# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 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_1
_database_code_depnum_ccdc_archive 'CCDC 1574896'
_audit_update_record             
;
2017-09-17 deposited with the CCDC.
2018-02-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H10 N6 O7 Pb'
_chemical_formula_sum            'C12 H10 N6 O7 Pb'
_chemical_formula_weight         557.45

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

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

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

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

_cell_length_a                   16.4079(3)
_cell_length_b                   7.18380(10)
_cell_length_c                   14.0179(3)
_cell_angle_alpha                90
_cell_angle_beta                 111.458(2)
_cell_angle_gamma                90
_cell_volume                     1537.78(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    16480
_cell_measurement_theta_min      2.83
_cell_measurement_theta_max      32.49

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.408
_exptl_crystal_F_000             1048
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_exptl_absorpt_coefficient_mu    11.026
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.345
_exptl_absorpt_correction_T_max  0.642
_exptl_absorpt_process_details   
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
        (compiled Apr 28 2010,14:27:37)
Analytical numeric absorption correction using a multifaceted crystal
        model based on expressions derived by R.C. Clark & J.S. Reid.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;

_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source, sealed tube'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur 2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 8.3504
_diffrn_reflns_number            30637
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.913
_diffrn_reflns_theta_max         30.995
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4880
_reflns_number_gt                4111
_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       'CrysAlis Pro (Oxford Diffraction Ltd., 2010)'
_computing_cell_refinement       'CrysAlis Pro (Oxford Diffraction Ltd., 2010)'
_computing_data_reduction        'CrysAlis Pro (Oxford Diffraction Ltd., 2010)'
_computing_structure_solution    'SIR92 (Altomare et al, 1993)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond v.3.2f (Crystal Impact GbR, 2008)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_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 > 2σ(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     
'w=1/[σ²(Fo²)+(0.0222P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4880
_refine_ls_number_parameters     241
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0234
_refine_ls_R_factor_gt           0.0182
_refine_ls_wR_factor_ref         0.0407
_refine_ls_wR_factor_gt          0.0402
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_restrained_S_all      0.959
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb Pb 0.26487(2) 0.10349(2) 0.06755(2) 0.00810(3) Uani 1 1 d . . . . .
O1 O 0.39622(11) 0.0000(3) 0.23883(13) 0.0112(4) Uani 1 1 d . . . . .
N1 N 0.10494(14) 0.1749(3) 0.06853(16) 0.0105(4) Uani 1 1 d . . . . .
N2 N 0.23177(13) 0.0196(3) 0.23030(15) 0.0093(4) Uani 1 1 d . . . . .
N3 N 0.29515(14) -0.0697(3) 0.30981(17) 0.0100(4) Uani 1 1 d . . . . .
H3N H 0.280(2) -0.145(4) 0.344(2) 0.012 Uiso 1 1 d . U . . .
N4 N 0.59076(14) -0.2870(3) 0.46595(16) 0.0118(4) Uani 1 1 d . . . . .
C1 C 0.37656(16) -0.0757(3) 0.30639(19) 0.0090(5) Uani 1 1 d . . . . .
C2 C 0.44364(16) -0.1709(4) 0.39581(18) 0.0086(5) Uani 1 1 d . . . . .
C3 C 0.52375(16) -0.2147(3) 0.38826(19) 0.0107(5) Uani 1 1 d . . . . .
H3 H 0.5311 -0.1921 0.3251 0.013 Uiso 1 1 calc R U . . .
C4 C 0.57955(17) -0.3193(4) 0.55482(19) 0.0119(5) Uani 1 1 d . . . . .
H4 H 0.6271 -0.3694 0.6105 0.014 Uiso 1 1 calc R U . . .
C5 C 0.50182(17) -0.2829(3) 0.56882(19) 0.0115(5) Uani 1 1 d . . . . .
H5 H 0.4960 -0.3097 0.6324 0.014 Uiso 1 1 calc R U . . .
C6 C 0.43231(16) -0.2064(4) 0.48817(19) 0.0102(5) Uani 1 1 d . . . . .
H6 H 0.3784 -0.1790 0.4958 0.012 Uiso 1 1 calc R U . . .
C7 C 0.15635(17) 0.0372(4) 0.2368(2) 0.0103(5) Uani 1 1 d . . . . .
H7 H 0.1432(18) -0.007(4) 0.293(2) 0.012 Uiso 1 1 d . U . . .
C8 C 0.08609(16) 0.1287(3) 0.15192(19) 0.0096(5) Uani 1 1 d . . . . .
C9 C 0.00525(17) 0.1608(4) 0.1587(2) 0.0127(5) Uani 1 1 d . . . . .
H9 H -0.0053 0.1280 0.2189 0.015 Uiso 1 1 calc R U . . .
C10 C -0.06024(17) 0.2419(4) 0.0757(2) 0.0136(5) Uani 1 1 d . . . . .
H10 H -0.1163 0.2665 0.0783 0.016 Uiso 1 1 calc R U . . .
C11 C -0.04242(17) 0.2861(4) -0.0103(2) 0.0143(5) Uani 1 1 d . . . . .
H11 H -0.0863 0.3397 -0.0685 0.017 Uiso 1 1 calc R U . . .
C12 C 0.04066(17) 0.2513(4) -0.0106(2) 0.0131(5) Uani 1 1 d . . . . .
H12 H 0.0525 0.2833 -0.0700 0.016 Uiso 1 1 calc R U . . .
N5 N 0.27504(14) 0.5146(3) 0.10387(18) 0.0140(4) Uani 1 1 d . . . . .
O2 O 0.30583(13) 0.3925(3) 0.17441(14) 0.0156(4) Uani 1 1 d . . . . .
O3 O 0.23468(13) 0.4563(3) 0.01351(15) 0.0173(4) Uani 1 1 d . . . . .
O4 O 0.28560(15) 0.6813(3) 0.12234(17) 0.0261(5) Uani 1 1 d . . . . .
N6 N 0.18702(14) -0.0200(3) -0.16984(16) 0.0127(4) Uani 1 1 d . . . . .
O5 O 0.25046(13) -0.1123(3) -0.10642(15) 0.0162(4) Uani 1 1 d . . . . .
O6 O 0.16902(14) 0.1357(3) -0.14111(15) 0.0185(4) Uani 1 1 d . . . . .
O7 O 0.14456(13) -0.0847(3) -0.25519(15) 0.0207(4) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb O2 2.5039(18) . ?
Pb N2 2.602(2) . ?
Pb O3 2.639(2) . ?
Pb N1 2.679(2) . ?
Pb O1 2.6789(17) . ?
Pb N4 2.695(2) 2_655 ?
O1 C1 1.233(3) . ?
N1 C12 1.337(3) . ?
N1 C8 1.355(3) . ?
N2 C7 1.280(3) . ?
N2 N3 1.374(3) . ?
N3 C1 1.355(3) . ?
N3 H3N 0.82(3) . ?
N4 C3 1.338(3) . ?
N4 C4 1.344(3) . ?
N4 Pb 2.695(2) 2_645 ?
C1 C2 1.497(3) . ?
C2 C3 1.393(3) . ?
C2 C6 1.397(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.384(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.392(3) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.474(3) . ?
C7 H7 0.94(3) . ?
C8 C9 1.383(3) . ?
C9 C10 1.391(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.378(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.387(4) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
N5 O4 1.224(3) . ?
N5 O3 1.267(3) . ?
N5 O2 1.279(3) . ?
N6 O7 1.234(3) . ?
N6 O6 1.260(3) . ?
N6 O5 1.279(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Pb N2 76.35(6) . . ?
O2 Pb O3 49.96(6) . . ?
N2 Pb O3 113.37(6) . . ?
O2 Pb N1 83.53(6) . . ?
N2 Pb N1 61.37(6) . . ?
O3 Pb N1 74.72(6) . . ?
O2 Pb O1 75.05(6) . . ?
N2 Pb O1 60.48(6) . . ?
O3 Pb O1 121.91(6) . . ?
N1 Pb O1 121.13(6) . . ?
O2 Pb N4 78.56(6) . 2_655 ?
N2 Pb N4 134.35(6) . 2_655 ?
O3 Pb N4 75.78(6) . 2_655 ?
N1 Pb N4 150.47(7) . 2_655 ?
O1 Pb N4 76.52(6) . 2_655 ?
C1 O1 Pb 117.39(15) . . ?
C12 N1 C8 117.1(2) . . ?
C12 N1 Pb 123.46(17) . . ?
C8 N1 Pb 119.39(16) . . ?
C7 N2 N3 116.9(2) . . ?
C7 N2 Pb 123.84(17) . . ?
N3 N2 Pb 118.73(15) . . ?
C1 N3 N2 116.7(2) . . ?
C1 N3 H3N 121(2) . . ?
N2 N3 H3N 118(2) . . ?
C3 N4 C4 118.1(2) . . ?
C3 N4 Pb 118.99(16) . 2_645 ?
C4 N4 Pb 122.55(16) . 2_645 ?
O1 C1 N3 123.5(2) . . ?
O1 C1 C2 121.7(2) . . ?
N3 C1 C2 114.6(2) . . ?
C3 C2 C6 118.6(2) . . ?
C3 C2 C1 117.7(2) . . ?
C6 C2 C1 123.6(2) . . ?
N4 C3 C2 122.9(2) . . ?
N4 C3 H3 118.5 . . ?
C2 C3 H3 118.5 . . ?
N4 C4 C5 123.0(2) . . ?
N4 C4 H4 118.5 . . ?
C5 C4 H4 118.5 . . ?
C4 C5 C6 118.9(2) . . ?
C4 C5 H5 120.6 . . ?
C6 C5 H5 120.6 . . ?
C5 C6 C2 118.5(2) . . ?
C5 C6 H6 120.7 . . ?
C2 C6 H6 120.7 . . ?
N2 C7 C8 118.5(2) . . ?
N2 C7 H7 123.2(17) . . ?
C8 C7 H7 118.3(17) . . ?
N1 C8 C9 123.1(2) . . ?
N1 C8 C7 116.6(2) . . ?
C9 C8 C7 120.3(2) . . ?
C8 C9 C10 118.6(2) . . ?
C8 C9 H9 120.7 . . ?
C10 C9 H9 120.7 . . ?
C11 C10 C9 118.8(2) . . ?
C11 C10 H10 120.6 . . ?
C9 C10 H10 120.6 . . ?
C10 C11 C12 119.0(2) . . ?
C10 C11 H11 120.5 . . ?
C12 C11 H11 120.5 . . ?
N1 C12 C11 123.3(2) . . ?
N1 C12 H12 118.3 . . ?
C11 C12 H12 118.3 . . ?
O4 N5 O3 121.1(2) . . ?
O4 N5 O2 121.5(2) . . ?
O3 N5 O2 117.4(2) . . ?
N5 O2 Pb 99.34(15) . . ?
N5 O3 Pb 93.21(14) . . ?
O7 N6 O6 121.9(2) . . ?
O7 N6 O5 120.4(2) . . ?
O6 N6 O5 117.7(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
C7 N2 N3 C1 -175.2(2) . . . . ?
Pb N2 N3 C1 12.5(3) . . . . ?
Pb O1 C1 N3 -16.2(3) . . . . ?
Pb O1 C1 C2 168.21(17) . . . . ?
N2 N3 C1 O1 2.9(4) . . . . ?
N2 N3 C1 C2 178.8(2) . . . . ?
O1 C1 C2 C3 -16.3(4) . . . . ?
N3 C1 C2 C3 167.7(2) . . . . ?
O1 C1 C2 C6 159.2(2) . . . . ?
N3 C1 C2 C6 -16.8(3) . . . . ?
C4 N4 C3 C2 0.3(4) . . . . ?
Pb N4 C3 C2 173.69(18) 2_645 . . . ?
C6 C2 C3 N4 -0.9(4) . . . . ?
C1 C2 C3 N4 174.9(2) . . . . ?
C3 N4 C4 C5 0.7(4) . . . . ?
Pb N4 C4 C5 -172.41(19) 2_645 . . . ?
N4 C4 C5 C6 -1.1(4) . . . . ?
C4 C5 C6 C2 0.6(4) . . . . ?
C3 C2 C6 C5 0.4(4) . . . . ?
C1 C2 C6 C5 -175.1(2) . . . . ?
N3 N2 C7 C8 -178.7(2) . . . . ?
Pb N2 C7 C8 -6.8(3) . . . . ?
C12 N1 C8 C9 -1.4(4) . . . . ?
Pb N1 C8 C9 179.97(18) . . . . ?
C12 N1 C8 C7 177.4(2) . . . . ?
Pb N1 C8 C7 -1.2(3) . . . . ?
N2 C7 C8 N1 5.1(4) . . . . ?
N2 C7 C8 C9 -176.0(2) . . . . ?
N1 C8 C9 C10 0.8(4) . . . . ?
C7 C8 C9 C10 -177.9(2) . . . . ?
C8 C9 C10 C11 0.5(4) . . . . ?
C9 C10 C11 C12 -1.1(4) . . . . ?
C8 N1 C12 C11 0.7(4) . . . . ?
Pb N1 C12 C11 179.25(19) . . . . ?
C10 C11 C12 N1 0.6(4) . . . . ?
O4 N5 O2 Pb -175.6(2) . . . . ?
O3 N5 O2 Pb 2.9(2) . . . . ?
O4 N5 O3 Pb 175.8(2) . . . . ?
O2 N5 O3 Pb -2.7(2) . . . . ?

_refine_diff_density_max         1.723
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.165

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

data_2
_database_code_depnum_ccdc_archive 'CCDC 1574897'
_audit_update_record             
;
2017-09-17 deposited with the CCDC.
2018-02-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C13 H12 N4 O2 Pb'
_chemical_formula_sum            'C13 H12 N4 O2 Pb'
_chemical_formula_weight         463.46

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

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

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.2696(6)
_cell_length_b                   9.6656(9)
_cell_length_c                   10.0853(9)
_cell_angle_alpha                93.2160(10)
_cell_angle_beta                 100.9110(10)
_cell_angle_gamma                105.0700(10)
_cell_volume                     667.75(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    2754
_cell_measurement_theta_min      2.31
_cell_measurement_theta_max      24.35

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.305
_exptl_crystal_F_000             432
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.440
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.130
_exptl_absorpt_coefficient_mu    12.640
_shelx_estimated_absorpt_T_min   0.072
_shelx_estimated_absorpt_T_max   0.290
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0619
_exptl_absorpt_correction_T_max  0.3003
_exptl_absorpt_process_details   ?

_exptl_absorpt_special_details   
;
 ?
;

_diffrn_ambient_temperature      193(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART1000 CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            3588
_diffrn_reflns_av_unetI/netI     0.0554
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.069
_diffrn_reflns_theta_max         25.042
_diffrn_reflns_theta_full        25.042
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 0.987
_reflns_number_total             2329
_reflns_number_gt                2171
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond v.3.2f (Crystal Impact GbR, 2008)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_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     
'w=1/[σ²(Fo²)+(0.0604P)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         2329
_refine_ls_number_parameters     182
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0340
_refine_ls_wR_factor_ref         0.0912
_refine_ls_wR_factor_gt          0.0893
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_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 0.27717(3) 0.07250(2) 0.50631(2) 0.01525(14) Uani 1 1 d . . . . .
O1 O 0.4583(8) 0.3238(5) 0.6090(5) 0.0231(12) Uani 1 1 d . . . . .
N4 N 0.8162(10) 0.7363(8) 0.6906(7) 0.0244(16) Uani 1 1 d . . . . .
N3 N 0.6238(9) 0.2517(6) 0.8031(6) 0.0194(14) Uani 1 1 d . . . . .
N2 N 0.5068(8) 0.1154(6) 0.7523(6) 0.0159(13) Uani 1 1 d . . . . .
N1 N 0.3047(9) -0.1582(6) 0.6456(6) 0.0196(14) Uani 1 1 d . . . . .
C1 C 0.7128(11) 0.5987(8) 0.6647(8) 0.0189(16) Uani 1 1 d . . . . .
H1 H 0.6352 0.5662 0.5760 0.023 Uiso 1 1 calc R U . . .
C2 C 0.7112(10) 0.4994(8) 0.7594(7) 0.0156(15) Uani 1 1 d . . . . .
C3 C 0.8226(10) 0.5468(7) 0.8885(8) 0.0183(15) Uani 1 1 d . . . . .
H3 H 0.8240 0.4826 0.9564 0.022 Uiso 1 1 calc R U . . .
C4 C 0.9330(11) 0.6903(8) 0.9180(8) 0.0229(17) Uani 1 1 d . . . . .
H4 H 1.0122 0.7258 1.0058 0.027 Uiso 1 1 calc R U . . .
C5 C 0.9242(12) 0.7799(8) 0.8160(9) 0.0233(18) Uani 1 1 d . . . . .
H5 H 0.9991 0.8778 0.8363 0.028 Uiso 1 1 calc R U . . .
C6 C 0.5858(10) 0.3480(8) 0.7176(7) 0.0157(15) Uani 1 1 d . . . . .
C7 C 0.5304(11) 0.0140(8) 0.8232(8) 0.0187(15) Uani 1 1 d . . . . .
H7 H 0.6194 0.0343 0.9086 0.022 Uiso 1 1 calc R U . . .
C8 C 0.4166(11) -0.1366(8) 0.7704(8) 0.0206(16) Uani 1 1 d . . . . .
C9 C 0.2090(12) -0.2937(8) 0.5940(9) 0.0277(18) Uani 1 1 d . . . . .
H9 H 0.1325 -0.3097 0.5042 0.033 Uiso 1 1 calc R U . . .
C10 C 0.2147(13) -0.4111(9) 0.6633(9) 0.0274(19) Uani 1 1 d . . . . .
H10 H 0.1423 -0.5055 0.6231 0.033 Uiso 1 1 calc R U . . .
C11 C 0.3280(13) -0.3886(9) 0.7923(10) 0.0267(19) Uani 1 1 d . . . . .
H11 H 0.3363 -0.4678 0.8426 0.032 Uiso 1 1 calc R U . . .
C12 C 0.4306(12) -0.2484(8) 0.8486(8) 0.0213(16) Uani 1 1 d . . . . .
H12 H 0.5080 -0.2300 0.9382 0.026 Uiso 1 1 calc R U . . .
C13 C 0.0757(13) 0.1756(9) 0.7363(9) 0.0258(19) Uani 1 1 d . . . . .
H13A H 0.1526 0.1351 0.8063 0.039 Uiso 1 1 calc R U . . .
H13B H -0.0509 0.1714 0.7588 0.039 Uiso 1 1 calc R U . . .
H13C H 0.1454 0.2762 0.7320 0.039 Uiso 1 1 calc R U . . .
O2 O 0.0470(7) 0.0959(5) 0.6102(5) 0.0219(12) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb O2 2.187(5) . ?
Pb O1 2.499(5) . ?
Pb O2 2.515(5) 2_556 ?
Pb N2 2.659(6) . ?
Pb N1 2.732(6) . ?
O1 C6 1.260(9) . ?
N4 C1 1.330(10) . ?
N4 C5 1.337(11) . ?
N3 C6 1.349(10) . ?
N3 N2 1.378(8) . ?
N2 C7 1.273(10) . ?
N1 C9 1.336(9) . ?
N1 C8 1.335(10) . ?
C1 C2 1.391(10) . ?
C1 H1 0.9500 . ?
C2 C3 1.379(10) . ?
C2 C6 1.497(10) . ?
C3 C4 1.393(10) . ?
C3 H3 0.9500 . ?
C4 C5 1.384(12) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C7 C8 1.485(10) . ?
C7 H7 0.9500 . ?
C8 C12 1.387(11) . ?
C9 C10 1.371(12) . ?
C9 H9 0.9500 . ?
C10 C11 1.374(13) . ?
C10 H10 0.9500 . ?
C11 C12 1.393(11) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 O2 1.400(9) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
O2 Pb 2.515(5) 2_556 ?

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
O2 Pb O1 86.62(18) . . ?
O2 Pb O2 68.89(19) . 2_556 ?
O1 Pb O2 146.12(18) . 2_556 ?
O2 Pb N2 86.25(19) . . ?
O1 Pb N2 60.51(17) . . ?
O2 Pb N2 136.24(18) 2_556 . ?
O2 Pb N1 88.4(2) . . ?
O1 Pb N1 120.95(18) . . ?
O2 Pb N1 82.66(18) 2_556 . ?
N2 Pb N1 60.45(18) . . ?
C6 O1 Pb 121.4(5) . . ?
C1 N4 C5 117.0(7) . . ?
C6 N3 N2 110.2(6) . . ?
C7 N2 N3 116.3(6) . . ?
C7 N2 Pb 123.6(5) . . ?
N3 N2 Pb 119.7(4) . . ?
C9 N1 C8 118.0(7) . . ?
C9 N1 Pb 122.4(5) . . ?
C8 N1 Pb 119.6(5) . . ?
N4 C1 C2 124.1(7) . . ?
N4 C1 H1 118.0 . . ?
C2 C1 H1 118.0 . . ?
C3 C2 C1 118.0(7) . . ?
C3 C2 C6 123.3(7) . . ?
C1 C2 C6 118.7(7) . . ?
C2 C3 C4 119.0(7) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
C5 C4 C3 118.2(7) . . ?
C5 C4 H4 120.9 . . ?
C3 C4 H4 120.9 . . ?
N4 C5 C4 123.7(7) . . ?
N4 C5 H5 118.2 . . ?
C4 C5 H5 118.2 . . ?
O1 C6 N3 127.2(6) . . ?
O1 C6 C2 117.9(7) . . ?
N3 C6 C2 114.9(6) . . ?
N2 C7 C8 119.0(7) . . ?
N2 C7 H7 120.5 . . ?
C8 C7 H7 120.5 . . ?
N1 C8 C12 122.4(7) . . ?
N1 C8 C7 117.2(7) . . ?
C12 C8 C7 120.3(7) . . ?
N1 C9 C10 123.7(8) . . ?
N1 C9 H9 118.1 . . ?
C10 C9 H9 118.1 . . ?
C9 C10 C11 118.3(7) . . ?
C9 C10 H10 120.8 . . ?
C11 C10 H10 120.8 . . ?
C10 C11 C12 119.3(8) . . ?
C10 C11 H11 120.4 . . ?
C12 C11 H11 120.4 . . ?
C8 C12 C11 118.3(8) . . ?
C8 C12 H12 120.9 . . ?
C11 C12 H12 120.9 . . ?
O2 C13 H13A 109.5 . . ?
O2 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
O2 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C13 O2 Pb 125.6(5) . . ?
C13 O2 Pb 122.6(5) . 2_556 ?
Pb O2 Pb 111.11(19) . 2_556 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 N3 N2 C7 179.2(7) . . . . ?
C6 N3 N2 Pb 5.6(7) . . . . ?
C5 N4 C1 C2 -0.1(12) . . . . ?
N4 C1 C2 C3 0.5(12) . . . . ?
N4 C1 C2 C6 179.1(7) . . . . ?
C1 C2 C3 C4 -0.8(11) . . . . ?
C6 C2 C3 C4 -179.3(7) . . . . ?
C2 C3 C4 C5 0.7(11) . . . . ?
C1 N4 C5 C4 -0.1(13) . . . . ?
C3 C4 C5 N4 -0.2(12) . . . . ?
Pb O1 C6 N3 -10.5(10) . . . . ?
Pb O1 C6 C2 169.6(5) . . . . ?
N2 N3 C6 O1 2.8(10) . . . . ?
N2 N3 C6 C2 -177.3(6) . . . . ?
C3 C2 C6 O1 164.4(7) . . . . ?
C1 C2 C6 O1 -14.1(10) . . . . ?
C3 C2 C6 N3 -15.5(11) . . . . ?
C1 C2 C6 N3 166.0(7) . . . . ?
N3 N2 C7 C8 -176.6(6) . . . . ?
Pb N2 C7 C8 -3.4(9) . . . . ?
C9 N1 C8 C12 -2.4(11) . . . . ?
Pb N1 C8 C12 177.3(5) . . . . ?
C9 N1 C8 C7 176.8(7) . . . . ?
Pb N1 C8 C7 -3.6(9) . . . . ?
N2 C7 C8 N1 4.6(10) . . . . ?
N2 C7 C8 C12 -176.2(7) . . . . ?
C8 N1 C9 C10 2.0(12) . . . . ?
Pb N1 C9 C10 -177.7(6) . . . . ?
N1 C9 C10 C11 -1.1(13) . . . . ?
C9 C10 C11 C12 0.7(13) . . . . ?
N1 C8 C12 C11 2.0(11) . . . . ?
C7 C8 C12 C11 -177.1(7) . . . . ?
C10 C11 C12 C8 -1.1(12) . . . . ?

_refine_diff_density_max         2.257
_refine_diff_density_min         -2.766
_refine_diff_density_rms         0.267

####################################################################### 
# 
# 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 1574899'
_audit_update_record             
;
2017-09-17 deposited with the CCDC.
2018-02-22 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         'C21 H24 N6 O7 Pb2'
_chemical_formula_sum            'C21 H24 N6 O7 Pb2'
_chemical_formula_weight         886.84

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

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

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

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

_cell_length_a                   10.281(5)
_cell_length_b                   17.050(8)
_cell_length_c                   15.015(7)
_cell_angle_alpha                90
_cell_angle_beta                 106.77(3)
_cell_angle_gamma                90
_cell_volume                     2520(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5062
_cell_measurement_theta_min      2.39
_cell_measurement_theta_max      32.90

_exptl_crystal_description       block
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.338
_exptl_crystal_F_000             1648
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    13.397
_shelx_estimated_absorpt_T_min   0.135
_shelx_estimated_absorpt_T_max   0.197
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.3691
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1563 before and 0.0590 after correction.
The Ratio of minimum to maximum transmission is 0.4944.
The λ/2 correction factor is 0.0015.
;

_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_source                   '(Mo) X-ray Source, sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            39215
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.069
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.988
_reflns_number_total             7596
_reflns_number_gt                6219
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    
'L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard, H. Puschmann, in preparation (2013)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond v.3.2f (Crystal Impact GbR, 2008)'
_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)+(0.0357P)²+0.4506P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00051(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         7596
_refine_ls_number_parameters     331
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0267
_refine_ls_wR_factor_ref         0.0684
_refine_ls_wR_factor_gt          0.0625
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.055
_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_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 0.36856(2) 0.85931(2) 0.99410(2) 0.01398(5) Uani 1 1 d . . . . .
Pb2 Pb 0.46502(2) 0.82701(2) 0.73306(2) 0.01515(5) Uani 1 1 d . . . . .
O1 O 0.4390(3) 0.91726(16) 0.86640(18) 0.0185(6) Uani 1 1 d . . . . .
N1 N 0.2219(3) 0.9210(2) 1.0849(2) 0.0162(7) Uani 1 1 d . . . . .
N2 N 0.3204(4) 1.00113(19) 0.9657(2) 0.0137(7) Uani 1 1 d . . . . .
N3 N 0.3738(4) 1.0410(2) 0.9053(2) 0.0168(7) Uani 1 1 d . . . . .
N4 N 0.4758(4) 1.02727(19) 0.7913(2) 0.0159(7) Uani 1 1 d . . . . .
H4N H 0.4718 1.0785 0.7842 0.019 Uiso 1 1 calc R U . . .
N5 N 0.5290(3) 0.9808(2) 0.7372(2) 0.0151(7) Uani 1 1 d . . . . .
N6 N 0.6024(4) 0.8770(2) 0.6268(2) 0.0183(7) Uani 1 1 d . . . . .
C1 C 0.1733(5) 0.8801(3) 1.1442(3) 0.0213(9) Uani 1 1 d . . . . .
H1 H 0.1965 0.8262 1.1535 0.026 Uiso 1 1 calc R U . . .
C2 C 0.0909(5) 0.9126(3) 1.1925(3) 0.0249(10) Uani 1 1 d . . . . .
H2 H 0.0594 0.8817 1.2346 0.030 Uiso 1 1 calc R U . . .
C3 C 0.0551(5) 0.9903(3) 1.1787(3) 0.0269(10) Uani 1 1 d . . . . .
H3 H -0.0041 1.0136 1.2094 0.032 Uiso 1 1 calc R U . . .
C4 C 0.1074(5) 1.0343(3) 1.1188(3) 0.0219(9) Uani 1 1 d . . . . .
H4 H 0.0858 1.0883 1.1090 0.026 Uiso 1 1 calc R U . . .
C5 C 0.1920(4) 0.9978(2) 1.0732(3) 0.0156(8) Uani 1 1 d . . . . .
C6 C 0.2498(4) 1.0412(2) 1.0088(3) 0.0169(8) Uani 1 1 d . . . . .
C7 C 0.2240(5) 1.1273(3) 0.9959(3) 0.0232(10) Uani 1 1 d . . . . .
H7A H 0.2710 1.1478 0.9526 0.035 Uiso 1 1 calc R U . . .
H7B H 0.2580 1.1540 1.0560 0.035 Uiso 1 1 calc R U . . .
H7C H 0.1262 1.1367 0.9707 0.035 Uiso 1 1 calc R U . . .
C8 C 0.4283(4) 0.9912(2) 0.8576(3) 0.0147(8) Uani 1 1 d . . . . .
C9 C 0.5721(4) 1.0107(3) 0.6717(3) 0.0168(8) Uani 1 1 d . . . . .
C10 C 0.5695(5) 1.0962(3) 0.6470(3) 0.0244(10) Uani 1 1 d . . . . .
H10A H 0.5063 1.1239 0.6739 0.037 Uiso 1 1 calc R U . . .
H10B H 0.5398 1.1021 0.5792 0.037 Uiso 1 1 calc R U . . .
H10C H 0.6608 1.1183 0.6719 0.037 Uiso 1 1 calc R U . . .
C11 C 0.6280(4) 0.9536(3) 0.6191(3) 0.0169(8) Uani 1 1 d . . . . .
C12 C 0.7075(5) 0.9785(3) 0.5630(3) 0.0262(10) Uani 1 1 d . . . . .
H12 H 0.7230 1.0329 0.5566 0.031 Uiso 1 1 calc R U . . .
C13 C 0.7635(5) 0.9237(3) 0.5168(3) 0.0321(11) Uani 1 1 d . . . . .
H13 H 0.8191 0.9399 0.4794 0.038 Uiso 1 1 calc R U . . .
C14 C 0.7374(5) 0.8457(3) 0.5259(3) 0.0273(11) Uani 1 1 d . . . . .
H14 H 0.7749 0.8068 0.4952 0.033 Uiso 1 1 calc R U . . .
C15 C 0.6548(5) 0.8247(3) 0.5810(3) 0.0208(9) Uani 1 1 d . . . . .
H15 H 0.6350 0.7707 0.5862 0.025 Uiso 1 1 calc R U . . .
O2 O 0.1545(3) 0.85453(17) 0.8846(2) 0.0199(6) Uani 1 1 d . . . . .
O3 O 0.2601(3) 0.76949(18) 0.8167(2) 0.0235(7) Uani 1 1 d . . . . .
O4 O 0.3074(3) 0.77435(18) 0.5810(2) 0.0247(7) Uani 1 1 d . . . . .
O5 O 0.2644(3) 0.89657(19) 0.6113(2) 0.0295(7) Uani 1 1 d . . . . .
O6 O 0.7250(4) 0.7746(2) 0.8055(2) 0.0315(8) Uani 1 1 d . . . . .
O7 O 0.5759(3) 0.69093(18) 0.7172(2) 0.0202(6) Uani 1 1 d . . . . .
C16 C 0.1604(4) 0.8111(3) 0.8165(3) 0.0179(8) Uani 1 1 d . . . . .
C17 C 0.0346(5) 0.8135(3) 0.7327(3) 0.0273(10) Uani 1 1 d . . . . .
H17A H 0.0366 0.8609 0.6963 0.041 Uiso 1 1 calc R U . . .
H17B H -0.0470 0.8139 0.7540 0.041 Uiso 1 1 calc R U . . .
H17C H 0.0333 0.7671 0.6939 0.041 Uiso 1 1 calc R U . . .
C18 C 0.2355(5) 0.8359(3) 0.5626(3) 0.0220(9) Uani 1 1 d . . . . .
C19 C 0.1113(6) 0.8342(3) 0.4801(4) 0.0352(12) Uani 1 1 d . . . . .
H19A H 0.0545 0.7893 0.4854 0.053 Uiso 1 1 calc R U . . .
H19B H 0.1386 0.8293 0.4229 0.053 Uiso 1 1 calc R U . . .
H19C H 0.0596 0.8828 0.4780 0.053 Uiso 1 1 calc R U . . .
C20 C 0.6963(5) 0.7089(3) 0.7696(3) 0.0216(9) Uani 1 1 d . . . . .
C21 C 0.8052(5) 0.6475(3) 0.7857(4) 0.0361(13) Uani 1 1 d . . . . .
H21A H 0.8919 0.6699 0.8225 0.054 Uiso 1 1 calc R U . . .
H21B H 0.8138 0.6293 0.7257 0.054 Uiso 1 1 calc R U . . .
H21C H 0.7811 0.6032 0.8194 0.054 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 O2 2.338(3) . ?
Pb1 O1 2.445(3) . ?
Pb1 N2 2.480(3) . ?
Pb1 N1 2.535(3) . ?
Pb2 O4 2.551(3) . ?
Pb2 N6 2.563(3) . ?
Pb2 O1 2.599(3) . ?
Pb2 O5 2.613(4) . ?
Pb2 O7 2.626(3) . ?
Pb2 N5 2.700(4) . ?
Pb2 O6 2.729(4) . ?
O1 C8 1.269(5) . ?
N1 C1 1.336(5) . ?
N1 C5 1.344(5) . ?
N2 C6 1.297(5) . ?
N2 N3 1.369(4) . ?
N3 C8 1.335(5) . ?
N4 N5 1.358(4) . ?
N4 C8 1.374(5) . ?
N4 H4N 0.8800 . ?
N5 C9 1.293(5) . ?
N6 C15 1.332(5) . ?
N6 C11 1.343(5) . ?
C1 C2 1.380(6) . ?
C1 H1 0.9500 . ?
C2 C3 1.375(7) . ?
C2 H2 0.9500 . ?
C3 C4 1.391(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.399(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.473(6) . ?
C6 C7 1.495(6) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C9 C11 1.471(6) . ?
C9 C10 1.503(6) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.398(5) . ?
C12 C13 1.384(6) . ?
C12 H12 0.9500 . ?
C13 C14 1.372(7) . ?
C13 H13 0.9500 . ?
C14 C15 1.394(6) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
O2 C16 1.278(5) . ?
O3 C16 1.246(5) . ?
O4 C18 1.268(5) . ?
O5 C18 1.252(5) . ?
O6 C20 1.241(5) . ?
O7 C20 1.297(5) . ?
C16 C17 1.522(6) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.501(7) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C21 1.501(7) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 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
O2 Pb1 O1 83.94(11) . . ?
O2 Pb1 N2 79.19(11) . . ?
O1 Pb1 N2 63.97(10) . . ?
O2 Pb1 N1 78.89(11) . . ?
O1 Pb1 N1 127.65(10) . . ?
N2 Pb1 N1 64.37(11) . . ?
O4 Pb2 N6 83.23(11) . . ?
O4 Pb2 O1 135.85(10) . . ?
N6 Pb2 O1 118.69(10) . . ?
O4 Pb2 O5 50.53(10) . . ?
N6 Pb2 O5 83.02(11) . . ?
O1 Pb2 O5 91.98(10) . . ?
O4 Pb2 O7 77.78(10) . . ?
N6 Pb2 O7 84.62(11) . . ?
O1 Pb2 O7 137.44(9) . . ?
O5 Pb2 O7 127.83(10) . . ?
O4 Pb2 N5 116.74(10) . . ?
N6 Pb2 N5 61.08(10) . . ?
O1 Pb2 N5 59.07(9) . . ?
O5 Pb2 N5 73.32(11) . . ?
O7 Pb2 N5 138.67(10) . . ?
O4 Pb2 O6 122.52(10) . . ?
N6 Pb2 O6 72.84(11) . . ?
O1 Pb2 O6 101.16(10) . . ?
O5 Pb2 O6 155.78(10) . . ?
O7 Pb2 O6 49.15(10) . . ?
N5 Pb2 O6 96.01(11) . . ?
C8 O1 Pb1 116.6(2) . . ?
C8 O1 Pb2 122.2(2) . . ?
Pb1 O1 Pb2 118.97(11) . . ?
C1 N1 C5 118.6(3) . . ?
C1 N1 Pb1 122.5(3) . . ?
C5 N1 Pb1 118.9(2) . . ?
C6 N2 N3 117.3(3) . . ?
C6 N2 Pb1 122.7(3) . . ?
N3 N2 Pb1 119.9(2) . . ?
C8 N3 N2 110.6(3) . . ?
N5 N4 C8 117.4(3) . . ?
N5 N4 H4N 121.3 . . ?
C8 N4 H4N 121.3 . . ?
C9 N5 N4 120.7(4) . . ?
C9 N5 Pb2 120.0(3) . . ?
N4 N5 Pb2 116.3(2) . . ?
C15 N6 C11 119.3(4) . . ?
C15 N6 Pb2 118.4(3) . . ?
C11 N6 Pb2 122.3(3) . . ?
N1 C1 C2 123.0(4) . . ?
N1 C1 H1 118.5 . . ?
C2 C1 H1 118.5 . . ?
C3 C2 C1 119.1(4) . . ?
C3 C2 H2 120.5 . . ?
C1 C2 H2 120.5 . . ?
C2 C3 C4 118.7(4) . . ?
C2 C3 H3 120.7 . . ?
C4 C3 H3 120.7 . . ?
C3 C4 C5 119.2(4) . . ?
C3 C4 H4 120.4 . . ?
C5 C4 H4 120.4 . . ?
N1 C5 C4 121.4(4) . . ?
N1 C5 C6 117.0(3) . . ?
C4 C5 C6 121.6(4) . . ?
N2 C6 C5 116.9(4) . . ?
N2 C6 C7 123.8(4) . . ?
C5 C6 C7 119.3(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 . . ?
O1 C8 N3 127.8(3) . . ?
O1 C8 N4 118.9(3) . . ?
N3 C8 N4 113.3(3) . . ?
N5 C9 C11 114.9(4) . . ?
N5 C9 C10 125.7(4) . . ?
C11 C9 C10 119.4(3) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N6 C11 C12 120.7(4) . . ?
N6 C11 C9 118.7(3) . . ?
C12 C11 C9 120.6(4) . . ?
C13 C12 C11 119.8(4) . . ?
C13 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
C14 C13 C12 118.9(4) . . ?
C14 C13 H13 120.5 . . ?
C12 C13 H13 120.5 . . ?
C13 C14 C15 118.6(4) . . ?
C13 C14 H14 120.7 . . ?
C15 C14 H14 120.7 . . ?
N6 C15 C14 122.7(4) . . ?
N6 C15 H15 118.6 . . ?
C14 C15 H15 118.6 . . ?
C16 O2 Pb1 109.3(3) . . ?
C18 O4 Pb2 94.8(3) . . ?
C18 O5 Pb2 92.3(3) . . ?
C20 O6 Pb2 92.3(3) . . ?
C20 O7 Pb2 95.7(3) . . ?
O3 C16 O2 123.9(4) . . ?
O3 C16 C17 121.2(4) . . ?
O2 C16 C17 114.9(4) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O5 C18 O4 122.1(5) . . ?
O5 C18 C19 120.1(4) . . ?
O4 C18 C19 117.9(4) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O6 C20 O7 122.8(4) . . ?
O6 C20 C21 119.1(4) . . ?
O7 C20 C21 118.0(4) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 N2 N3 C8 -172.0(4) . . . . ?
Pb1 N2 N3 C8 10.6(4) . . . . ?
C8 N4 N5 C9 178.1(4) . . . . ?
C8 N4 N5 Pb2 17.8(4) . . . . ?
C5 N1 C1 C2 1.6(7) . . . . ?
Pb1 N1 C1 C2 -178.5(3) . . . . ?
N1 C1 C2 C3 0.9(7) . . . . ?
C1 C2 C3 C4 -2.3(7) . . . . ?
C2 C3 C4 C5 1.3(7) . . . . ?
C1 N1 C5 C4 -2.6(6) . . . . ?
Pb1 N1 C5 C4 177.6(3) . . . . ?
C1 N1 C5 C6 178.8(4) . . . . ?
Pb1 N1 C5 C6 -1.1(5) . . . . ?
C3 C4 C5 N1 1.1(7) . . . . ?
C3 C4 C5 C6 179.7(4) . . . . ?
N3 N2 C6 C5 179.6(3) . . . . ?
Pb1 N2 C6 C5 -3.0(5) . . . . ?
N3 N2 C6 C7 0.1(6) . . . . ?
Pb1 N2 C6 C7 177.4(3) . . . . ?
N1 C5 C6 N2 2.6(6) . . . . ?
C4 C5 C6 N2 -176.0(4) . . . . ?
N1 C5 C6 C7 -177.8(4) . . . . ?
C4 C5 C6 C7 3.6(6) . . . . ?
Pb1 O1 C8 N3 -5.4(6) . . . . ?
Pb2 O1 C8 N3 157.2(3) . . . . ?
Pb1 O1 C8 N4 175.3(3) . . . . ?
Pb2 O1 C8 N4 -22.1(5) . . . . ?
N2 N3 C8 O1 -3.4(6) . . . . ?
N2 N3 C8 N4 175.9(3) . . . . ?
N5 N4 C8 O1 1.5(6) . . . . ?
N5 N4 C8 N3 -177.9(3) . . . . ?
N4 N5 C9 C11 179.6(3) . . . . ?
Pb2 N5 C9 C11 -20.9(5) . . . . ?
N4 N5 C9 C10 -0.1(7) . . . . ?
Pb2 N5 C9 C10 159.4(3) . . . . ?
C15 N6 C11 C12 0.8(6) . . . . ?
Pb2 N6 C11 C12 177.7(3) . . . . ?
C15 N6 C11 C9 -178.6(4) . . . . ?
Pb2 N6 C11 C9 -1.7(5) . . . . ?
N5 C9 C11 N6 15.2(6) . . . . ?
C10 C9 C11 N6 -165.1(4) . . . . ?
N5 C9 C11 C12 -164.2(4) . . . . ?
C10 C9 C11 C12 15.5(6) . . . . ?
N6 C11 C12 C13 -1.8(7) . . . . ?
C9 C11 C12 C13 177.6(4) . . . . ?
C11 C12 C13 C14 1.2(8) . . . . ?
C12 C13 C14 C15 0.3(8) . . . . ?
C11 N6 C15 C14 0.8(7) . . . . ?
Pb2 N6 C15 C14 -176.2(4) . . . . ?
C13 C14 C15 N6 -1.4(7) . . . . ?
Pb1 O2 C16 O3 9.6(5) . . . . ?
Pb1 O2 C16 C17 -170.3(3) . . . . ?
Pb2 O5 C18 O4 -5.3(4) . . . . ?
Pb2 O5 C18 C19 173.9(4) . . . . ?
Pb2 O4 C18 O5 5.4(4) . . . . ?
Pb2 O4 C18 C19 -173.8(4) . . . . ?
Pb2 O6 C20 O7 1.7(4) . . . . ?
Pb2 O6 C20 C21 -179.3(4) . . . . ?
Pb2 O7 C20 O6 -1.8(4) . . . . ?
Pb2 O7 C20 C21 179.2(3) . . . . ?

_refine_diff_density_max         2.409
_refine_diff_density_min         -1.930
_refine_diff_density_rms         0.288

####################################################################### 
# 
# 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 1574898'
_audit_update_record             
;
2017-09-17 deposited with the CCDC.
2018-02-22 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         'C15 H16 N10 O13 Pb2'
_chemical_formula_sum            'C15 H16 N10 O13 Pb2'
_chemical_formula_weight         958.76

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

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

_cell_length_a                   25.620(3)
_cell_length_b                   8.762(2)
_cell_length_c                   11.862(4)
_cell_angle_alpha                90
_cell_angle_beta                 111.828(17)
_cell_angle_gamma                90
_cell_volume                     2471.9(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    294(2)
_cell_measurement_reflns_used    25
_cell_measurement_theta_min      3.25
_cell_measurement_theta_max      22.57

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.576
_exptl_crystal_F_000             1776
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.18
_exptl_absorpt_coefficient_mu    13.690
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_correction_T_min  0.0932
_exptl_absorpt_correction_T_max  0.1919

_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      294(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega scans'
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_standards_number         1
_diffrn_standards_interval_time  60
_diffrn_standards_decay_%        0
_diffrn_reflns_number            2285
_diffrn_reflns_av_unetI/netI     0.0444
_diffrn_reflns_av_R_equivalents  0.0509
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_theta_min         1.712
_diffrn_reflns_theta_max         24.974
_diffrn_reflns_theta_full        24.974
_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 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2165
_reflns_number_gt                1760
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond v.3.2f (Crystal Impact GbR, 2008)'
_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)+(0.1042P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00189(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2165
_refine_ls_number_parameters     184
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0547
_refine_ls_wR_factor_ref         0.1451
_refine_ls_wR_factor_gt          0.1350
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.062
_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 0.42835(2) 0.13753(5) 0.56759(4) 0.0278(3) Uani 1 1 d . . . . .
O1 O 0.5000 0.2890(16) 0.7500 0.048(4) Uani 1 2 d S T P . .
N1 N 0.3567(4) 0.2614(12) 0.3871(9) 0.028(2) Uani 1 1 d . . . . .
N2 N 0.4289(4) 0.4298(13) 0.5595(10) 0.034(3) Uani 1 1 d . . . . .
N3 N 0.4651(5) 0.5120(12) 0.6584(10) 0.038(3) Uani 1 1 d . . . . .
H3N H 0.4648 0.6101 0.6600 0.046 Uiso 1 1 calc R U . . .
C1 C 0.3211(6) 0.1735(15) 0.2985(12) 0.031(3) Uani 1 1 d . . . . .
H1 H 0.3208 0.0690 0.3118 0.038 Uiso 1 1 calc R U . . .
C2 C 0.2856(6) 0.2307(19) 0.1907(12) 0.040(4) Uani 1 1 d . . . . .
H2 H 0.2617 0.1662 0.1316 0.048 Uiso 1 1 calc R U . . .
C3 C 0.2855(7) 0.3837(17) 0.1704(13) 0.044(4) Uani 1 1 d . . . . .
H3 H 0.2616 0.4243 0.0968 0.052 Uiso 1 1 calc R U . . .
C4 C 0.3203(6) 0.4772(17) 0.2576(13) 0.041(3) Uani 1 1 d . . . . .
H4 H 0.3203 0.5821 0.2458 0.049 Uiso 1 1 calc R U . . .
C5 C 0.3567(5) 0.4092(15) 0.3671(12) 0.030(3) Uani 1 1 d . . . . .
C6 C 0.3955(5) 0.5058(16) 0.4681(12) 0.032(3) Uani 1 1 d . . . . .
C7 C 0.5000 0.431(2) 0.7500 0.031(4) Uani 1 2 d S T P . .
C8 C 0.3929(7) 0.6760(17) 0.4571(15) 0.058(5) Uani 1 1 d . . . . .
H8A H 0.3672 0.7152 0.4918 0.086 Uiso 1 1 calc R U . . .
H8B H 0.3803 0.7041 0.3730 0.086 Uiso 1 1 calc R U . . .
H8C H 0.4297 0.7179 0.4996 0.086 Uiso 1 1 calc R U . . .
N4 N 0.3209(6) 0.1280(13) 0.6044(13) 0.045(3) Uani 1 1 d . . . . .
O2 O 0.3597(5) 0.2278(12) 0.6488(10) 0.051(3) Uani 1 1 d . . . . .
O3 O 0.3285(4) 0.0244(11) 0.5426(10) 0.043(2) Uani 1 1 d . . . . .
O4 O 0.2772(6) 0.1365(14) 0.6271(18) 0.091(5) Uani 1 1 d . . . . .
N5 N 0.4511(5) 0.1264(12) 0.3154(12) 0.037(3) Uani 1 1 d . . . . .
O5 O 0.4709(4) 0.2262(11) 0.3959(9) 0.045(3) Uani 1 1 d . . . . .
O6 O 0.4394(5) 0.1613(13) 0.2082(10) 0.056(3) Uani 1 1 d . . . . .
O7 O 0.4434(5) -0.0027(12) 0.3425(12) 0.066(4) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb O2 2.430(11) . ?
Pb N1 2.492(10) . ?
Pb N2 2.563(11) . ?
Pb O1 2.619(7) . ?
Pb O3 2.655(10) . ?
Pb O5 2.756(10) . ?
O1 C7 1.24(3) . ?
O1 Pb 2.619(7) 2_656 ?
N1 C5 1.316(17) . ?
N1 C1 1.348(16) . ?
N2 C6 1.289(15) . ?
N2 N3 1.395(14) . ?
N3 C7 1.329(14) . ?
N3 H3N 0.8600 . ?
C1 C2 1.360(19) . ?
C1 H1 0.9300 . ?
C2 C3 1.36(2) . ?
C2 H2 0.9300 . ?
C3 C4 1.36(2) . ?
C3 H3 0.9300 . ?
C4 C5 1.418(18) . ?
C4 H4 0.9300 . ?
C5 C6 1.501(18) . ?
C6 C8 1.497(19) . ?
C7 N3 1.329(14) 2_656 ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
N4 O3 1.227(15) . ?
N4 O4 1.247(17) . ?
N4 O2 1.282(16) . ?
N5 O7 1.212(14) . ?
N5 O6 1.231(17) . ?
N5 O5 1.254(14) . ?

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
O2 Pb N1 77.8(4) . . ?
O2 Pb N2 72.8(4) . . ?
N1 Pb N2 62.9(3) . . ?
O2 Pb O1 84.0(3) . . ?
N1 Pb O1 123.7(4) . . ?
N2 Pb O1 60.8(3) . . ?
O2 Pb O3 50.0(3) . . ?
N1 Pb O3 72.3(3) . . ?
N2 Pb O3 112.8(3) . . ?
O1 Pb O3 129.2(2) . . ?
O2 Pb O5 138.1(4) . . ?
N1 Pb O5 67.0(3) . . ?
N2 Pb O5 71.4(3) . . ?
O1 Pb O5 96.8(2) . . ?
O3 Pb O5 130.7(3) . . ?
C7 O1 Pb 120.4(3) . . ?
C7 O1 Pb 120.4(3) . 2_656 ?
Pb O1 Pb 119.1(5) . 2_656 ?
C5 N1 C1 117.9(11) . . ?
C5 N1 Pb 122.3(8) . . ?
C1 N1 Pb 119.3(8) . . ?
C6 N2 N3 117.8(11) . . ?
C6 N2 Pb 122.4(9) . . ?
N3 N2 Pb 119.7(7) . . ?
C7 N3 N2 116.5(11) . . ?
C7 N3 H3N 121.8 . . ?
N2 N3 H3N 121.8 . . ?
N1 C1 C2 123.0(13) . . ?
N1 C1 H1 118.5 . . ?
C2 C1 H1 118.5 . . ?
C1 C2 C3 119.0(13) . . ?
C1 C2 H2 120.5 . . ?
C3 C2 H2 120.5 . . ?
C4 C3 C2 120.0(14) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C3 C4 C5 117.7(13) . . ?
C3 C4 H4 121.1 . . ?
C5 C4 H4 121.1 . . ?
N1 C5 C4 122.3(12) . . ?
N1 C5 C6 117.1(11) . . ?
C4 C5 C6 120.6(12) . . ?
N2 C6 C8 125.6(12) . . ?
N2 C6 C5 114.6(12) . . ?
C8 C6 C5 119.9(11) . . ?
O1 C7 N3 122.4(8) . 2_656 ?
O1 C7 N3 122.4(8) . . ?
N3 C7 N3 115.1(17) 2_656 . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O3 N4 O4 121.9(14) . . ?
O3 N4 O2 118.5(12) . . ?
O4 N4 O2 119.5(15) . . ?
N4 O2 Pb 100.4(8) . . ?
N4 O3 Pb 91.1(8) . . ?
O7 N5 O6 120.3(12) . . ?
O7 N5 O5 120.6(13) . . ?
O6 N5 O5 119.1(12) . . ?
N5 O5 Pb 101.9(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
C6 N2 N3 C7 -178.4(12) . . . . ?
Pb N2 N3 C7 3.8(15) . . . . ?
C5 N1 C1 C2 0.0(19) . . . . ?
Pb N1 C1 C2 -171.6(10) . . . . ?
N1 C1 C2 C3 0(2) . . . . ?
C1 C2 C3 C4 0(2) . . . . ?
C2 C3 C4 C5 1(2) . . . . ?
C1 N1 C5 C4 1.0(19) . . . . ?
Pb N1 C5 C4 172.3(10) . . . . ?
C1 N1 C5 C6 178.3(12) . . . . ?
Pb N1 C5 C6 -10.4(15) . . . . ?
C3 C4 C5 N1 -2(2) . . . . ?
C3 C4 C5 C6 -178.8(14) . . . . ?
N3 N2 C6 C8 2(2) . . . . ?
Pb N2 C6 C8 179.5(12) . . . . ?
N3 N2 C6 C5 -178.2(12) . . . . ?
Pb N2 C6 C5 -0.4(16) . . . . ?
N1 C5 C6 N2 6.8(18) . . . . ?
C4 C5 C6 N2 -175.8(13) . . . . ?
N1 C5 C6 C8 -173.0(13) . . . . ?
C4 C5 C6 C8 4(2) . . . . ?
Pb O1 C7 N3 178.8(7) . . . 2_656 ?
Pb O1 C7 N3 -1.2(7) 2_656 . . 2_656 ?
Pb O1 C7 N3 -1.2(7) . . . . ?
Pb O1 C7 N3 178.8(7) 2_656 . . . ?
N2 N3 C7 O1 -1.7(14) . . . . ?
N2 N3 C7 N3 178.3(14) . . . 2_656 ?
O3 N4 O2 Pb 1.4(13) . . . . ?
O4 N4 O2 Pb 179.9(12) . . . . ?
O4 N4 O3 Pb -179.7(14) . . . . ?
O2 N4 O3 Pb -1.3(12) . . . . ?
O7 N5 O5 Pb -32.4(14) . . . . ?
O6 N5 O5 Pb 147.5(10) . . . . ?

_refine_diff_density_max         2.617
_refine_diff_density_min         -2.456
_refine_diff_density_rms         0.348

