# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1840504'
_audit_update_record             
;
2018-07-12 deposited with the CCDC.
2018-07-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H34 N14 O4 Pb2'
_chemical_formula_weight         1165.17

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -4.0753 8.5060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   10.9860(4)
_cell_length_b                   21.7326(7)
_cell_length_c                   8.8856(4)
_cell_angle_alpha                90
_cell_angle_beta                 108.941(4)
_cell_angle_gamma                90
_cell_volume                     2006.60(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3673
_cell_measurement_theta_min      4.71
_cell_measurement_theta_max      61.48

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.928
_exptl_crystal_F_000             1112
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    16.613
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.00143
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
        (compiled May  6 2009,17:20:42)
        Empirical absorption correction using spherical harmonics,
        implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.5418
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Xcalibur, Onyx'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 8.1241
_diffrn_reflns_number            5500
_diffrn_reflns_av_unetI/netI     0.0852
_diffrn_reflns_av_R_equivalents  0.0923
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         4.717
_diffrn_reflns_theta_max         61.616
_diffrn_reflns_theta_full        61.616
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measured_fraction_theta_full 0.947
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_Laue_measured_fraction_full 0.947
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_point_group_measured_fraction_full 0.947
_reflns_number_total             2951
_reflns_number_gt                2443
_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, Oxford Diffraction Ltd.,
        Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
        (compiled May  6 2009,17:20:42)
;
_computing_cell_refinement       
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
        (compiled May  6 2009,17:20:42)
;
_computing_data_reduction        
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
        (compiled May  6 2009,17:20:42)
;
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    
;    
ORTEP-3 for Windows (Farrugia, 1997), DIAMOND (Brandenburg,
1999) and Mercury (Macrae et al., 2006)
;
_computing_publication_material  'PLATON (Spek, 2009)'
_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)+(0.1086P)²+46.7203P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2951
_refine_ls_number_parameters     263
_refine_ls_number_restraints     419
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0721
_refine_ls_wR_factor_ref         0.1875
_refine_ls_wR_factor_gt          0.1757
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_restrained_S_all      0.935
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb Pb 0.07591(5) 0.01649(2) 0.30755(7) 0.0271(3) Uani 1 1 d . U . . .
O1 O -0.1070(9) -0.0511(5) 0.1814(11) 0.032(2) Uani 1 1 d . U . . .
N1 N -0.1810(12) 0.0213(5) -0.0227(14) 0.026(3) Uani 1 1 d . U . . .
N2 N -0.0841(10) 0.0581(5) 0.0649(12) 0.022(2) Uani 1 1 d . U . . .
N3 N 0.1050(11) 0.1323(5) 0.2356(14) 0.027(2) Uani 1 1 d . U . . .
N4 N -0.0627(12) 0.0599(7) 0.4339(14) 0.034(3) Uani 1 1 d . U . . .
N5 N -0.1185(13) 0.1069(7) 0.3801(16) 0.042(3) Uani 1 1 d . U . . .
N6 N -0.1678(18) 0.1516(9) 0.326(2) 0.072(6) Uani 1 1 d . U . . .
C1 C -0.1815(12) -0.0306(6) 0.0445(16) 0.021(3) Uani 1 1 d . U . . .
C2 C -0.0905(13) 0.1150(6) 0.0159(16) 0.024(3) Uani 1 1 d . U . . .
C10 C 0.0142(13) 0.1564(6) 0.1055(18) 0.028(3) Uani 1 1 d . U . . .
C11 C 0.0208(15) 0.2173(7) 0.065(2) 0.039(4) Uani 1 1 d . U . . .
H11 H -0.043902 0.234104 -0.020019 0.047 Uiso 1 1 calc R U . . .
C12 C 0.1228(16) 0.2534(8) 0.152(2) 0.045(4) Uani 1 1 d . U . . .
H12 H 0.129534 0.293943 0.121784 0.054 Uiso 1 1 calc R U . . .
C13 C 0.2136(15) 0.2288(7) 0.281(2) 0.044(4) Uani 1 1 d . U . . .
H13 H 0.282814 0.252341 0.341890 0.053 Uiso 1 1 calc R U . . .
C14 C 0.2000(14) 0.1673(7) 0.320(2) 0.036(3) Uani 1 1 d . U . . .
H14 H 0.260728 0.150620 0.409684 0.043 Uiso 1 1 calc R U . . .
C21 C -0.2925(12) -0.0746(7) -0.0426(18) 0.030(3) Uani 1 1 d . U . . .
C22 C -0.3857(14) -0.0570(8) -0.188(2) 0.044(4) Uani 1 1 d . U . . .
H22 H -0.381441 -0.019298 -0.235531 0.053 Uiso 1 1 calc R U . . .
C23 C -0.4821(16) -0.0982(7) -0.255(2) 0.049(5) Uani 1 1 d . U . . .
H23 H -0.547590 -0.087576 -0.348007 0.059 Uiso 1 1 calc R U . . .
C24 C -0.4836(16) -0.1545(8) -0.188(2) 0.049(4) Uani 1 1 d . U . . .
H24 H -0.549605 -0.181799 -0.237993 0.058 Uiso 1 1 calc R U . . .
N7 N -0.3940(13) -0.1715(6) -0.0549(18) 0.046(3) Uani 1 1 d . U . . .
C26 C -0.2992(14) -0.1319(7) 0.0134(19) 0.034(3) Uani 1 1 d . U . . .
H26 H -0.234198 -0.144439 0.104477 0.040 Uiso 1 1 calc R U . . .
C30 C -0.1982(13) 0.1407(6) -0.1199(18) 0.029(3) Uani 1 1 d . U . . .
C31 C -0.3162(15) 0.1528(8) -0.101(2) 0.041(4) Uani 1 1 d . U . . .
H31 H -0.326772 0.144635 -0.003492 0.049 Uiso 1 1 calc R U . . .
C32 C -0.4152(17) 0.1756(10) -0.218(2) 0.053(4) Uani 1 1 d . U . . .
H32 H -0.495590 0.178306 -0.204976 0.064 Uiso 1 1 calc R U . . .
C33 C -0.4000(17) 0.1952(8) -0.359(2) 0.049(4) Uani 1 1 d . U . . .
H33 H -0.466079 0.214916 -0.436894 0.059 Uiso 1 1 calc R U . . .
C34 C -0.2822(17) 0.1842(9) -0.378(2) 0.054(4) Uani 1 1 d . U . . .
H34 H -0.269491 0.195842 -0.472922 0.064 Uiso 1 1 calc R U . . .
C35 C -0.1834(16) 0.1565(8) -0.261(2) 0.041(3) Uani 1 1 d . U . . .
H35 H -0.105952 0.148475 -0.278895 0.049 Uiso 1 1 calc R U . . .
C50 C 0.3489(19) 0.0406(13) 0.659(3) 0.074(7) Uani 1 1 d . U . . .
H50A H 0.420851 0.068111 0.696550 0.111 Uiso 1 1 calc R U . . .
H50B H 0.358533 0.015646 0.574846 0.111 Uiso 1 1 calc R U . . .
H50C H 0.345271 0.014695 0.745254 0.111 Uiso 1 1 calc R U . . .
O2 O 0.2337(11) 0.0752(7) 0.6023(15) 0.055(3) Uani 1 1 d . U . . .
H50 H 0.168860 0.073902 0.664686 0.082 Uiso 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb N4 2.362(12) . ?
Pb O1 2.447(9) . ?
Pb N2 2.469(10) . ?
Pb N3 2.642(12) . ?
O1 C1 1.304(16) . ?
N1 C1 1.278(17) . ?
N1 N2 1.357(16) . ?
N2 C2 1.305(18) . ?
N3 C14 1.312(18) . ?
N3 C10 1.364(18) . ?
N4 N5 1.208(19) . ?
N5 N6 1.14(2) . ?
C1 C21 1.544(19) . ?
C2 C10 1.475(19) . ?
C2 C30 1.50(2) . ?
C10 C11 1.38(2) . ?
C11 C12 1.38(2) . ?
C11 H11 0.9300 . ?
C12 C13 1.36(2) . ?
C12 H12 0.9300 . ?
C13 C14 1.40(2) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C21 C26 1.35(2) . ?
C21 C22 1.42(2) . ?
C22 C23 1.37(2) . ?
C22 H22 0.9300 . ?
C23 C24 1.36(2) . ?
C23 H23 0.9300 . ?
C24 N7 1.32(2) . ?
C24 H24 0.9300 . ?
N7 C26 1.335(19) . ?
C26 H26 0.9300 . ?
C30 C31 1.38(2) . ?
C30 C35 1.36(2) . ?
C31 C32 1.33(2) . ?
C31 H31 0.9300 . ?
C32 C33 1.38(3) . ?
C32 H32 0.9300 . ?
C33 C34 1.38(3) . ?
C33 H33 0.9300 . ?
C34 C35 1.37(2) . ?
C34 H34 0.9300 . ?
C35 H35 0.9300 . ?
C50 O2 1.42(2) . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 0.9600 . ?
O2 H50 1.0346 . ?

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
N4 Pb O1 84.1(4) . . ?
N4 Pb N2 83.3(4) . . ?
O1 Pb N2 64.8(3) . . ?
N4 Pb N3 83.2(4) . . ?
O1 Pb N3 127.4(3) . . ?
N2 Pb N3 63.1(3) . . ?
C1 O1 Pb 113.4(8) . . ?
C1 N1 N2 112.0(11) . . ?
C2 N2 N1 114.8(10) . . ?
C2 N2 Pb 125.8(9) . . ?
N1 N2 Pb 119.3(8) . . ?
C14 N3 C10 119.3(13) . . ?
C14 N3 Pb 123.4(10) . . ?
C10 N3 Pb 117.3(8) . . ?
N5 N4 Pb 118.2(10) . . ?
N6 N5 N4 177.3(18) . . ?
N1 C1 O1 129.8(13) . . ?
N1 C1 C21 115.7(12) . . ?
O1 C1 C21 114.3(11) . . ?
N2 C2 C10 116.8(12) . . ?
N2 C2 C30 124.5(12) . . ?
C10 C2 C30 118.7(12) . . ?
N3 C10 C11 120.2(13) . . ?
N3 C10 C2 116.8(12) . . ?
C11 C10 C2 123.0(13) . . ?
C10 C11 C12 120.3(15) . . ?
C10 C11 H11 119.8 . . ?
C12 C11 H11 119.8 . . ?
C13 C12 C11 119.1(16) . . ?
C13 C12 H12 120.5 . . ?
C11 C12 H12 120.5 . . ?
C12 C13 C14 118.4(15) . . ?
C12 C13 H13 120.8 . . ?
C14 C13 H13 120.8 . . ?
N3 C14 C13 122.7(15) . . ?
N3 C14 H14 118.7 . . ?
C13 C14 H14 118.7 . . ?
C26 C21 C22 118.3(14) . . ?
C26 C21 C1 120.9(12) . . ?
C22 C21 C1 120.7(13) . . ?
C23 C22 C21 116.8(16) . . ?
C23 C22 H22 121.6 . . ?
C21 C22 H22 121.6 . . ?
C24 C23 C22 121.0(16) . . ?
C24 C23 H23 119.5 . . ?
C22 C23 H23 119.5 . . ?
N7 C24 C23 122.0(15) . . ?
N7 C24 H24 119.0 . . ?
C23 C24 H24 119.0 . . ?
C24 N7 C26 118.0(15) . . ?
N7 C26 C21 123.7(14) . . ?
N7 C26 H26 118.2 . . ?
C21 C26 H26 118.2 . . ?
C31 C30 C35 117.3(14) . . ?
C31 C30 C2 120.0(14) . . ?
C35 C30 C2 122.6(14) . . ?
C32 C31 C30 122.4(17) . . ?
C32 C31 H31 118.8 . . ?
C30 C31 H31 118.8 . . ?
C31 C32 C33 120.9(18) . . ?
C31 C32 H32 119.6 . . ?
C33 C32 H32 119.6 . . ?
C34 C33 C32 117.0(16) . . ?
C34 C33 H33 121.5 . . ?
C32 C33 H33 121.5 . . ?
C33 C34 C35 121.5(19) . . ?
C33 C34 H34 119.2 . . ?
C35 C34 H34 119.2 . . ?
C30 C35 C34 120.5(17) . . ?
C30 C35 H35 119.8 . . ?
C34 C35 H35 119.8 . . ?
O2 C50 H50A 109.5 . . ?
O2 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
O2 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C50 O2 H50 118.9 . . ?

_refine_diff_density_max         2.953
_refine_diff_density_min         -3.287
_refine_diff_density_rms         0.297

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1840505'
_audit_update_record             
;
2018-04-29 deposited with the CCDC.
2018-07-18 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT780_shelx               
;
PROBLEM: Coordinates do not Form a Properly Connected Set  
RESPONSE: This alert is an artefact due to the oligomeric nature 
of the complex - all the atoms in the asimmetric unit are in fact 
properly connected. 
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H15 Br N4 O2 Pb'
_chemical_formula_weight         606.44

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'
Br Br -0.2901 2.4595 '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'
_symmetry_space_group_name_H-M   P-1

_cell_length_a                   9.2807(13)
_cell_length_b                   10.2962(15)
_cell_length_c                   10.9703(13)
_cell_angle_alpha                103.736(2)
_cell_angle_beta                 105.229(3)
_cell_angle_gamma                102.200(2)
_cell_volume                     939.7(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    183(2)
_cell_measurement_reflns_used    3689
_cell_measurement_theta_min      3.3638
_cell_measurement_theta_max      26.3484


_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.143
_exptl_crystal_F_000             568
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    11.122
_shelx_estimated_absorpt_T_min   0.193
_shelx_estimated_absorpt_T_max   0.226
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   '(Blessing, 1995)'
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6642
_diffrn_ambient_temperature      183(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source_power             2.0000
_diffrn_source_voltage           50.0000
_diffrn_source_current           40.0000
_diffrn_radiation_source         'Sealed Tube'
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_detector       CCD
_diffrn_measurement_device       
;
Mercury (2x2 bin mode)
;
_diffrn_detector_area_resol_mean 14.9365
_diffrn_measurement_method       dtprofit.ref
_diffrn_reflns_number            8225
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_av_R_equivalents  0.0228
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.292
_diffrn_reflns_theta_max         26.344
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             3753
_reflns_number_gt                3456
_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       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0302P)²+3.8537P] 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         3753
_refine_ls_number_parameters     241
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_gt           0.0294
_refine_ls_wR_factor_ref         0.0703
_refine_ls_wR_factor_gt          0.0670
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_restrained_S_all      1.145
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.30987(2) 1.07814(2) 0.07443(2) 0.01879(8) Uani 1 1 d . . . . .
Br1 Br 0.44832(6) 0.86892(6) 0.10274(5) 0.02256(12) Uani 1 1 d . . . . .
O1 O 0.1506(5) 0.9069(4) -0.1495(4) 0.0237(8) Uani 1 1 d . . . . .
N1 N -0.0230(5) 0.8041(5) -0.0539(4) 0.0203(9) Uani 1 1 d . . . . .
N2 N 0.0815(5) 0.8957(5) 0.0678(4) 0.0179(9) Uani 1 1 d . . . . .
N3 N 0.2849(6) 1.0667(5) 0.3036(5) 0.0234(10) Uani 1 1 d . . . . .
N4 N -0.2463(8) 0.5028(6) -0.5276(6) 0.0442(15) Uani 1 1 d . . . . .
C1 C 0.0615(6) 0.8670(6) 0.1720(5) 0.0185(10) Uani 1 1 d . . . . .
C2 C 0.1719(7) 0.9581(6) 0.3020(5) 0.0213(11) Uani 1 1 d . . . . .
C3 C 0.1659(8) 0.9289(7) 0.4190(6) 0.0318(14) Uani 1 1 d . . . . .
H3 H 0.0858 0.8528 0.4168 0.038 Uiso 1 1 calc R U . . .
C4 C 0.2795(9) 1.0133(8) 0.5388(6) 0.0394(16) Uani 1 1 d . . . . .
H4 H 0.2783 0.9939 0.6190 0.047 Uiso 1 1 calc R U . . .
C5 C 0.3930(8) 1.1243(7) 0.5414(6) 0.0347(14) Uani 1 1 d . . . . .
H5 H 0.4707 1.1835 0.6225 0.042 Uiso 1 1 calc R U . . .
C6 C 0.3906(8) 1.1473(7) 0.4207(6) 0.0305(13) Uani 1 1 d . . . . .
H6 H 0.4684 1.2245 0.4217 0.037 Uiso 1 1 calc R U . . .
C7 C 0.0282(6) 0.8205(5) -0.1535(5) 0.0172(10) Uani 1 1 d . . . . .
C8 C -0.0724(6) 0.7124(6) -0.2841(5) 0.0192(11) Uani 1 1 d . . . . .
C9 C -0.0375(7) 0.7152(7) -0.3996(6) 0.0298(13) Uani 1 1 d . . . . .
H9 H 0.0460 0.7880 -0.3978 0.036 Uiso 1 1 calc R U . . .
C10 C -0.1270(9) 0.6098(7) -0.5175(6) 0.0369(15) Uani 1 1 d . . . . .
H10 H -0.1025 0.6133 -0.5957 0.044 Uiso 1 1 calc R U . . .
C11 C -0.2812(9) 0.5057(8) -0.4165(7) 0.0466(19) Uani 1 1 d . . . . .
H11 H -0.3691 0.4349 -0.4221 0.056 Uiso 1 1 calc R U . . .
C12 C -0.1994(9) 0.6033(7) -0.2957(7) 0.0360(15) Uani 1 1 d . . . . .
H12 H -0.2283 0.5972 -0.2199 0.043 Uiso 1 1 calc R U . . .
C13 C -0.0641(6) 0.7414(5) 0.1619(5) 0.0188(10) Uani 1 1 d . . . . .
C14 C -0.2055(7) 0.7537(6) 0.1770(6) 0.0243(12) Uani 1 1 d . . . . .
H14 H -0.2206 0.8436 0.2002 0.029 Uiso 1 1 calc R U . . .
C15 C -0.3247(7) 0.6364(6) 0.1586(6) 0.0275(13) Uani 1 1 d . . . . .
H15 H -0.4210 0.6461 0.1685 0.033 Uiso 1 1 calc R U . . .
C16 C -0.3026(7) 0.5038(6) 0.1255(6) 0.0279(13) Uani 1 1 d . . . . .
H16 H -0.3837 0.4226 0.1117 0.033 Uiso 1 1 calc R U . . .
C17 C -0.1574(8) 0.4924(7) 0.1128(6) 0.0320(14) Uani 1 1 d . . . . .
H17 H -0.1411 0.4029 0.0905 0.038 Uiso 1 1 calc R U . . .
C18 C -0.0397(8) 0.6097(6) 0.1323(6) 0.0284(13) Uani 1 1 d . . . . .
H18 H 0.0581 0.6012 0.1257 0.034 Uiso 1 1 calc R U . . .
O2 O -0.3770(5) 0.2321(5) -0.7359(5) 0.0343(10) Uani 1 1 d D . . . .
H2A H -0.325(9) 0.314(5) -0.686(7) 0.051 Uiso 1 1 d D U . . .
H2B H -0.312(8) 0.202(8) -0.771(8) 0.051 Uiso 1 1 d D 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 N2 2.489(5) . ?
Pb1 O1 2.503(4) . ?
Pb1 N3 2.612(5) . ?
Pb1 Br1 2.7687(6) . ?
O1 C7 1.270(7) . ?
N1 C7 1.332(7) . ?
N1 N2 1.395(6) . ?
N2 C1 1.295(7) . ?
N3 C6 1.337(8) . ?
N3 C2 1.355(7) . ?
N4 C11 1.336(10) . ?
N4 C10 1.347(10) . ?
C1 C2 1.468(8) . ?
C1 C13 1.507(7) . ?
C2 C3 1.399(8) . ?
C3 C4 1.391(9) . ?
C3 H3 0.9500 . ?
C4 C5 1.370(10) . ?
C4 H4 0.9500 . ?
C5 C6 1.395(9) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.504(7) . ?
C8 C9 1.393(8) . ?
C8 C12 1.401(8) . ?
C9 C10 1.388(9) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 C12 1.363(9) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C14 1.394(8) . ?
C13 C18 1.398(8) . ?
C14 C15 1.387(8) . ?
C14 H14 0.9500 . ?
C15 C16 1.401(9) . ?
C15 H15 0.9500 . ?
C16 C17 1.417(9) . ?
C16 H16 0.9500 . ?
C17 C18 1.376(9) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
O2 H2A 0.85(4) . ?
O2 H2B 0.86(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Pb1 O1 64.06(13) . . ?
N2 Pb1 N3 63.52(15) . . ?
O1 Pb1 N3 127.06(14) . . ?
N2 Pb1 Br1 80.44(10) . . ?
O1 Pb1 Br1 83.68(10) . . ?
N3 Pb1 Br1 81.03(11) . . ?
C7 O1 Pb1 115.5(3) . . ?
C7 N1 N2 111.0(4) . . ?
C1 N2 N1 115.4(4) . . ?
C1 N2 Pb1 123.9(4) . . ?
N1 N2 Pb1 120.1(3) . . ?
C6 N3 C2 118.4(5) . . ?
C6 N3 Pb1 123.7(4) . . ?
C2 N3 Pb1 117.0(4) . . ?
C11 N4 C10 115.9(6) . . ?
N2 C1 C2 117.3(5) . . ?
N2 C1 C13 122.1(5) . . ?
C2 C1 C13 120.6(5) . . ?
N3 C2 C3 121.3(5) . . ?
N3 C2 C1 117.5(5) . . ?
C3 C2 C1 121.1(5) . . ?
C4 C3 C2 118.8(6) . . ?
C4 C3 H3 120.6 . . ?
C2 C3 H3 120.6 . . ?
C5 C4 C3 120.2(6) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 C6 117.6(6) . . ?
C4 C5 H5 121.2 . . ?
C6 C5 H5 121.2 . . ?
N3 C6 C5 123.7(6) . . ?
N3 C6 H6 118.2 . . ?
C5 C6 H6 118.2 . . ?
O1 C7 N1 128.9(5) . . ?
O1 C7 C8 118.7(5) . . ?
N1 C7 C8 112.2(5) . . ?
C9 C8 C12 117.0(5) . . ?
C9 C8 C7 120.0(5) . . ?
C12 C8 C7 122.9(5) . . ?
C10 C9 C8 118.9(6) . . ?
C10 C9 H9 120.6 . . ?
C8 C9 H9 120.6 . . ?
N4 C10 C9 123.9(6) . . ?
N4 C10 H10 118.0 . . ?
C9 C10 H10 118.0 . . ?
N4 C11 C12 124.6(7) . . ?
N4 C11 H11 117.7 . . ?
C12 C11 H11 117.7 . . ?
C11 C12 C8 119.6(6) . . ?
C11 C12 H12 120.2 . . ?
C8 C12 H12 120.2 . . ?
C14 C13 C18 119.7(5) . . ?
C14 C13 C1 121.1(5) . . ?
C18 C13 C1 119.2(5) . . ?
C15 C14 C13 120.9(5) . . ?
C15 C14 H14 119.6 . . ?
C13 C14 H14 119.6 . . ?
C14 C15 C16 119.7(6) . . ?
C14 C15 H15 120.1 . . ?
C16 C15 H15 120.1 . . ?
C15 C16 C17 119.0(6) . . ?
C15 C16 H16 120.5 . . ?
C17 C16 H16 120.5 . . ?
C18 C17 C16 120.7(6) . . ?
C18 C17 H17 119.7 . . ?
C16 C17 H17 119.7 . . ?
C17 C18 C13 120.0(6) . . ?
C17 C18 H18 120.0 . . ?
C13 C18 H18 120.0 . . ?
H2A O2 H2B 104(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 N1 N2 C1 -164.9(5) . . . . ?
C7 N1 N2 Pb1 6.9(5) . . . . ?
N1 N2 C1 C2 178.1(4) . . . . ?
Pb1 N2 C1 C2 6.7(7) . . . . ?
N1 N2 C1 C13 1.3(7) . . . . ?
Pb1 N2 C1 C13 -170.1(4) . . . . ?
C6 N3 C2 C3 -0.7(8) . . . . ?
Pb1 N3 C2 C3 168.9(5) . . . . ?
C6 N3 C2 C1 -177.2(5) . . . . ?
Pb1 N3 C2 C1 -7.6(6) . . . . ?
N2 C1 C2 N3 1.2(7) . . . . ?
C13 C1 C2 N3 178.0(5) . . . . ?
N2 C1 C2 C3 -175.3(5) . . . . ?
C13 C1 C2 C3 1.5(8) . . . . ?
N3 C2 C3 C4 -0.4(10) . . . . ?
C1 C2 C3 C4 175.9(6) . . . . ?
C2 C3 C4 C5 1.2(11) . . . . ?
C3 C4 C5 C6 -0.7(11) . . . . ?
C2 N3 C6 C5 1.3(9) . . . . ?
Pb1 N3 C6 C5 -167.6(5) . . . . ?
C4 C5 C6 N3 -0.5(11) . . . . ?
Pb1 O1 C7 N1 -3.6(7) . . . . ?
Pb1 O1 C7 C8 -178.9(3) . . . . ?
N2 N1 C7 O1 -2.0(8) . . . . ?
N2 N1 C7 C8 173.5(4) . . . . ?
O1 C7 C8 C9 -5.1(8) . . . . ?
N1 C7 C8 C9 178.9(5) . . . . ?
O1 C7 C8 C12 172.6(6) . . . . ?
N1 C7 C8 C12 -3.4(8) . . . . ?
C12 C8 C9 C10 -1.3(9) . . . . ?
C7 C8 C9 C10 176.5(6) . . . . ?
C11 N4 C10 C9 3.1(12) . . . . ?
C8 C9 C10 N4 -0.5(11) . . . . ?
C10 N4 C11 C12 -4.0(13) . . . . ?
N4 C11 C12 C8 2.4(13) . . . . ?
C9 C8 C12 C11 0.5(10) . . . . ?
C7 C8 C12 C11 -177.2(7) . . . . ?
N2 C1 C13 C14 -98.9(7) . . . . ?
C2 C1 C13 C14 84.4(7) . . . . ?
N2 C1 C13 C18 78.8(7) . . . . ?
C2 C1 C13 C18 -97.8(6) . . . . ?
C18 C13 C14 C15 -2.2(8) . . . . ?
C1 C13 C14 C15 175.5(5) . . . . ?
C13 C14 C15 C16 0.5(9) . . . . ?
C14 C15 C16 C17 0.7(9) . . . . ?
C15 C16 C17 C18 -0.2(9) . . . . ?
C16 C17 C18 C13 -1.5(9) . . . . ?
C14 C13 C18 C17 2.7(9) . . . . ?
C1 C13 C18 C17 -175.1(5) . . . . ?

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
O2 H2A N4 0.85(4) 2.11(5) 2.924(7) 161(7) .
O2 H2B O1 0.86(4) 2.29(4) 3.139(6) 171(8) 2_564

_refine_diff_density_max         2.503
_refine_diff_density_min         -1.387
_refine_diff_density_rms         0.171

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1840507'
_audit_update_record             
;
2018-04-29 deposited with the CCDC.
2018-07-18 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT029_shelx               
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.833 Note 
RESPONSE: Due to crystal size the crystal was poorly diffracting and therefore
a large proportion of reflections were not observed. This has also led to some 
other problems with modeling of the structure, namely somewhat reduced 
precision in interatomic bonds, and impossibility of assignement of hydrogen 
positions on the solvent molecule. 
;

_vrf_PLAT041_shelx               
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ     Please Check
RESPONSE: Missing from the model are four hydrogen atoms of the methanol 
solvent. The solvent molecules occupy channels in the structure and are 
severely disordered. As a result, methanol molecules were could be modeled 
only approximetely, making any placement of hydrogen atoms unjustified. Th
;
# end Validation Reply Form


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C62 H56 N16 O2 Pb2 S4'
_chemical_formula_weight         1599.84

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'
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                   9.7763(6)
_cell_length_b                   11.3341(7)
_cell_length_c                   15.0580(10)
_cell_angle_alpha                105.607(7)
_cell_angle_beta                 91.747(6)
_cell_angle_gamma                101.222(6)
_cell_volume                     1570.19(18)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4486
_cell_measurement_theta_min      4.0346
_cell_measurement_theta_max      37.6792

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.692
_exptl_crystal_F_000             784
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    5.544
_exptl_absorpt_correction_T_min  0.24525
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  
;
Oxford Diffraction Xcalibur CCD
diffractometer
;
_diffrn_radiation_monochromator  graphite
_diffrn_detector_area_resol_mean 16.3426
_diffrn_reflns_number            5941
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         4.050
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.833
_diffrn_measured_fraction_theta_full 0.833
_diffrn_reflns_Laue_measured_fraction_max 0.833
_diffrn_reflns_Laue_measured_fraction_full 0.833
_diffrn_reflns_point_group_measured_fraction_max 0.833
_diffrn_reflns_point_group_measured_fraction_full 0.833
_reflns_number_total             4605
_reflns_number_gt                3967
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1087P)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         4605
_refine_ls_number_parameters     388
_refine_ls_number_restraints     17
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0509
_refine_ls_wR_factor_ref         0.1367
_refine_ls_wR_factor_gt          0.1336
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_restrained_S_all      1.004
_refine_ls_shift/su_max          0.008
_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
O1 O -0.090(2) 0.334(2) 0.8611(17) 0.231(9) Uani 1 1 d D U . . .
C31 C -0.169(3) 0.4077(18) 0.829(2) 0.27(2) Uani 1 1 d D U . A 1
Pb1 Pb 0.60106(3) 0.43273(3) 0.68632(2) 0.04442(16) Uani 1 1 d . . . . .
C10 C 0.1678(10) -0.0384(9) 0.6650(7) 0.048(2) Uani 1 1 d . . . . .
H10 H 0.2065 -0.0570 0.6085 0.058 Uiso 1 1 calc R U . . .
C11 C 0.0380(11) -0.1004(11) 0.6732(9) 0.064(3) Uani 1 1 d . . . . .
H11 H -0.0111 -0.1624 0.6225 0.076 Uiso 1 1 calc R U . . .
C17 C 0.5354(12) -0.0216(10) 0.8214(7) 0.054(3) Uani 1 1 d . . . . .
H17 H 0.4814 -0.0584 0.7653 0.065 Uiso 1 1 calc R U . . .
N3 N 0.4305(7) 0.1091(7) 0.6542(5) 0.0397(16) Uani 1 1 d . . . . .
C20 C 0.6916(13) 0.0760(15) 0.9843(9) 0.082(4) Uani 1 1 d . . . . .
H20 H 0.7477 0.1104 1.0398 0.099 Uiso 1 1 calc R U . . .
N2 N 0.5659(7) 0.1772(7) 0.6521(5) 0.0401(17) Uani 1 1 d . . . . .
C28 C 0.3499(12) 0.6077(11) 0.6760(9) 0.069(3) Uani 1 1 d . . . . .
H28 H 0.3976 0.6152 0.6246 0.082 Uiso 1 1 calc R U . . .
N5 N 0.4403(7) 0.3676(7) 0.8097(5) 0.0388(16) Uani 1 1 d . . . . .
C7 C 0.6326(12) -0.0245(10) 0.5882(8) 0.062(3) Uani 1 1 d . . . . .
H7A H 0.7158 -0.0483 0.5636 0.093 Uiso 1 1 calc R U . . .
H7B H 0.6131 -0.0556 0.6408 0.093 Uiso 1 1 calc R U . . .
H7C H 0.5553 -0.0592 0.5416 0.093 Uiso 1 1 calc R U . . .
C23 C 0.3166(12) 0.4477(13) 0.9430(9) 0.073(3) Uani 1 1 d . . . . .
H23A H 0.2606 0.5099 0.9585 0.109 Uiso 1 1 calc R U . . .
H23B H 0.2618 0.3678 0.9433 0.109 Uiso 1 1 calc R U . . .
H23C H 0.3963 0.4703 0.9876 0.109 Uiso 1 1 calc R U . . .
N4 N 0.4978(7) 0.2999(7) 0.8602(5) 0.0413(17) Uani 1 1 d . . . . .
C9 C 0.2440(9) 0.0530(8) 0.7406(6) 0.041(2) Uani 1 1 d . . . . .
N6 N 0.3872(8) 0.5353(8) 0.7256(6) 0.0489(19) Uani 1 1 d . . . . .
C29 C 0.3735(12) 0.3507(10) 0.4759(8) 0.059(3) Uani 1 1 d . . . . .
N1 N 0.7997(9) 0.3066(9) 0.6060(8) 0.063(2) Uani 1 1 d . . . . .
C21 C 0.6222(12) 0.1534(11) 0.9502(6) 0.068(3) Uani 1 1 d D . . . .
H21 H 0.6265 0.2362 0.9835 0.082 Uiso 1 1 calc R U . . .
C16 C 0.5460(8) 0.1010(8) 0.8640(5) 0.044(2) Uani 1 1 d D . . . .
C12 C -0.0211(11) -0.0734(11) 0.7538(9) 0.064(3) Uani 1 1 d . . . . .
H12 H -0.1123 -0.1134 0.7578 0.077 Uiso 1 1 calc R U . . .
C8 C 0.3859(8) 0.1177(8) 0.7341(6) 0.0348(18) Uani 1 1 d . . . . .
C13 C 0.0538(10) 0.0132(10) 0.8295(9) 0.071(3) Uani 1 1 d D . . . .
H13 H 0.0159 0.0265 0.8864 0.085 Uiso 1 1 calc R U . . .
C6 C 0.6538(10) 0.1144(8) 0.6170(6) 0.041(2) Uani 1 1 d . . . . .
C26 C 0.1756(15) 0.6595(14) 0.7725(12) 0.087(4) Uani 1 1 d . . . . .
H26 H 0.1024 0.7007 0.7875 0.104 Uiso 1 1 calc R U . . .
C3 C 1.0367(13) 0.2076(17) 0.5918(10) 0.084(4) Uani 1 1 d . . . . .
H3 H 1.1171 0.1748 0.5879 0.101 Uiso 1 1 calc R U . . .
C5 C 0.7902(11) 0.1870(10) 0.6059(7) 0.050(2) Uani 1 1 d . . . . .
C14 C 0.1840(10) 0.0808(11) 0.8233(8) 0.058(3) Uani 1 1 d . . . . .
H14 H 0.2309 0.1442 0.8740 0.070 Uiso 1 1 calc R U . . .
C4 C 0.9117(13) 0.1373(12) 0.5993(8) 0.067(3) Uani 1 1 d . . . . .
H4 H 0.9058 0.0547 0.6001 0.080 Uiso 1 1 calc R U . . .
C15 C 0.4782(8) 0.1820(8) 0.8210(6) 0.0374(19) Uani 1 1 d . . . . .
C27 C 0.2474(13) 0.6695(12) 0.6975(11) 0.078(4) Uani 1 1 d . . . . .
H27 H 0.2246 0.7192 0.6615 0.093 Uiso 1 1 calc R U . . .
C18 C 0.6040(13) -0.0923(13) 0.8604(9) 0.073(3) Uani 1 1 d . . . . .
H18 H 0.5965 -0.1765 0.8296 0.088 Uiso 1 1 calc R U . . .
C25 C 0.2145(12) 0.5858(11) 0.8265(10) 0.071(3) Uani 1 1 d . . . . .
H25 H 0.1690 0.5789 0.8788 0.085 Uiso 1 1 calc R U . . .
C19 C 0.6812(13) -0.0436(14) 0.9414(9) 0.071(3) Uani 1 1 d . . . . .
H19 H 0.7267 -0.0931 0.9671 0.085 Uiso 1 1 calc R U . . .
C24 C 0.3201(9) 0.5245(9) 0.8008(7) 0.047(2) Uani 1 1 d . . . . .
C22 C 0.3643(9) 0.4404(9) 0.8507(6) 0.043(2) Uani 1 1 d . . . . .
S1 S 0.2776(3) 0.3451(3) 0.3857(3) 0.0835(11) Uani 1 1 d . . . . .
C1 C 0.9210(12) 0.3745(14) 0.5972(11) 0.086(4) Uani 1 1 d . . . . .
H1 H 0.9258 0.4567 0.5956 0.104 Uiso 1 1 calc R U . . .
C2 C 1.0418(14) 0.3274(19) 0.5901(11) 0.095(5) Uani 1 1 d . . . . .
H2 H 1.1264 0.3778 0.5843 0.114 Uiso 1 1 calc R U . . .
N7 N 0.4412(15) 0.3477(12) 0.5369(8) 0.094(4) Uani 1 1 d . . . . .
S2 S 0.9301(7) 0.7442(7) 0.9401(4) 0.1412(19) Uani 1 1 d . U . . .
C30 C 0.8083(16) 0.6534(17) 0.8671(12) 0.100(4) Uani 1 1 d . U . . .
N8 N 0.6878(15) 0.6232(14) 0.8481(9) 0.107(4) Uani 1 1 d . 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
O1 C31 1.401(2) . ?
Pb1 N7 2.543(13) . ?
Pb1 N6 2.593(7) . ?
Pb1 N5 2.633(6) . ?
Pb1 N2 2.752(7) . ?
Pb1 N1 2.751(8) . ?
Pb1 N8 2.766(14) . ?
Pb1 S1 3.051(3) 2_666 ?
C10 C11 1.352(15) . ?
C10 C9 1.392(13) . ?
C11 C12 1.345(17) . ?
C17 C16 1.347(14) . ?
C17 C18 1.368(14) . ?
N3 C8 1.278(11) . ?
N3 N2 1.402(10) . ?
C20 C19 1.32(2) . ?
C20 C21 1.395(16) . ?
N2 C6 1.260(11) . ?
C28 C27 1.330(15) . ?
C28 N6 1.339(12) . ?
N5 C22 1.268(11) . ?
N5 N4 1.392(9) . ?
C7 C6 1.487(13) . ?
C23 C22 1.465(14) . ?
N4 C15 1.281(12) . ?
C9 C14 1.378(15) . ?
C9 C8 1.457(11) . ?
N6 C24 1.349(12) . ?
C29 N7 1.128(15) . ?
C29 S1 1.606(12) . ?
N1 C1 1.313(15) . ?
N1 C5 1.340(13) . ?
C21 C16 1.395(2) . ?
C16 C15 1.495(11) . ?
C12 C13 1.367(17) . ?
C8 C15 1.489(12) . ?
C13 C14 1.372(14) . ?
C6 C5 1.464(14) . ?
C26 C27 1.367(19) . ?
C26 C25 1.405(18) . ?
C3 C2 1.36(2) . ?
C3 C4 1.349(19) . ?
C5 C4 1.406(14) . ?
C18 C19 1.335(19) . ?
C25 C24 1.362(14) . ?
C24 C22 1.478(13) . ?
S1 Pb1 3.051(3) 2_666 ?
C1 C2 1.383(18) . ?
S2 C30 1.59(2) . ?
C30 N8 1.165(18) . ?

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
N7 Pb1 N6 76.7(4) . . ?
N7 Pb1 N5 103.1(3) . . ?
N6 Pb1 N5 61.4(2) . . ?
N7 Pb1 N2 76.7(3) . . ?
N6 Pb1 N2 119.0(2) . . ?
N5 Pb1 N2 72.9(2) . . ?
N7 Pb1 N1 90.9(4) . . ?
N6 Pb1 N1 167.5(3) . . ?
N5 Pb1 N1 124.4(2) . . ?
N2 Pb1 N1 58.4(2) . . ?
N7 Pb1 N8 148.0(4) . . ?
N6 Pb1 N8 74.7(4) . . ?
N5 Pb1 N8 75.2(3) . . ?
N2 Pb1 N8 130.5(3) . . ?
N1 Pb1 N8 116.9(4) . . ?
N7 Pb1 S1 86.9(3) . 2_666 ?
N6 Pb1 S1 87.02(19) . 2_666 ?
N5 Pb1 S1 142.72(18) . 2_666 ?
N2 Pb1 S1 144.01(17) . 2_666 ?
N1 Pb1 S1 90.65(19) . 2_666 ?
N8 Pb1 S1 77.7(3) . 2_666 ?
C11 C10 C9 120.4(11) . . ?
C12 C11 C10 120.9(12) . . ?
C16 C17 C18 120.2(10) . . ?
C8 N3 N2 116.4(7) . . ?
C19 C20 C21 123.0(12) . . ?
C6 N2 N3 116.4(8) . . ?
C6 N2 Pb1 124.7(6) . . ?
N3 N2 Pb1 117.3(5) . . ?
C27 C28 N6 122.6(11) . . ?
C22 N5 N4 117.6(7) . . ?
C22 N5 Pb1 119.3(5) . . ?
N4 N5 Pb1 113.9(5) . . ?
C15 N4 N5 115.0(7) . . ?
C14 C9 C10 118.9(9) . . ?
C14 C9 C8 119.8(9) . . ?
C10 C9 C8 121.2(8) . . ?
C28 N6 C24 119.4(8) . . ?
C28 N6 Pb1 120.3(7) . . ?
C24 N6 Pb1 120.0(6) . . ?
N7 C29 S1 176.1(13) . . ?
C1 N1 C5 119.8(10) . . ?
C1 N1 Pb1 117.2(9) . . ?
C5 N1 Pb1 119.2(6) . . ?
C20 C21 C16 117.0(11) . . ?
C17 C16 C21 119.2(9) . . ?
C17 C16 C15 121.4(7) . . ?
C21 C16 C15 119.4(8) . . ?
C11 C12 C13 119.5(10) . . ?
N3 C8 C9 119.0(8) . . ?
N3 C8 C15 122.1(7) . . ?
C9 C8 C15 118.7(7) . . ?
C12 C13 C14 121.3(11) . . ?
N2 C6 C5 115.9(9) . . ?
N2 C6 C7 126.2(9) . . ?
C5 C6 C7 117.8(8) . . ?
C27 C26 C25 118.7(10) . . ?
C2 C3 C4 118.2(11) . . ?
N1 C5 C4 119.2(10) . . ?
N1 C5 C6 118.5(8) . . ?
C4 C5 C6 122.3(10) . . ?
C9 C14 C13 118.8(11) . . ?
C3 C4 C5 121.0(12) . . ?
N4 C15 C8 123.3(7) . . ?
N4 C15 C16 120.0(7) . . ?
C8 C15 C16 116.6(7) . . ?
C28 C27 C26 119.7(11) . . ?
C19 C18 C17 121.8(13) . . ?
C24 C25 C26 118.8(12) . . ?
C20 C19 C18 118.6(11) . . ?
N6 C24 C25 120.7(10) . . ?
N6 C24 C22 116.4(8) . . ?
C25 C24 C22 122.8(10) . . ?
N5 C22 C23 125.5(9) . . ?
N5 C22 C24 117.0(8) . . ?
C23 C22 C24 117.5(9) . . ?
C29 S1 Pb1 109.0(4) . 2_666 ?
N1 C1 C2 122.0(14) . . ?
C3 C2 C1 119.9(13) . . ?
C29 N7 Pb1 157.4(11) . . ?
N8 C30 S2 145.5(18) . . ?
C30 N8 Pb1 115.7(15) . . ?

_refine_diff_density_max         1.679
_refine_diff_density_min         -1.768
_refine_diff_density_rms         0.161

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 1840508'
_audit_update_record             
;
2018-04-29 deposited with the CCDC.
2018-07-18 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         ?
_chemical_formula_sum            'C10 H10 N6 Pb S3'
_chemical_formula_weight         517.61

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_H-M_alt        'P c'
_space_group_name_Hall           'P -2yc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   9.0368(7)
_cell_length_b                   11.3777(10)
_cell_length_c                   7.6503(6)
_cell_angle_alpha                90
_cell_angle_beta                 112.279(4)
_cell_angle_gamma                90
_cell_volume                     727.87(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1804
_cell_measurement_theta_min      3.02
_cell_measurement_theta_max      30.13

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.362
_exptl_crystal_F_000             484
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    12.017
_shelx_estimated_absorpt_T_min   0.266
_shelx_estimated_absorpt_T_max   0.533
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER SADABS'
_exptl_absorpt_correction_T_min  0.6543
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'BRUKER APPEX-II CCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_reflns_number            4086
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.436
_diffrn_reflns_theta_max         29.561
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4086
_reflns_number_gt                3970
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.991
_reflns_Friedel_fraction_max     0.998
_reflns_Friedel_fraction_full    0.998

_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       'APPEX2 (BRUKER AXS, 2005)'
_computing_cell_refinement       'APPEX2 (BRUKER AXS, 2005)'
_computing_data_reduction        'APPEX2 (BRUKER AXS, 2005)'
_computing_structure_solution    'DIRDIF2008 (Breurskens et al, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (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)+(0.0243P)²+1.1133P] 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_abs_structure_details 
;
 Flack x determined using 1911 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.020(5)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4086
_refine_ls_number_parameters     191
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0229
_refine_ls_R_factor_gt           0.0217
_refine_ls_wR_factor_ref         0.0467
_refine_ls_wR_factor_gt          0.0461
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.049
_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
C1 C -0.0591(8) 0.3984(6) 0.5576(10) 0.0142(14) Uani 1 1 d . . . . .
H1 H -0.1522 0.3612 0.5605 0.017 Uiso 1 1 calc R U . . .
C2 C -0.0510(8) 0.5209(6) 0.5651(10) 0.0167(14) Uani 1 1 d . . . . .
H2 H -0.1367 0.5662 0.5724 0.020 Uiso 1 1 calc R U . . .
C3 C 0.0831(9) 0.5735(6) 0.5616(10) 0.0154(14) Uani 1 1 d . . . . .
H3 H 0.0916 0.6568 0.5648 0.018 Uiso 1 1 calc R U . . .
C4 C 0.2082(8) 0.5046(6) 0.5534(9) 0.0129(12) Uani 1 1 d . . . . .
H4 H 0.3034 0.5402 0.5538 0.015 Uiso 1 1 calc R U . . .
C5 C 0.1909(8) 0.3827(5) 0.5447(9) 0.0104(12) Uani 1 1 d . . . . .
C6 C 0.3163(7) 0.3060(6) 0.5235(8) 0.0085(12) Uani 1 1 d . . . . .
C7 C 0.4713(8) 0.3588(6) 0.5341(10) 0.0135(13) Uani 1 1 d . . . . .
H7A H 0.5594 0.3059 0.6042 0.020 Uiso 1 1 calc R U . . .
H7B H 0.4869 0.4347 0.5990 0.020 Uiso 1 1 calc R U . . .
H7C H 0.4689 0.3702 0.4061 0.020 Uiso 1 1 calc R U . . .
C8 C 0.3745(7) 0.0109(6) 0.4266(8) 0.0087(11) Uani 1 1 d . . . . .
C9 C -0.1110(7) 0.1545(6) 0.0068(9) 0.0083(11) Uani 1 1 d . . . . .
C10 C -0.3733(7) 0.2360(6) 0.2132(10) 0.0115(12) Uani 1 1 d . . . . .
N1 N 0.0578(6) 0.3312(5) 0.5467(7) 0.0103(10) Uani 1 1 d . . . . .
N2 N 0.2813(6) 0.1964(5) 0.4904(7) 0.0077(10) Uani 1 1 d . . . . .
N3 N 0.3919(7) 0.1280(5) 0.4555(8) 0.0086(10) Uani 1 1 d . . . . .
H3N H 0.473(10) 0.154(7) 0.446(11) 0.010 Uiso 1 1 d . U . . .
N4 N 0.4899(6) -0.0396(5) 0.3889(7) 0.0096(10) Uani 1 1 d D . . . .
H41N H 0.498(11) -0.115(3) 0.394(12) 0.012 Uiso 1 1 d D U . . .
H42N H 0.564(9) 0.005(7) 0.371(11) 0.012 Uiso 1 1 d . U . . .
N5 N -0.0447(7) 0.1678(5) 0.1695(8) 0.0132(11) Uani 1 1 d . . . . .
N6 N -0.3276(7) 0.1732(5) 0.3422(8) 0.0132(11) Uani 1 1 d . . . . .
Pb1 Pb 0.01133(2) 0.11091(2) 0.49449(2) 0.00729(6) Uani 1 1 d . . . . .
S1 S 0.21885(18) -0.06819(14) 0.4376(2) 0.0093(3) Uani 1 1 d . . . . .
S2 S -0.1961(2) 0.13359(15) -0.2207(2) 0.0122(3) Uani 1 1 d . . . . .
S3 S -0.43971(19) 0.32502(15) 0.0310(2) 0.0142(3) 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
C1 N1 1.332(9) . ?
C1 C2 1.396(10) . ?
C1 H1 0.9500 . ?
C2 C3 1.361(10) . ?
C2 H2 0.9500 . ?
C3 C4 1.396(9) . ?
C3 H3 0.9500 . ?
C4 C5 1.395(9) . ?
C4 H4 0.9500 . ?
C5 N1 1.344(8) . ?
C5 C6 1.487(9) . ?
C6 N2 1.287(8) . ?
C6 C7 1.498(9) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 N4 1.315(8) . ?
C8 N3 1.351(8) . ?
C8 S1 1.699(6) . ?
C9 N5 1.169(8) . ?
C9 S2 1.632(6) . ?
C10 N6 1.160(9) . ?
C10 S3 1.642(7) . ?
N1 Pb1 2.548(6) . ?
N2 N3 1.370(7) . ?
N2 Pb1 2.638(5) . ?
N3 H3N 0.81(9) . ?
N4 H41N 0.86(3) . ?
N4 H42N 0.89(8) . ?
N5 Pb1 2.430(5) . ?
Pb1 S1 2.9117(16) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 123.1(6) . . ?
N1 C1 H1 118.5 . . ?
C2 C1 H1 118.5 . . ?
C3 C2 C1 118.1(6) . . ?
C3 C2 H2 120.9 . . ?
C1 C2 H2 120.9 . . ?
C2 C3 C4 119.7(7) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C5 C4 C3 118.9(6) . . ?
C5 C4 H4 120.6 . . ?
C3 C4 H4 120.6 . . ?
N1 C5 C4 121.2(6) . . ?
N1 C5 C6 117.9(6) . . ?
C4 C5 C6 120.9(6) . . ?
N2 C6 C5 116.7(5) . . ?
N2 C6 C7 123.6(6) . . ?
C5 C6 C7 119.6(6) . . ?
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 . . ?
N4 C8 N3 114.5(6) . . ?
N4 C8 S1 121.3(5) . . ?
N3 C8 S1 124.2(5) . . ?
N5 C9 S2 177.4(6) . . ?
N6 C10 S3 179.4(6) . . ?
C1 N1 C5 119.0(6) . . ?
C1 N1 Pb1 119.1(4) . . ?
C5 N1 Pb1 121.5(4) . . ?
C6 N2 N3 116.4(5) . . ?
C6 N2 Pb1 120.9(4) . . ?
N3 N2 Pb1 122.6(4) . . ?
C8 N3 N2 123.0(5) . . ?
C8 N3 H3N 113(6) . . ?
N2 N3 H3N 124(6) . . ?
C8 N4 H41N 119(6) . . ?
C8 N4 H42N 119(5) . . ?
H41N N4 H42N 121(8) . . ?
C9 N5 Pb1 151.5(5) . . ?
N5 Pb1 N1 81.75(18) . . ?
N5 Pb1 N2 74.00(17) . . ?
N1 Pb1 N2 62.66(17) . . ?
N5 Pb1 S1 85.95(14) . . ?
N1 Pb1 S1 129.40(12) . . ?
N2 Pb1 S1 66.76(12) . . ?
C8 S1 Pb1 103.3(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 -0.2(11) . . . . ?
C1 C2 C3 C4 -0.9(11) . . . . ?
C2 C3 C4 C5 1.4(10) . . . . ?
C3 C4 C5 N1 -0.9(10) . . . . ?
C3 C4 C5 C6 176.1(6) . . . . ?
N1 C5 C6 N2 6.4(9) . . . . ?
C4 C5 C6 N2 -170.7(6) . . . . ?
N1 C5 C6 C7 -175.7(6) . . . . ?
C4 C5 C6 C7 7.2(9) . . . . ?
C2 C1 N1 C5 0.7(10) . . . . ?
C2 C1 N1 Pb1 -172.7(5) . . . . ?
C4 C5 N1 C1 -0.1(10) . . . . ?
C6 C5 N1 C1 -177.2(6) . . . . ?
C4 C5 N1 Pb1 173.2(5) . . . . ?
C6 C5 N1 Pb1 -3.9(8) . . . . ?
C5 C6 N2 N3 174.8(5) . . . . ?
C7 C6 N2 N3 -3.0(9) . . . . ?
C5 C6 N2 Pb1 -5.8(7) . . . . ?
C7 C6 N2 Pb1 176.4(5) . . . . ?
N4 C8 N3 N2 177.8(5) . . . . ?
S1 C8 N3 N2 -2.4(9) . . . . ?
C6 N2 N3 C8 177.1(6) . . . . ?
Pb1 N2 N3 C8 -2.3(8) . . . . ?
N4 C8 S1 Pb1 -175.4(5) . . . . ?
N3 C8 S1 Pb1 4.8(6) . . . . ?

_refine_diff_density_max         0.586
_refine_diff_density_min         -0.862
_refine_diff_density_rms         0.122

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC4
_database_code_depnum_ccdc_archive 'CCDC 1840506'
_audit_update_record             
;
2018-04-29 deposited with the CCDC.
2018-07-18 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         ?
_chemical_formula_sum            'C29 H24 N8 O3 Pb S2'
_chemical_formula_weight         803.87

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_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                   10.3837(2)
_cell_length_b                   11.5738(3)
_cell_length_c                   14.3370(3)
_cell_angle_alpha                95.2160(10)
_cell_angle_beta                 90.1200(10)
_cell_angle_gamma                113.7360(10)
_cell_volume                     1569.31(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    6668
_cell_measurement_theta_min      2.53
_cell_measurement_theta_max      19.46

_exptl_crystal_description       prismatic
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.699
_exptl_crystal_F_000             782
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    5.552
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4348
_exptl_absorpt_correction_T_max  0.8511
_exptl_absorpt_process_details   '(Blessing, 1995)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(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            29301
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_av_R_equivalents  0.0573
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.526
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_full        24.998
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measured_fraction_theta_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_point_group_measured_fraction_full 0.970
_reflns_number_total             5348
_reflns_number_gt                4282
_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 APEX2'
_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)+(0.0433P)²+1.9253P] 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         5348
_refine_ls_number_parameters     389
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0388
_refine_ls_wR_factor_ref         0.0900
_refine_ls_wR_factor_gt          0.0823
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.025
_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 0.86497(3) 0.95144(2) 0.66497(2) 0.04800(11) Uani 1 1 d . . . . .
C1 C 0.6140(6) 0.6457(6) 0.6482(4) 0.0428(15) Uani 1 1 d . . . . .
C2 C 0.9397(6) 0.7065(5) 0.7554(4) 0.0359(13) Uani 1 1 d . . . . .
C3 C 1.0660(6) 0.8237(5) 0.7885(4) 0.0363(13) Uani 1 1 d . . . . .
C4 C 1.1682(6) 1.1494(5) 0.7788(4) 0.0387(14) Uani 1 1 d . . . . .
C5 C 0.4842(6) 0.5293(7) 0.6207(4) 0.0471(16) Uani 1 1 d . . . . .
C6 C 0.3609(7) 0.5408(8) 0.5930(5) 0.0600(19) Uani 1 1 d . . . . .
H6 H 0.3584 0.6201 0.5921 0.072 Uiso 1 1 calc R U . . .
C7 C 0.2439(8) 0.4323(9) 0.5672(5) 0.072(2) Uani 1 1 d . . . . .
H7 H 0.1599 0.4360 0.5485 0.086 Uiso 1 1 calc R U . . .
C8 C 0.2539(9) 0.3187(10) 0.5697(5) 0.082(3) Uani 1 1 d . . . . .
H8 H 0.1755 0.2439 0.5527 0.099 Uiso 1 1 calc R U . . .
C9 C 0.3798(8) 0.3131(7) 0.5973(5) 0.068(2) Uani 1 1 d . . . . .
H9 H 0.3842 0.2344 0.5976 0.082 Uiso 1 1 calc R U . . .
C10 C 0.9302(6) 0.5808(5) 0.7786(4) 0.0382(14) Uani 1 1 d . . . . .
C11 C 0.9335(7) 0.4906(6) 0.7077(5) 0.0523(17) Uani 1 1 d . . . . .
H11 H 0.9422 0.5095 0.6458 0.063 Uiso 1 1 calc R U . . .
C12 C 0.9238(8) 0.3751(7) 0.7293(6) 0.065(2) Uani 1 1 d . . . . .
H12 H 0.9284 0.3163 0.6821 0.078 Uiso 1 1 calc R U . . .
C13 C 0.9075(7) 0.3452(7) 0.8198(7) 0.064(2) Uani 1 1 d . . . . .
H13 H 0.9000 0.2658 0.8338 0.077 Uiso 1 1 calc R U . . .
C14 C 0.9022(7) 0.4314(6) 0.8901(5) 0.0566(18) Uani 1 1 d . . . . .
H14 H 0.8892 0.4102 0.9514 0.068 Uiso 1 1 calc R U . . .
C15 C 0.9162(7) 0.5494(6) 0.8694(5) 0.0487(16) Uani 1 1 d . . . . .
H15 H 0.9163 0.6089 0.9176 0.058 Uiso 1 1 calc R U . . .
C16 C 1.1857(6) 0.8185(5) 0.8411(4) 0.0369(14) Uani 1 1 d . . . . .
C17 C 1.2884(7) 0.7898(6) 0.7944(5) 0.0509(17) Uani 1 1 d . . . . .
H17 H 1.2780 0.7658 0.7302 0.061 Uiso 1 1 calc R U . . .
C18 C 1.4057(7) 0.7975(7) 0.8444(6) 0.063(2) Uani 1 1 d . . . . .
H18 H 1.4749 0.7799 0.8129 0.076 Uiso 1 1 calc R U . . .
C19 C 1.4227(7) 0.8303(6) 0.9389(6) 0.0576(19) Uani 1 1 d . . . . .
H19 H 1.5022 0.8343 0.9714 0.069 Uiso 1 1 calc R U . . .
C20 C 1.3227(7) 0.8571(6) 0.9850(5) 0.0547(18) Uani 1 1 d . . . . .
H20 H 1.3338 0.8791 1.0494 0.066 Uiso 1 1 calc R U . . .
C21 C 1.2029(6) 0.8521(6) 0.9370(4) 0.0454(15) Uani 1 1 d . . . . .
H21 H 1.1353 0.8713 0.9692 0.055 Uiso 1 1 calc R U . . .
C22 C 1.2955(6) 1.2626(5) 0.8138(4) 0.0411(15) Uani 1 1 d . . . . .
C23 C 1.2887(8) 1.3808(6) 0.8259(5) 0.0555(18) Uani 1 1 d . . . . .
H23 H 1.2061 1.3900 0.8115 0.067 Uiso 1 1 calc R U . . .
C24 C 1.4083(9) 1.4836(6) 0.8600(5) 0.068(2) Uani 1 1 d . . . . .
H24 H 1.4085 1.5643 0.8692 0.081 Uiso 1 1 calc R U . . .
C25 C 1.5259(8) 1.4650(7) 0.8799(5) 0.068(2) Uani 1 1 d . . . . .
H25 H 1.6083 1.5329 0.9024 0.081 Uiso 1 1 calc R U . . .
C26 C 1.5217(7) 1.3444(7) 0.8662(5) 0.061(2) Uani 1 1 d . . . . .
H26 H 1.6031 1.3330 0.8800 0.074 Uiso 1 1 calc R U . . .
C27 C 0.7925(7) 0.8994(7) 0.8814(6) 0.0563(19) Uani 1 1 d . . . . .
C28 C 0.5647(16) 1.0653(16) 0.6760(14) 0.213(9) Uani 1 1 d . . . . .
H28A H 0.4949 1.0261 0.6258 0.320 Uiso 1 1 calc R U . . .
H28B H 0.5726 1.1500 0.6934 0.320 Uiso 1 1 calc R U . . .
H28C H 0.5376 1.0170 0.7290 0.320 Uiso 1 1 calc R U . . .
N1 N 0.7217(5) 0.6226(4) 0.6820(3) 0.0407(12) Uani 1 1 d . . . . .
H1 H 0.7135 0.5463 0.6861 0.049 Uiso 1 1 calc R U . . .
N2 N 0.8440(5) 0.7240(4) 0.7093(3) 0.0372(11) Uani 1 1 d . . . . .
N3 N 1.0636(5) 0.9282(4) 0.7675(3) 0.0388(12) Uani 1 1 d . . . . .
N4 N 1.1748(5) 1.0391(4) 0.7943(4) 0.0405(12) Uani 1 1 d . . . . .
H4 H 1.2488 1.0387 0.8211 0.049 Uiso 1 1 calc R U . . .
N5 N 0.4948(6) 0.4188(5) 0.6236(4) 0.0537(14) Uani 1 1 d . . . . .
N6 N 1.4087(5) 1.2440(5) 0.8348(4) 0.0515(14) Uani 1 1 d . . . . .
N7 N 0.7881(6) 0.9609(6) 0.8248(5) 0.0634(17) Uani 1 1 d . . . . .
O1 O 0.6203(5) 0.7526(4) 0.6413(3) 0.0578(12) Uani 1 1 d . . . . .
O2 O 1.0656(4) 1.1553(4) 0.7399(3) 0.0523(11) Uani 1 1 d . . . . .
O3 O 0.6954(9) 1.0694(8) 0.6462(6) 0.137(3) Uani 1 1 d . . . . .
H3 H 0.7350 1.1341 0.6076 0.206 Uiso 1 1 calc R U . . .
S1 S 0.8003(3) 0.8150(2) 0.96519(15) 0.0766(6) Uani 1 1 d . . . . .
C29 C 0.1126(11) 0.8508(17) 0.5442(7) 0.117(5) Uani 1 1 d . . . . .
N8 N 0.0978(9) 0.9312(7) 0.5416(5) 0.060(2) Uani 1 1 d . . . . .
S2 S 0.1542(4) 0.7295(4) 0.5325(2) 0.1334(11) 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 N7 2.436(6) . ?
Pb1 O2 2.575(4) . ?
Pb1 N3 2.644(5) . ?
Pb1 O1 2.648(4) . ?
Pb1 O3 2.652(7) . ?
Pb1 N2 2.688(5) . ?
C1 O1 1.225(7) . ?
C1 N1 1.348(8) . ?
C1 C5 1.492(8) . ?
C2 N2 1.284(7) . ?
C2 C10 1.486(8) . ?
C2 C3 1.494(8) . ?
C3 N3 1.283(7) . ?
C3 C16 1.477(8) . ?
C4 O2 1.230(7) . ?
C4 N4 1.345(7) . ?
C4 C22 1.483(8) . ?
C5 N5 1.332(8) . ?
C5 C6 1.400(9) . ?
C6 C7 1.369(10) . ?
C6 H6 0.9300 . ?
C7 C8 1.364(12) . ?
C7 H7 0.9300 . ?
C8 C9 1.393(12) . ?
C8 H8 0.9300 . ?
C9 N5 1.343(8) . ?
C9 H9 0.9300 . ?
C10 C15 1.376(9) . ?
C10 C11 1.400(9) . ?
C11 C12 1.364(9) . ?
C11 H11 0.9300 . ?
C12 C13 1.367(11) . ?
C12 H12 0.9300 . ?
C13 C14 1.369(10) . ?
C13 H13 0.9300 . ?
C14 C15 1.374(9) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C21 1.385(8) . ?
C16 C17 1.395(9) . ?
C17 C18 1.378(9) . ?
C17 H17 0.9300 . ?
C18 C19 1.366(10) . ?
C18 H18 0.9300 . ?
C19 C20 1.354(10) . ?
C19 H19 0.9300 . ?
C20 C21 1.398(9) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C22 N6 1.316(8) . ?
C22 C23 1.394(9) . ?
C23 C24 1.379(10) . ?
C23 H23 0.9300 . ?
C24 C25 1.357(11) . ?
C24 H24 0.9300 . ?
C25 C26 1.374(10) . ?
C25 H25 0.9300 . ?
C26 N6 1.317(8) . ?
C26 H26 0.9300 . ?
C27 N7 1.139(9) . ?
C27 S1 1.637(10) . ?
C28 O3 1.407(13) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
N1 N2 1.363(6) . ?
N1 H1 0.8600 . ?
N3 N4 1.357(6) . ?
N4 H4 0.8600 . ?
O3 H3 0.9300 . ?
C29 N8 1.006(17) . ?
C29 S2 1.623(18) . ?

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
N7 Pb1 O2 78.85(19) . . ?
N7 Pb1 N3 76.08(19) . . ?
O2 Pb1 N3 61.90(14) . . ?
N7 Pb1 O1 82.31(19) . . ?
O2 Pb1 O1 160.77(15) . . ?
N3 Pb1 O1 116.97(14) . . ?
N7 Pb1 O3 79.5(3) . . ?
O2 Pb1 O3 92.3(2) . . ?
N3 Pb1 O3 147.3(2) . . ?
O1 Pb1 O3 80.4(2) . . ?
N7 Pb1 N2 80.76(19) . . ?
O2 Pb1 N2 119.88(13) . . ?
N3 Pb1 N2 58.44(14) . . ?
O1 Pb1 N2 60.01(14) . . ?
O3 Pb1 N2 137.6(2) . . ?
O1 C1 N1 123.5(5) . . ?
O1 C1 C5 122.3(6) . . ?
N1 C1 C5 114.2(6) . . ?
N2 C2 C10 124.6(5) . . ?
N2 C2 C3 115.6(5) . . ?
C10 C2 C3 119.8(5) . . ?
N3 C3 C16 122.6(5) . . ?
N3 C3 C2 115.6(5) . . ?
C16 C3 C2 121.8(5) . . ?
O2 C4 N4 122.9(5) . . ?
O2 C4 C22 123.6(5) . . ?
N4 C4 C22 113.5(5) . . ?
N5 C5 C6 123.9(6) . . ?
N5 C5 C1 116.4(6) . . ?
C6 C5 C1 119.7(7) . . ?
C7 C6 C5 118.4(8) . . ?
C7 C6 H6 120.8 . . ?
C5 C6 H6 120.8 . . ?
C8 C7 C6 118.2(8) . . ?
C8 C7 H7 120.9 . . ?
C6 C7 H7 120.9 . . ?
C7 C8 C9 121.0(7) . . ?
C7 C8 H8 119.5 . . ?
C9 C8 H8 119.5 . . ?
N5 C9 C8 121.4(8) . . ?
N5 C9 H9 119.3 . . ?
C8 C9 H9 119.3 . . ?
C15 C10 C11 118.4(6) . . ?
C15 C10 C2 121.3(6) . . ?
C11 C10 C2 120.4(6) . . ?
C12 C11 C10 120.2(7) . . ?
C12 C11 H11 119.9 . . ?
C10 C11 H11 119.9 . . ?
C11 C12 C13 120.4(7) . . ?
C11 C12 H12 119.8 . . ?
C13 C12 H12 119.8 . . ?
C12 C13 C14 120.4(6) . . ?
C12 C13 H13 119.8 . . ?
C14 C13 H13 119.8 . . ?
C13 C14 C15 119.6(7) . . ?
C13 C14 H14 120.2 . . ?
C15 C14 H14 120.2 . . ?
C10 C15 C14 121.0(6) . . ?
C10 C15 H15 119.5 . . ?
C14 C15 H15 119.5 . . ?
C21 C16 C17 119.1(6) . . ?
C21 C16 C3 120.0(5) . . ?
C17 C16 C3 120.7(5) . . ?
C18 C17 C16 119.3(7) . . ?
C18 C17 H17 120.3 . . ?
C16 C17 H17 120.3 . . ?
C19 C18 C17 121.6(7) . . ?
C19 C18 H18 119.2 . . ?
C17 C18 H18 119.2 . . ?
C20 C19 C18 119.4(6) . . ?
C20 C19 H19 120.3 . . ?
C18 C19 H19 120.3 . . ?
C19 C20 C21 120.9(6) . . ?
C19 C20 H20 119.5 . . ?
C21 C20 H20 119.5 . . ?
C16 C21 C20 119.6(6) . . ?
C16 C21 H21 120.2 . . ?
C20 C21 H21 120.2 . . ?
N6 C22 C23 123.5(6) . . ?
N6 C22 C4 117.2(5) . . ?
C23 C22 C4 119.3(6) . . ?
C24 C23 C22 117.7(7) . . ?
C24 C23 H23 121.1 . . ?
C22 C23 H23 121.1 . . ?
C25 C24 C23 118.7(7) . . ?
C25 C24 H24 120.6 . . ?
C23 C24 H24 120.6 . . ?
C24 C25 C26 119.1(7) . . ?
C24 C25 H25 120.5 . . ?
C26 C25 H25 120.5 . . ?
N6 C26 C25 123.7(7) . . ?
N6 C26 H26 118.2 . . ?
C25 C26 H26 118.2 . . ?
N7 C27 S1 178.1(7) . . ?
O3 C28 H28A 109.5 . . ?
O3 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
O3 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C1 N1 N2 118.0(5) . . ?
C1 N1 H1 121.0 . . ?
N2 N1 H1 121.0 . . ?
C2 N2 N1 119.1(5) . . ?
C2 N2 Pb1 124.2(4) . . ?
N1 N2 Pb1 116.6(3) . . ?
C3 N3 N4 119.3(5) . . ?
C3 N3 Pb1 126.0(4) . . ?
N4 N3 Pb1 114.6(3) . . ?
C4 N4 N3 119.4(5) . . ?
C4 N4 H4 120.3 . . ?
N3 N4 H4 120.3 . . ?
C5 N5 C9 117.2(6) . . ?
C22 N6 C26 117.2(6) . . ?
C27 N7 Pb1 126.6(6) . . ?
C1 O1 Pb1 120.3(4) . . ?
C4 O2 Pb1 120.0(4) . . ?
C28 O3 Pb1 140.2(9) . . ?
C28 O3 H3 109.9 . . ?
Pb1 O3 H3 109.9 . . ?
N8 C29 S2 169.8(12) . . ?

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
N2 C2 C3 N3 0.4(8) . . . . ?
C10 C2 C3 N3 -178.2(5) . . . . ?
N2 C2 C3 C16 -179.1(5) . . . . ?
C10 C2 C3 C16 2.3(8) . . . . ?
O1 C1 C5 N5 174.1(6) . . . . ?
N1 C1 C5 N5 -6.6(8) . . . . ?
O1 C1 C5 C6 -5.3(9) . . . . ?
N1 C1 C5 C6 174.0(6) . . . . ?
N5 C5 C6 C7 0.0(10) . . . . ?
C1 C5 C6 C7 179.3(6) . . . . ?
C5 C6 C7 C8 -0.1(11) . . . . ?
C6 C7 C8 C9 -0.3(12) . . . . ?
C7 C8 C9 N5 0.9(12) . . . . ?
N2 C2 C10 C15 -111.0(7) . . . . ?
C3 C2 C10 C15 67.4(8) . . . . ?
N2 C2 C10 C11 68.1(8) . . . . ?
C3 C2 C10 C11 -113.4(6) . . . . ?
C15 C10 C11 C12 -0.4(10) . . . . ?
C2 C10 C11 C12 -179.6(6) . . . . ?
C10 C11 C12 C13 1.6(11) . . . . ?
C11 C12 C13 C14 -0.7(12) . . . . ?
C12 C13 C14 C15 -1.3(11) . . . . ?
C11 C10 C15 C14 -1.6(9) . . . . ?
C2 C10 C15 C14 177.5(5) . . . . ?
C13 C14 C15 C10 2.5(10) . . . . ?
N3 C3 C16 C21 76.3(8) . . . . ?
C2 C3 C16 C21 -104.3(7) . . . . ?
N3 C3 C16 C17 -98.5(7) . . . . ?
C2 C3 C16 C17 81.0(7) . . . . ?
C21 C16 C17 C18 -1.0(9) . . . . ?
C3 C16 C17 C18 173.8(6) . . . . ?
C16 C17 C18 C19 1.2(10) . . . . ?
C17 C18 C19 C20 -0.5(11) . . . . ?
C18 C19 C20 C21 -0.3(10) . . . . ?
C17 C16 C21 C20 0.2(9) . . . . ?
C3 C16 C21 C20 -174.7(5) . . . . ?
C19 C20 C21 C16 0.5(9) . . . . ?
O2 C4 C22 N6 -165.3(6) . . . . ?
N4 C4 C22 N6 15.3(8) . . . . ?
O2 C4 C22 C23 16.9(9) . . . . ?
N4 C4 C22 C23 -162.5(6) . . . . ?
N6 C22 C23 C24 1.3(10) . . . . ?
C4 C22 C23 C24 179.0(6) . . . . ?
C22 C23 C24 C25 0.0(11) . . . . ?
C23 C24 C25 C26 -0.6(12) . . . . ?
C24 C25 C26 N6 -0.2(12) . . . . ?
O1 C1 N1 N2 -0.3(9) . . . . ?
C5 C1 N1 N2 -179.6(5) . . . . ?
C10 C2 N2 N1 2.7(9) . . . . ?
C3 C2 N2 N1 -175.9(5) . . . . ?
C10 C2 N2 Pb1 -178.7(4) . . . . ?
C3 C2 N2 Pb1 2.7(7) . . . . ?
C1 N1 N2 C2 168.8(5) . . . . ?
C1 N1 N2 Pb1 -9.9(6) . . . . ?
C16 C3 N3 N4 -0.1(9) . . . . ?
C2 C3 N3 N4 -179.5(5) . . . . ?
C16 C3 N3 Pb1 175.9(4) . . . . ?
C2 C3 N3 Pb1 -3.5(7) . . . . ?
O2 C4 N4 N3 -0.8(9) . . . . ?
C22 C4 N4 N3 178.6(5) . . . . ?
C3 N3 N4 C4 -175.0(5) . . . . ?
Pb1 N3 N4 C4 8.6(7) . . . . ?
C6 C5 N5 C9 0.6(10) . . . . ?
C1 C5 N5 C9 -178.7(6) . . . . ?
C8 C9 N5 C5 -1.0(10) . . . . ?
C23 C22 N6 C26 -2.0(10) . . . . ?
C4 C22 N6 C26 -179.7(6) . . . . ?
C25 C26 N6 C22 1.4(11) . . . . ?
N1 C1 O1 Pb1 10.8(8) . . . . ?
C5 C1 O1 Pb1 -170.0(4) . . . . ?
N4 C4 O2 Pb1 -8.1(8) . . . . ?
C22 C4 O2 Pb1 172.6(4) . . . . ?

_refine_diff_density_max         1.158
_refine_diff_density_min         -0.803
_refine_diff_density_rms         0.106

