . ?
C5 N1 C1 117.7(5) . . ?
C5 N1 Pb1 119.6(3) . 2_756 ?
C1 N1 Pb1 122.0(4) . 2_756 ?
C6 N2 N3 117.0(4) . . ?
C7 N3 N2 117.9(4) . . ?
C10 N4 C13 117.7(5) . . ?
C10 N4 Pb1 118.0(3) . 2_767 ?
C13 N4 Pb1 124.3(3) . 2_767 ?
C14 N5 Pb1 135.0(6) . 2_757 ?
N1 C1 C2 122.2(5) . . ?
C3 C2 C1 120.1(5) . . ?
C2 C3 C4 118.3(5) . . ?
C5 C4 C3 117.9(5) . . ?
C5 C4 C6 117.1(4) . . ?
C3 C4 C6 124.9(5) . . ?
N1 C5 C4 123.9(5) . . ?
O1 C6 N2 123.2(5) . . ?
O1 C6 C4 119.0(5) . . ?
N2 C6 C4 117.7(4) . . ?
N3 C7 C9 115.5(4) . . ?
N3 C7 C8 126.7(5) . . ?
C9 C7 C8 117.8(4) . . ?
C10 C9 C11 117.8(5) . . ?
C10 C9 C7 119.4(4) . . ?
C11 C9 C7 122.9(4) . . ?
N4 C10 C9 123.5(5) . . ?
C12 C11 C9 118.5(5) . . ?
C13 C12 C11 119.7(5) . . ?
N4 C13 C12 122.9(5) . . ?
N5 C14 S1 168.1(8) . . ?
N6 C15 S2 175.9(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 H2N N6 0.86 2.11 2.939(7) 161.3 2_766

_diffrn_measured_fraction_theta_max 0.977
_diffrn_reflns_theta_full        28.60
_diffrn_measured_fraction_theta_full 0.977
_refine_diff_density_max         1.901
_refine_diff_density_min         -1.146
_refine_diff_density_rms         0.166

