# Electronic Supplementary Material (ESI) for Dalton Transactions.
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#  experimental, refinement, atomic coordinates,
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#  as required by the journal to which it was submitted.
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data_5

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C37 H30 N22 O21 Pb5, 2(C3 H7 N1 O1), C1 H4 O'
_chemical_formula_sum            'C44 H48 N24 O24 Pb5'
_chemical_formula_weight         2333.01

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           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

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

_cell_length_a                   28.1919(17)
_cell_length_b                   19.7200(10)
_cell_length_c                   11.8904(8)
_cell_angle_alpha                90
_cell_angle_beta                 111.140(2)
_cell_angle_gamma                90
_cell_volume                     6165.5(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9486
_cell_measurement_theta_min      2.46
_cell_measurement_theta_max      25.34

_exptl_crystal_description       Block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.513
_exptl_crystal_F_000             4328
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.160
_exptl_absorpt_coefficient_mu    13.708
_shelx_estimated_absorpt_T_min   0.114
_shelx_estimated_absorpt_T_max   0.218
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.04
_exptl_absorpt_correction_T_max  0.10
_exptl_absorpt_process_details   SADABS
_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_measurement_device_type  'Bruker APEX-II PHOTON 100 detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            46755
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.463
_diffrn_reflns_theta_max         25.408
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             5832
_reflns_number_gt                4847
_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    'SIR97 (Giacovazzo et al, 1997)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_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)+(0.0902P)²+293.6295P] 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         5832
_refine_ls_number_parameters     412
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0626
_refine_ls_wR_factor_ref         0.1793
_refine_ls_wR_factor_gt          0.1732
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.448 0.000 6 3 ' '
2 0.000 0.554 0.000 8 5 ' '
3 0.500 0.052 0.000 8 5 ' '
4 0.500 0.946 0.000 6 3 ' '
5 0.500 0.000 0.500 660 176 '4 DMF and 2 MeOH'
6 1.000 0.500 0.500 660 176 '4 DMF and 2 MeOH'
_platon_squeeze_details          
;These disordered dimethylformamide and 
 methanol molecules could not be modelled reliably, were 
 removed from the model but included in the empirical formulae.
 This justify the B-level alert in the checkcif report.The strategy
 improved the R1 factor by 8.20%. The electron count suggests the presence of 
 8 DMF and 4 methanol molecules per unit cell (electron count = 392), 
 2 DMF and one methanol molecules per asymmetric unit.
 Thermogravimetric and elemental analysis data support these results.
;

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 0.13608(2) 0.23519(3) 0.09129(5) 0.03445(18) Uani 1 1 d . . . . .
Pb3 Pb 0.20830(3) 0.0000 0.09361(10) 0.0548(3) Uani 1 2 d S T P . .
Pb2 Pb 0.06991(3) 0.0000 0.11283(10) 0.0555(3) Uani 1 2 d S T P . .
Pb4 Pb 0.37188(4) 0.0000 -0.14929(9) 0.0583(3) Uani 1 2 d S T P . .
N13 N 0.1024(8) 0.0000 -0.1224(17) 0.050(5) Uani 1 2 d S T P . .
O1 O 0.1450(3) 0.3532(5) 0.1674(9) 0.039(2) Uani 1 1 d . . . . .
N7 N 0.0492(4) 0.2629(5) 0.1439(12) 0.041(3) Uani 1 1 d . . . . .
O5 O 0.0861(4) 0.1374(5) 0.1420(10) 0.047(2) Uani 1 1 d . . . . .
O11 O 0.2304(6) 0.0000 -0.0985(19) 0.070(5) Uani 1 2 d S T P . .
O3 O 0.1982(3) 0.1407(5) 0.1364(10) 0.047(2) Uani 1 1 d . . . . .
N4 N 0.2352(4) 0.2672(5) 0.1421(10) 0.034(2) Uani 1 1 d . . . . .
N5 N 0.3366(4) 0.2903(6) 0.1765(14) 0.051(3) Uani 1 1 d . . . . .
O6 O 0.0169(4) 0.0907(5) 0.1519(13) 0.063(3) Uani 1 1 d . . . . .
N6 N 0.3509(4) 0.1771(6) 0.1686(13) 0.052(3) Uani 1 1 d . . . . .
H6A H 0.3816 0.1870 0.1764 0.078 Uiso 1 1 calc R U . . .
H6B H 0.3413 0.1354 0.1624 0.078 Uiso 1 1 calc R U . . .
C12 C 0.0222(5) 0.2119(7) 0.1584(11) 0.032(3) Uani 1 1 d . . . . .
O4 O 0.2734(4) 0.0968(5) 0.1607(13) 0.065(3) Uani 1 1 d . . . . .
N1 N 0.1657(5) 0.2434(6) 0.3102(11) 0.043(3) Uani 1 1 d . . . . .
C11 C 0.0440(5) 0.1423(7) 0.1507(12) 0.036(3) Uani 1 1 d . . . . .
O2 O 0.1660(6) 0.4215(6) 0.3244(12) 0.074(4) Uani 1 1 d . . . . .
O8 O 0.2260(7) 0.0000 0.397(3) 0.104(9) Uani 1 2 d S T P . .
C8 C 0.2535(5) 0.3299(8) 0.1518(14) 0.043(3) Uani 1 1 d . . . . .
H8 H 0.2325 0.3667 0.1489 0.052 Uiso 1 1 calc R U . . .
N9 N -0.0542(4) 0.1692(7) 0.1835(12) 0.049(3) Uani 1 1 d . . . . .
H9A H -0.0822 0.1775 0.1944 0.074 Uiso 1 1 calc R U . . .
H9B H -0.0446 0.1281 0.1812 0.074 Uiso 1 1 calc R U . . .
C21 C 0.2735(11) 0.0000 -0.087(3) 0.058(6) Uani 1 2 d S T P . .
H21 H 0.2967 0.0000 -0.0082 0.070 Uiso 1 2 calc R U P . .
N10 N 0.0906(9) 0.0000 0.3409(17) 0.055(5) Uani 1 2 d S T P . .
C9 C 0.3039(5) 0.3402(8) 0.1662(15) 0.047(4) Uani 1 1 d . . . . .
H9 H 0.3154 0.3846 0.1689 0.057 Uiso 1 1 calc R U . . .
C7 C 0.2666(5) 0.2152(6) 0.1501(11) 0.030(3) Uani 1 1 d . . . . .
O7 O 0.1582(7) 0.0000 0.224(2) 0.080(6) Uani 1 2 d S T P . .
C15 C -0.0255(5) 0.2208(7) 0.1701(12) 0.037(3) Uani 1 1 d . . . . .
N8 N -0.0425(5) 0.2841(7) 0.1746(16) 0.063(4) Uani 1 1 d . . . . .
O10 O 0.0701(8) 0.0000 -0.215(2) 0.098(8) Uani 1 2 d S T P . .
O9 O 0.1238(6) -0.0529(7) -0.0789(17) 0.096(5) Uani 1 1 d . . . . .
C6 C 0.2451(5) 0.1458(7) 0.1496(13) 0.037(3) Uani 1 1 d . . . . .
C10 C 0.3185(5) 0.2258(7) 0.1661(12) 0.035(3) Uani 1 1 d . . . . .
C2 C 0.1715(5) 0.3044(7) 0.3622(13) 0.041(3) Uani 1 1 d . . . . .
C13 C 0.0322(6) 0.3242(8) 0.148(2) 0.064(5) Uani 1 1 d . . . . .
H13 H 0.0512 0.3613 0.1404 0.076 Uiso 1 1 calc R U . . .
O12 O 0.2912(8) 0.0000 -0.165(2) 0.089(6) Uani 1 2 d S T P . .
C14 C -0.0143(6) 0.3348(8) 0.1637(19) 0.063(5) Uani 1 1 d . . . . .
H14 H -0.0254 0.3790 0.1665 0.076 Uiso 1 1 calc R U . . .
C1 C 0.1599(5) 0.3635(7) 0.2791(15) 0.043(3) Uani 1 1 d . . . . .
C20 C 0.1596(14) 0.0000 0.527(3) 0.082(10) Uani 1 2 d S T P . .
N2 N 0.1973(9) 0.2576(10) 0.5622(15) 0.096(7) Uani 1 1 d . . . . .
C3 C 0.1765(7) 0.1884(8) 0.3813(16) 0.059(4) Uani 1 1 d . . . . .
H3 H 0.1734 0.1455 0.3470 0.071 Uiso 1 1 calc R U . . .
C17 C 0.1440(10) 0.0000 0.400(3) 0.069(7) Uani 1 2 d S TU P . .
C18 C 0.0619(13) 0.0000 0.391(4) 0.100(12) Uani 1 2 d S T P . .
H18 H 0.0273 0.0000 0.3460 0.120 Uiso 1 2 calc R U P . .
C4 C 0.1920(8) 0.1950(11) 0.5020(17) 0.075(6) Uani 1 1 d . . . . .
H4 H 0.1997 0.1557 0.5485 0.090 Uiso 1 1 calc R U . . .
C19 C 0.0779(16) 0.0000 0.522(4) 0.132(18) Uani 1 2 d S T P . .
H19 H 0.0532 0.0000 0.5571 0.159 Uiso 1 2 calc R U P . .
C5 C 0.1882(9) 0.3105(11) 0.4887(19) 0.076(6) Uani 1 1 d . . . . .
C16 C 0.1757(10) 0.0000 0.343(2) 0.062(6) Uani 1 2 d S TU P . .
N3 N 0.1951(10) 0.3697(10) 0.5468(16) 0.112(8) Uani 1 1 d . . . . .
H3A H 0.2045 0.3705 0.6241 0.167 Uiso 1 1 calc R U . . .
H3B H 0.1902 0.4071 0.5070 0.167 Uiso 1 1 calc R U . . .
N11 N 0.1296(15) 0.0000 0.598(3) 0.135(14) Uani 1 2 d S T P . .
N12 N 0.2142(14) 0.0000 0.606(4) 0.142(14) Uani 1 2 d S T P . .
H12A H 0.2227 0.0000 0.6835 0.213 Uiso 1 2 calc R U P . .
H12B H 0.2373 0.0000 0.5750 0.213 Uiso 1 2 calc R U P . .
O13 O 0.3898(8) 0.0534(11) 0.080(2) 0.130(8) Uani 1 1 d . U . . .
C22 C 0.394(2) 0.0000 0.139(6) 0.141(19) Uani 1 2 d S TU P . .
H22 H 0.4010 0.0000 0.2217 0.169 Uiso 1 2 calc R U P . .


_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 N1 2.436(12) . ?
Pb1 O1 2.477(10) . ?
Pb1 O3 2.481(10) . ?
Pb1 O5 2.584(10) . ?
Pb1 N4 2.711(10) . ?
Pb1 N7 2.793(10) . ?
Pb3 O7 2.44(2) . ?
Pb3 O4 2.567(11) 6 ?
Pb3 O4 2.567(11) . ?
Pb3 O11 2.58(2) . ?
Pb3 O9 2.729(16) 6 ?
Pb3 O9 2.729(16) . ?
Pb2 O7 2.360(18) . ?
Pb2 O6 2.479(11) . ?
Pb2 O6 2.479(11) 6 ?
Pb2 N10 2.56(2) . ?
Pb2 O5 2.750(10) 6 ?
Pb2 O5 2.750(10) . ?
Pb4 O12 2.22(2) . ?
Pb4 O2 2.504(13) 4_545 ?
Pb4 O2 2.504(13) 7 ?
N13 O10 1.15(3) . ?
N13 O9 1.222(18) 6 ?
N13 O9 1.222(18) . ?
O1 C1 1.257(18) . ?
N7 C13 1.309(19) . ?
N7 C12 1.309(17) . ?
O5 C11 1.232(15) . ?
O11 C21 1.17(3) . ?
O3 C6 1.275(16) . ?
N4 C8 1.328(17) . ?
N4 C7 1.337(16) . ?
N5 C9 1.324(19) . ?
N5 C10 1.361(18) . ?
O6 C11 1.274(17) . ?
N6 C10 1.318(18) . ?
C12 C15 1.412(17) . ?
C12 C11 1.520(18) . ?
O4 C6 1.229(17) . ?
N1 C2 1.336(19) . ?
N1 C3 1.340(19) . ?
O2 C1 1.249(18) . ?
O2 Pb4 2.504(13) 7 ?
O8 C16 1.33(3) . ?
C8 C9 1.384(18) . ?
N9 C15 1.345(18) . ?
C21 O12 1.20(3) . ?
N10 C18 1.17(4) . ?
N10 C17 1.41(3) . ?
C7 C10 1.420(18) . ?
C7 C6 1.497(18) . ?
O7 C16 1.32(3) . ?
C15 N8 1.345(19) . ?
N8 C14 1.31(2) . ?
C2 C5 1.41(2) . ?
C2 C1 1.48(2) . ?
C13 C14 1.41(2) . ?
C20 N11 1.39(5) . ?
C20 C17 1.41(4) . ?
C20 N12 1.49(5) . ?
N2 C5 1.32(3) . ?
N2 C4 1.41(3) . ?
C3 C4 1.35(3) . ?
C17 C16 1.31(4) . ?
C18 C19 1.45(6) . ?
C19 N11 1.41(5) . ?
C5 N3 1.33(3) . ?
O13 C22 1.24(4) . ?
C22 O13 1.24(4) 6 ?

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 Pb1 O1 66.2(4) . . ?
N1 Pb1 O3 82.9(4) . . ?
O1 Pb1 O3 131.0(3) . . ?
N1 Pb1 O5 78.8(4) . . ?
O1 Pb1 O5 127.4(3) . . ?
O3 Pb1 O5 78.0(3) . . ?
N1 Pb1 N4 79.5(4) . . ?
O1 Pb1 N4 74.9(3) . . ?
O3 Pb1 N4 62.4(3) . . ?
O5 Pb1 N4 136.6(3) . . ?
N1 Pb1 N7 74.8(4) . . ?
O1 Pb1 N7 73.5(3) . . ?
O3 Pb1 N7 135.0(3) . . ?
O5 Pb1 N7 59.8(3) . . ?
N4 Pb1 N7 145.2(4) . . ?
O7 Pb3 O4 108.3(4) . 6 ?
O7 Pb3 O4 108.3(4) . . ?
O4 Pb3 O4 96.1(5) 6 . ?
O7 Pb3 O11 160.4(6) . . ?
O4 Pb3 O11 84.3(4) 6 . ?
O4 Pb3 O11 84.3(4) . . ?
O7 Pb3 O9 85.9(6) . 6 ?
O4 Pb3 O9 148.2(5) 6 6 ?
O4 Pb3 O9 106.3(4) . 6 ?
O11 Pb3 O9 76.0(5) . 6 ?
O7 Pb3 O9 85.9(6) . . ?
O4 Pb3 O9 106.3(4) 6 . ?
O4 Pb3 O9 148.2(5) . . ?
O11 Pb3 O9 76.0(5) . . ?
O9 Pb3 O9 45.0(6) 6 . ?
O7 Pb2 O6 118.7(4) . . ?
O7 Pb2 O6 118.7(4) . 6 ?
O6 Pb2 O6 92.4(5) . 6 ?
O7 Pb2 N10 67.5(8) . . ?
O6 Pb2 N10 74.0(5) . . ?
O6 Pb2 N10 74.0(5) 6 . ?
O7 Pb2 O5 80.5(2) . 6 ?
O6 Pb2 O5 140.5(3) . 6 ?
O6 Pb2 O5 49.4(3) 6 6 ?
N10 Pb2 O5 84.4(2) . 6 ?
O7 Pb2 O5 80.5(2) . . ?
O6 Pb2 O5 49.4(3) . . ?
O6 Pb2 O5 140.5(3) 6 . ?
N10 Pb2 O5 84.4(2) . . ?
O5 Pb2 O5 160.6(4) 6 . ?
O12 Pb4 O2 79.3(6) . 4_545 ?
O12 Pb4 O2 79.3(6) . 7 ?
O2 Pb4 O2 76.4(5) 4_545 7 ?
O10 N13 O9 120.3(12) . 6 ?
O10 N13 O9 120.3(12) . . ?
O9 N13 O9 117(2) 6 . ?
C1 O1 Pb1 119.2(9) . . ?
C13 N7 C12 117.9(11) . . ?
C13 N7 Pb1 123.5(9) . . ?
C12 N7 Pb1 118.5(8) . . ?
C11 O5 Pb1 125.8(9) . . ?
C11 O5 Pb2 88.0(8) . . ?
Pb1 O5 Pb2 141.8(4) . . ?
C21 O11 Pb3 118(2) . . ?
C6 O3 Pb1 125.9(8) . . ?
C8 N4 C7 118.7(11) . . ?
C8 N4 Pb1 125.0(8) . . ?
C7 N4 Pb1 116.1(8) . . ?
C9 N5 C10 117.3(11) . . ?
C11 O6 Pb2 99.8(8) . . ?
N7 C12 C15 122.4(12) . . ?
N7 C12 C11 114.8(11) . . ?
C15 C12 C11 122.6(12) . . ?
C6 O4 Pb3 100.8(8) . . ?
C2 N1 C3 118.4(13) . . ?
C2 N1 Pb1 119.4(9) . . ?
C3 N1 Pb1 122.2(11) . . ?
O5 C11 O6 122.6(13) . . ?
O5 C11 C12 119.8(12) . . ?
O6 C11 C12 117.6(11) . . ?
C1 O2 Pb4 104.9(10) . 7 ?
N4 C8 C9 119.8(13) . . ?
O11 C21 O12 128(3) . . ?
C18 N10 C17 123(3) . . ?
C18 N10 Pb2 128(2) . . ?
C17 N10 Pb2 109.0(18) . . ?
N5 C9 C8 123.6(14) . . ?
N4 C7 C10 121.4(12) . . ?
N4 C7 C6 116.3(11) . . ?
C10 C7 C6 122.1(11) . . ?
C16 O7 Pb2 120.6(18) . . ?
C16 O7 Pb3 127.0(16) . . ?
Pb2 O7 Pb3 112.4(9) . . ?
N9 C15 N8 117.3(12) . . ?
N9 C15 C12 123.5(13) . . ?
N8 C15 C12 119.1(13) . . ?
C14 N8 C15 117.8(12) . . ?
N13 O9 Pb3 98.9(11) . . ?
O4 C6 O3 123.6(12) . . ?
O4 C6 C7 118.1(11) . . ?
O3 C6 C7 118.2(12) . . ?
N6 C10 N5 116.3(12) . . ?
N6 C10 C7 124.6(12) . . ?
N5 C10 C7 119.0(12) . . ?
N1 C2 C5 120.5(14) . . ?
N1 C2 C1 116.0(13) . . ?
C5 C2 C1 123.5(15) . . ?
N7 C13 C14 120.9(14) . . ?
C21 O12 Pb4 130(2) . . ?
N8 C14 C13 121.7(14) . . ?
O2 C1 O1 122.9(14) . . ?
O2 C1 C2 118.0(14) . . ?
O1 C1 C2 119.1(13) . . ?
N11 C20 C17 129(3) . . ?
N11 C20 N12 110(3) . . ?
C17 C20 N12 122(4) . . ?
C5 N2 C4 113.3(17) . . ?
N1 C3 C4 120.5(17) . . ?
C16 C17 N10 123(3) . . ?
C16 C17 C20 124(3) . . ?
N10 C17 C20 114(3) . . ?
N10 C18 C19 123(3) . . ?
C3 C4 N2 124.0(17) . . ?
N11 C19 C18 122(3) . . ?
N2 C5 N3 112.9(19) . . ?
N2 C5 C2 123.2(19) . . ?
N3 C5 C2 123.9(19) . . ?
C17 C16 O7 120(3) . . ?
C17 C16 O8 124(3) . . ?
O7 C16 O8 116(3) . . ?
C19 N11 C20 109(3) . . ?
O13 C22 O13 116(6) . 6 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N12 H12B O8 0.86 2.03 2.63(6) 126.6 .
N12 H12A O12 0.86 2.12 2.80(4) 136.6 1_556
N12 H12A O11 0.86 2.52 3.37(5) 169.6 1_556
N3 H3B O2 0.86 2.05 2.67(2) 129.0 .
N3 H3A O4 0.86 2.49 3.33(2) 165.8 7_556
C19 H19 O10 0.93 2.57 3.21(5) 125.8 1_556
C18 H18 O10 0.93 2.62 3.55(4) 179.3 5
C14 H14 O13 0.93 2.60 3.35(2) 137.7 8_455
C13 H13 O1 0.93 2.55 3.156(17) 123.0 .
C9 H9 O9 0.93 2.63 3.35(2) 134.3 4
C9 H9 O11 0.93 2.60 3.310(17) 133.3 7
N9 H9B O6 0.86 2.03 2.666(16) 130.4 .
N9 H9A N5 0.86 2.31 3.150(15) 166.0 8_455
C8 H8 O1 0.93 2.57 3.164(16) 122.3 .
N6 H6B O13 0.86 2.53 3.01(2) 116.6 .
N6 H6B O4 0.86 2.05 2.673(16) 128.2 .
N6 H6A N8 0.86 2.22 3.077(16) 173.5 8

_refine_diff_density_max         7.152
_refine_diff_density_min         -2.589
_refine_diff_density_rms         0.317

_shelxl_version_number           2014/6

_database_code_depnum_ccdc_archive 'CCDC 1017108'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
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# 
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#  data retrieval see:
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#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_6

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H16 N12 O8 Pb2, 2(C3 H7 N1 O1), H2 O'
_chemical_formula_sum            'C28 H32 N14 O11 Pb2'
_chemical_formula_weight         1155.05

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                   7.8443(4)
_cell_length_b                   22.1845(13)
_cell_length_c                   21.7657(13)
_cell_angle_alpha                90
_cell_angle_beta                 90.842(2)
_cell_angle_gamma                90
_cell_volume                     3787.3(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9941
_cell_measurement_theta_min      2.62
_cell_measurement_theta_max      23.23

_exptl_crystal_description       Block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.026
_exptl_crystal_F_000             2200
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    8.953
_shelx_estimated_absorpt_T_min   0.156
_shelx_estimated_absorpt_T_max   0.347
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.11
_exptl_absorpt_correction_T_max  0.25
_exptl_absorpt_process_details   SADABS
_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_measurement_device_type  'Bruker APEX-II PHOTON 100 detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            43363
_diffrn_reflns_av_unetI/netI     0.0613
_diffrn_reflns_av_R_equivalents  0.0718
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.597
_diffrn_reflns_theta_max         25.358
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6930
_reflns_number_gt                4943
_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    'SIR97 (Giacovazzo et al, 1997)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_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)+(0.0650P)²+8.7097P] 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         6930
_refine_ls_number_parameters     397
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0526
_refine_ls_wR_factor_ref         0.1269
_refine_ls_wR_factor_gt          0.1172
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.036 0.201 -0.163 320 109 '2DMF and 1H2O'
2 -0.112 0.799 0.163 320 108 '2DMF and 1H2O'
3 0.042 0.299 0.337 320 110 '2DMF and 1H2O'
4 -0.114 0.701 0.663 320 107 '2DMF and 1H2O'
5 0.500 0.000 0.000 39 13 ' '
6 0.500 0.500 0.500 39 13 ' '
_platon_squeeze_details          
;These disordered dimethylformamide and water molecules could
 not be modelled reliably, were removed from the model but included
 in the empirical formulae. This justify the A-level alert
 in the checkcif report. The strategy improved the R1 factor by 13.84%.
 The electron count suggest the presence of 8 DMF and 4 water molecules
 per unit cell (electron count = 360), 2 DMF and 1 water molecules per
 asymmetric unit. Thermogravimetric and elemental analysis data support
 these results. 
;

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 0.50914(5) 0.70844(2) 0.32259(2) 0.03985(14) Uani 1 1 d . . . . .
Pb2 Pb -0.00377(5) 0.32371(2) 0.70492(2) 0.04063(14) Uani 1 1 d . . . . .
N10 N 0.7588(10) 0.9282(4) 0.4400(4) 0.037(2) Uani 1 1 d . . . . .
H10N H 0.8564 0.9107 0.4375 0.056 Uiso 1 1 calc R U . . .
N9 N 0.7519(10) 1.0328(4) 0.4102(4) 0.040(2) Uani 1 1 d . . . . .
H9N H 0.6579 1.0510 0.4013 0.061 Uiso 1 1 calc R U . . .
N8 N 1.0426(10) 1.0211(4) 0.3971(4) 0.043(2) Uani 1 1 d . . . . .
N7 N 1.0257(10) 1.0960(4) 0.2937(4) 0.044(2) Uani 1 1 d . . . . .
O5 O 0.7298(8) 1.1401(4) 0.2503(4) 0.057(2) Uani 1 1 d . . . . .
N1 N 0.5313(10) 0.6745(4) 0.4353(4) 0.046(2) Uani 1 1 d . . . . .
O1 O 0.2344(9) 0.6926(3) 0.3757(4) 0.049(2) Uani 1 1 d . . . . .
O2 O 0.0864(11) 0.6737(5) 0.4567(5) 0.085(3) Uani 1 1 d . . . . .
O8 O 0.9227(9) 0.8370(4) 0.3865(5) 0.073(3) Uani 1 1 d . . . . .
N11 N 0.4830(10) 0.8085(4) 0.3869(4) 0.042(2) Uani 1 1 d . . . . .
N12 N 0.4663(11) 0.9223(4) 0.4376(5) 0.050(3) Uani 1 1 d . . . . .
C18 C 0.6177(12) 0.8961(5) 0.4247(5) 0.036(2) Uani 1 1 d . . . . .
C17 C 0.7543(13) 0.9904(4) 0.4605(5) 0.038(2) Uani 1 1 d . . . . .
H17A H 0.6536 0.9965 0.4851 0.046 Uiso 1 1 calc R U . . .
H17B H 0.8534 0.9982 0.4865 0.046 Uiso 1 1 calc R U . . .
C16 C 0.8913(12) 1.0453(4) 0.3766(5) 0.036(2) Uani 1 1 d . . . . .
C13 C 0.8823(12) 1.0832(4) 0.3237(5) 0.035(2) Uani 1 1 d . . . . .
C12 C 0.7186(12) 1.1096(5) 0.2978(6) 0.044(3) Uani 1 1 d . . . . .
O6 O 0.5856(9) 1.0984(4) 0.3256(4) 0.072(3) Uani 1 1 d . . . . .
N5 N -0.0279(10) 0.4278(4) 0.6510(5) 0.048(2) Uani 1 1 d . . . . .
O3 O 0.2657(8) 0.3735(3) 0.6776(4) 0.049(2) Uani 1 1 d . . . . .
O4 O 0.4156(10) 0.4524(4) 0.6482(6) 0.094(4) Uani 1 1 d . . . . .
O7 O 0.7782(8) 0.7567(3) 0.3543(3) 0.0435(19) Uani 1 1 d . . . . .
C22 C 0.7879(13) 0.8086(5) 0.3780(5) 0.039(3) Uani 1 1 d . . . . .
C21 C 0.6253(12) 0.8384(4) 0.3980(5) 0.031(2) Uani 1 1 d . . . . .
C20 C 0.3318(14) 0.8337(5) 0.4018(6) 0.059(4) Uani 1 1 d . . . . .
H20 H 0.2308 0.8123 0.3960 0.071 Uiso 1 1 calc R U . . .
C19 C 0.3289(13) 0.8899(5) 0.4251(6) 0.055(3) Uani 1 1 d . . . . .
H19 H 0.2232 0.9071 0.4329 0.066 Uiso 1 1 calc R U . . .
C15 C 1.1760(14) 1.0356(5) 0.3653(5) 0.051(3) Uani 1 1 d . . . . .
H15 H 1.2806 1.0198 0.3779 0.061 Uiso 1 1 calc R U . . .
C14 C 1.1738(13) 1.0722(5) 0.3149(5) 0.049(3) Uani 1 1 d . . . . .
H14 H 1.2751 1.0809 0.2950 0.059 Uiso 1 1 calc R U . . .
C3 C 0.6797(14) 0.6648(6) 0.4641(6) 0.058(3) Uani 1 1 d . . . . .
H3 H 0.7822 0.6732 0.4449 0.070 Uiso 1 1 calc R U . . .
C4 C 0.6772(17) 0.6418(7) 0.5237(7) 0.084(5) Uani 1 1 d . . . . .
H4 H 0.7806 0.6300 0.5414 0.101 Uiso 1 1 calc R U . . .
N2 N 0.5379(14) 0.6356(7) 0.5569(6) 0.089(4) Uani 1 1 d . . . . .
C5 C 0.3944(16) 0.6483(7) 0.5281(6) 0.067(4) Uani 1 1 d . . . . .
N3 N 0.2469(15) 0.6429(6) 0.5587(6) 0.091(5) Uani 1 1 d . . . . .
H3N H 0.1530 0.6525 0.5403 0.110 Uiso 1 1 calc R U . . .
C6 C 0.241(2) 0.6221(8) 0.6193(9) 0.107(6) Uani 1 1 d . . . . .
H6A H 0.1367 0.6365 0.6376 0.129 Uiso 1 1 calc R U . . .
H6B H 0.3357 0.6399 0.6422 0.129 Uiso 1 1 calc R U . . .
N4 N 0.2495(17) 0.5547(6) 0.6266(7) 0.100(5) Uani 1 1 d . . . . .
H4N H 0.3476 0.5376 0.6305 0.120 Uiso 1 1 calc R U . . .
C7 C 0.1072(17) 0.5200(6) 0.6273(7) 0.071(4) Uani 1 1 d . . . . .
C10 C 0.1134(15) 0.4582(6) 0.6442(6) 0.063(4) Uani 1 1 d . . . . .
C11 C 0.2766(14) 0.4265(5) 0.6550(6) 0.056(3) Uani 1 1 d . . . . .
C9 C -0.1760(14) 0.4541(5) 0.6369(7) 0.062(4) Uani 1 1 d . . . . .
H9 H -0.2770 0.4329 0.6421 0.075 Uiso 1 1 calc R U . . .
C8 C -0.1820(18) 0.5124(7) 0.6146(8) 0.090(5) Uani 1 1 d . . . . .
H8 H -0.2868 0.5286 0.6028 0.107 Uiso 1 1 calc R U . . .
N6 N -0.0396(14) 0.5468(6) 0.6093(7) 0.104(5) Uani 1 1 d . . . . .
C2 C 0.3843(14) 0.6681(6) 0.4672(6) 0.057(3) Uani 1 1 d . . . . .
C1 C 0.2230(14) 0.6790(5) 0.4323(6) 0.045(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
Pb1 O7 2.456(6) . ?
Pb1 O1 2.485(8) . ?
Pb1 O3 2.534(7) 3_666 ?
Pb1 N1 2.570(9) . ?
Pb1 N11 2.634(8) . ?
Pb2 O5 2.459(7) 4_476 ?
Pb2 O3 2.465(7) . ?
Pb2 O1 2.528(7) 3_566 ?
Pb2 N5 2.595(9) . ?
Pb2 N7 2.635(9) 4_476 ?
N10 C18 1.353(12) . ?
N10 C17 1.451(12) . ?
N10 H10N 0.8600 . ?
N9 C16 1.354(12) . ?
N9 C17 1.444(13) . ?
N9 H9N 0.8600 . ?
N8 C15 1.303(13) . ?
N8 C16 1.372(12) . ?
N7 C13 1.340(12) . ?
N7 C14 1.351(13) . ?
N7 Pb2 2.635(9) 4_675 ?
O5 C12 1.240(12) . ?
O5 Pb2 2.459(7) 4_675 ?
N1 C3 1.331(14) . ?
N1 C2 1.362(14) . ?
O1 C1 1.273(13) . ?
O1 Pb2 2.528(7) 3_566 ?
O2 C1 1.209(13) . ?
O8 C22 1.243(12) . ?
N11 C21 1.318(12) . ?
N11 C20 1.355(13) . ?
N12 C19 1.320(13) . ?
N12 C18 1.356(12) . ?
C18 C21 1.407(13) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C16 C13 1.427(14) . ?
C13 C12 1.512(13) . ?
C12 O6 1.239(12) . ?
N5 C10 1.309(14) . ?
N5 C9 1.332(13) . ?
O3 C11 1.278(13) . ?
O3 Pb1 2.534(7) 3_666 ?
O4 C11 1.243(13) . ?
O7 C22 1.264(12) . ?
C22 C21 1.507(13) . ?
C20 C19 1.348(15) . ?
C20 H20 0.9300 . ?
C19 H19 0.9300 . ?
C15 C14 1.366(15) . ?
C15 H15 0.9300 . ?
C14 H14 0.9300 . ?
C3 C4 1.395(18) . ?
C3 H3 0.9300 . ?
C4 N2 1.326(17) . ?
C4 H4 0.9300 . ?
N2 C5 1.310(15) . ?
C5 N3 1.349(15) . ?
C5 C2 1.399(17) . ?
N3 C6 1.399(19) . ?
N3 H3N 0.8600 . ?
C6 N4 1.51(2) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
N4 C7 1.356(17) . ?
N4 H4N 0.8600 . ?
C7 N6 1.349(16) . ?
C7 C10 1.420(17) . ?
C10 C11 1.476(15) . ?
C9 C8 1.383(18) . ?
C9 H9 0.9300 . ?
C8 N6 1.359(18) . ?
C8 H8 0.9300 . ?
C2 C1 1.485(15) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O7 Pb1 O1 132.7(2) . . ?
O7 Pb1 O3 73.5(2) . 3_666 ?
O1 Pb1 O3 120.6(3) . 3_666 ?
O7 Pb1 N1 79.3(3) . . ?
O1 Pb1 N1 64.0(3) . . ?
O3 Pb1 N1 75.8(3) 3_666 . ?
O7 Pb1 N11 63.7(2) . . ?
O1 Pb1 N11 78.3(3) . . ?
O3 Pb1 N11 131.7(2) 3_666 . ?
N1 Pb1 N11 75.2(3) . . ?
O5 Pb2 O3 133.4(3) 4_476 . ?
O5 Pb2 O1 73.8(3) 4_476 3_566 ?
O3 Pb2 O1 120.3(3) . 3_566 ?
O5 Pb2 N5 80.5(3) 4_476 . ?
O3 Pb2 N5 63.2(3) . . ?
O1 Pb2 N5 76.5(3) 3_566 . ?
O5 Pb2 N7 63.3(2) 4_476 4_476 ?
O3 Pb2 N7 78.9(2) . 4_476 ?
O1 Pb2 N7 131.3(2) 3_566 4_476 ?
N5 Pb2 N7 74.6(3) . 4_476 ?
C18 N10 C17 123.5(8) . . ?
C18 N10 H10N 118.2 . . ?
C17 N10 H10N 118.2 . . ?
C16 N9 C17 122.8(9) . . ?
C16 N9 H9N 118.6 . . ?
C17 N9 H9N 118.6 . . ?
C15 N8 C16 115.3(9) . . ?
C13 N7 C14 118.3(9) . . ?
C13 N7 Pb2 115.8(6) . 4_675 ?
C14 N7 Pb2 125.5(7) . 4_675 ?
C12 O5 Pb2 125.8(6) . 4_675 ?
C3 N1 C2 119.0(10) . . ?
C3 N1 Pb1 122.8(8) . . ?
C2 N1 Pb1 118.1(7) . . ?
C1 O1 Pb1 123.9(6) . . ?
C1 O1 Pb2 125.3(7) . 3_566 ?
Pb1 O1 Pb2 108.3(3) . 3_566 ?
C21 N11 C20 119.4(9) . . ?
C21 N11 Pb1 116.7(6) . . ?
C20 N11 Pb1 123.4(7) . . ?
C19 N12 C18 116.0(9) . . ?
N10 C18 N12 116.0(9) . . ?
N10 C18 C21 122.7(9) . . ?
N12 C18 C21 121.2(9) . . ?
N9 C17 N10 112.8(9) . . ?
N9 C17 H17A 109.0 . . ?
N10 C17 H17A 109.0 . . ?
N9 C17 H17B 109.0 . . ?
N10 C17 H17B 109.0 . . ?
H17A C17 H17B 107.8 . . ?
N9 C16 N8 116.4(9) . . ?
N9 C16 C13 121.8(9) . . ?
N8 C16 C13 121.8(9) . . ?
N7 C13 C16 119.1(9) . . ?
N7 C13 C12 116.8(9) . . ?
C16 C13 C12 124.1(9) . . ?
O6 C12 O5 126.0(9) . . ?
O6 C12 C13 117.2(10) . . ?
O5 C12 C13 116.8(9) . . ?
C10 N5 C9 119.0(10) . . ?
C10 N5 Pb2 117.0(7) . . ?
C9 N5 Pb2 123.5(7) . . ?
C11 O3 Pb2 124.6(6) . . ?
C11 O3 Pb1 127.5(7) . 3_666 ?
Pb2 O3 Pb1 106.2(3) . 3_666 ?
C22 O7 Pb1 123.9(6) . . ?
O8 C22 O7 124.7(10) . . ?
O8 C22 C21 117.1(9) . . ?
O7 C22 C21 118.2(8) . . ?
N11 C21 C18 119.5(9) . . ?
N11 C21 C22 116.3(8) . . ?
C18 C21 C22 124.1(9) . . ?
C19 C20 N11 119.4(10) . . ?
C19 C20 H20 120.3 . . ?
N11 C20 H20 120.3 . . ?
N12 C19 C20 124.3(10) . . ?
N12 C19 H19 117.8 . . ?
C20 C19 H19 117.8 . . ?
N8 C15 C14 125.0(10) . . ?
N8 C15 H15 117.5 . . ?
C14 C15 H15 117.5 . . ?
N7 C14 C15 120.5(9) . . ?
N7 C14 H14 119.7 . . ?
C15 C14 H14 119.7 . . ?
N1 C3 C4 118.2(11) . . ?
N1 C3 H3 120.9 . . ?
C4 C3 H3 120.9 . . ?
N2 C4 C3 124.6(11) . . ?
N2 C4 H4 117.7 . . ?
C3 C4 H4 117.7 . . ?
C5 N2 C4 115.2(11) . . ?
N2 C5 N3 118.9(12) . . ?
N2 C5 C2 123.8(11) . . ?
N3 C5 C2 117.3(12) . . ?
C5 N3 C6 122.2(13) . . ?
C5 N3 H3N 118.9 . . ?
C6 N3 H3N 118.9 . . ?
N3 C6 N4 115.1(16) . . ?
N3 C6 H6A 108.5 . . ?
N4 C6 H6A 108.5 . . ?
N3 C6 H6B 108.5 . . ?
N4 C6 H6B 108.5 . . ?
H6A C6 H6B 107.5 . . ?
C7 N4 C6 122.0(13) . . ?
C7 N4 H4N 119.0 . . ?
C6 N4 H4N 119.0 . . ?
N6 C7 N4 116.5(13) . . ?
N6 C7 C10 121.8(12) . . ?
N4 C7 C10 121.7(13) . . ?
N5 C10 C7 120.1(11) . . ?
N5 C10 C11 118.0(11) . . ?
C7 C10 C11 121.9(11) . . ?
O4 C11 O3 122.3(11) . . ?
O4 C11 C10 121.4(11) . . ?
O3 C11 C10 115.9(10) . . ?
N5 C9 C8 121.1(12) . . ?
N5 C9 H9 119.5 . . ?
C8 C9 H9 119.5 . . ?
N6 C8 C9 122.1(12) . . ?
N6 C8 H8 118.9 . . ?
C9 C8 H8 118.9 . . ?
C7 N6 C8 115.2(12) . . ?
N1 C2 C5 118.6(10) . . ?
N1 C2 C1 116.4(11) . . ?
C5 C2 C1 124.9(11) . . ?
O2 C1 O1 121.5(10) . . ?
O2 C1 C2 120.9(12) . . ?
O1 C1 C2 117.5(10) . . ?

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
C17 N10 C18 N12 -9.0(15) . . . . ?
C17 N10 C18 C21 172.1(9) . . . . ?
C19 N12 C18 N10 -177.1(11) . . . . ?
C19 N12 C18 C21 1.8(16) . . . . ?
C16 N9 C17 N10 -74.6(12) . . . . ?
C18 N10 C17 N9 -85.6(12) . . . . ?
C17 N9 C16 N8 -7.8(14) . . . . ?
C17 N9 C16 C13 174.2(9) . . . . ?
C15 N8 C16 N9 -177.5(10) . . . . ?
C15 N8 C16 C13 0.5(15) . . . . ?
C14 N7 C13 C16 0.1(15) . . . . ?
Pb2 N7 C13 C16 -173.2(7) 4_675 . . . ?
C14 N7 C13 C12 -178.8(10) . . . . ?
Pb2 N7 C13 C12 8.0(12) 4_675 . . . ?
N9 C16 C13 N7 177.2(9) . . . . ?
N8 C16 C13 N7 -0.7(15) . . . . ?
N9 C16 C13 C12 -4.0(16) . . . . ?
N8 C16 C13 C12 178.1(10) . . . . ?
Pb2 O5 C12 O6 169.2(10) 4_675 . . . ?
Pb2 O5 C12 C13 -11.5(15) 4_675 . . . ?
N7 C13 C12 O6 -179.4(11) . . . . ?
C16 C13 C12 O6 1.8(17) . . . . ?
N7 C13 C12 O5 1.2(16) . . . . ?
C16 C13 C12 O5 -177.6(10) . . . . ?
Pb1 O7 C22 O8 -169.6(9) . . . . ?
Pb1 O7 C22 C21 10.9(14) . . . . ?
C20 N11 C21 C18 -0.3(16) . . . . ?
Pb1 N11 C21 C18 171.5(7) . . . . ?
C20 N11 C21 C22 -177.8(11) . . . . ?
Pb1 N11 C21 C22 -6.0(12) . . . . ?
N10 C18 C21 N11 176.7(10) . . . . ?
N12 C18 C21 N11 -2.1(16) . . . . ?
N10 C18 C21 C22 -6.0(16) . . . . ?
N12 C18 C21 C22 175.1(10) . . . . ?
O8 C22 C21 N11 178.0(11) . . . . ?
O7 C22 C21 N11 -2.4(15) . . . . ?
O8 C22 C21 C18 0.7(17) . . . . ?
O7 C22 C21 C18 -179.8(10) . . . . ?
C21 N11 C20 C19 2.9(19) . . . . ?
Pb1 N11 C20 C19 -168.3(10) . . . . ?
C18 N12 C19 C20 1(2) . . . . ?
N11 C20 C19 N12 -3(2) . . . . ?
C16 N8 C15 C14 0.3(18) . . . . ?
C13 N7 C14 C15 0.7(18) . . . . ?
Pb2 N7 C14 C15 173.2(9) 4_675 . . . ?
N8 C15 C14 N7 -1(2) . . . . ?
C2 N1 C3 C4 7.3(19) . . . . ?
Pb1 N1 C3 C4 -174.9(10) . . . . ?
N1 C3 C4 N2 -9(2) . . . . ?
C3 C4 N2 C5 5(3) . . . . ?
C4 N2 C5 N3 179.8(16) . . . . ?
C4 N2 C5 C2 -1(2) . . . . ?
N2 C5 N3 C6 -2(3) . . . . ?
C2 C5 N3 C6 178.4(15) . . . . ?
C5 N3 C6 N4 -81(2) . . . . ?
N3 C6 N4 C7 -91(2) . . . . ?
C6 N4 C7 N6 13(2) . . . . ?
C6 N4 C7 C10 -169.6(15) . . . . ?
C9 N5 C10 C7 6(2) . . . . ?
Pb2 N5 C10 C7 -166.6(11) . . . . ?
C9 N5 C10 C11 -174.8(13) . . . . ?
Pb2 N5 C10 C11 12.7(16) . . . . ?
N6 C7 C10 N5 -10(2) . . . . ?
N4 C7 C10 N5 172.3(14) . . . . ?
N6 C7 C10 C11 170.8(15) . . . . ?
N4 C7 C10 C11 -7(2) . . . . ?
Pb2 O3 C11 O4 171.9(10) . . . . ?
Pb1 O3 C11 O4 -25.2(19) 3_666 . . . ?
Pb2 O3 C11 C10 -1.2(16) . . . . ?
Pb1 O3 C11 C10 161.8(8) 3_666 . . . ?
N5 C10 C11 O4 178.7(14) . . . . ?
C7 C10 C11 O4 -2(2) . . . . ?
N5 C10 C11 O3 -8.2(19) . . . . ?
C7 C10 C11 O3 171.2(13) . . . . ?
C10 N5 C9 C8 1(2) . . . . ?
Pb2 N5 C9 C8 172.6(11) . . . . ?
N5 C9 C8 N6 -4(3) . . . . ?
N4 C7 N6 C8 -175.5(16) . . . . ?
C10 C7 N6 C8 7(2) . . . . ?
C9 C8 N6 C7 0(3) . . . . ?
C3 N1 C2 C5 -3.5(19) . . . . ?
Pb1 N1 C2 C5 178.6(10) . . . . ?
C3 N1 C2 C1 -179.5(11) . . . . ?
Pb1 N1 C2 C1 2.6(14) . . . . ?
N2 C5 C2 N1 0(2) . . . . ?
N3 C5 C2 N1 179.4(13) . . . . ?
N2 C5 C2 C1 175.9(14) . . . . ?
N3 C5 C2 C1 -5(2) . . . . ?
Pb1 O1 C1 O2 177.5(9) . . . . ?
Pb2 O1 C1 O2 -22.7(17) 3_566 . . . ?
Pb1 O1 C1 C2 -4.1(14) . . . . ?
Pb2 O1 C1 C2 155.7(8) 3_566 . . . ?
N1 C2 C1 O2 179.2(12) . . . . ?
C5 C2 C1 O2 3(2) . . . . ?
N1 C2 C1 O1 0.8(17) . . . . ?
C5 C2 C1 O1 -175.0(13) . . . . ?

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
N10 H10N O8 0.86 2.05 2.673(11) 128.8 .
N9 H9N O6 0.86 2.03 2.673(12) 130.9 .
C17 H17A N12 0.97 2.65 3.431(13) 138.2 3_676
C17 H17B N8 0.97 2.68 3.472(14) 138.7 3_776
C20 H20 O8 0.93 2.48 3.222(13) 136.4 1_455
C14 H14 O6 0.93 2.55 3.286(13) 136.9 1_655
C3 H3 O2 0.93 2.40 3.203(14) 145.0 1_655
N3 H3N O2 0.86 1.94 2.627(16) 135.5 .
N4 H4N O4 0.86 2.00 2.655(16) 132.1 .
C9 H9 O4 0.93 2.46 3.217(14) 139.2 1_455

_refine_diff_density_max         2.793
_refine_diff_density_min         -1.110
_refine_diff_density_rms         0.183

_shelxl_version_number           2014/6

_database_code_depnum_ccdc_archive 'CCDC 1017109'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H16 N12 O8 Pb2'
_chemical_formula_weight         966.83

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                   7.7520(3)
_cell_length_b                   7.8081(3)
_cell_length_c                   11.2756(5)
_cell_angle_alpha                85.184(2)
_cell_angle_beta                 86.853(2)
_cell_angle_gamma                67.1140(10)
_cell_volume                     626.36(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    6206
_cell_measurement_theta_min      2.85
_cell_measurement_theta_max      26.36

_exptl_crystal_description       Block
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.563
_exptl_crystal_F_000             448
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    13.496
_shelx_estimated_absorpt_T_min   0.103
_shelx_estimated_absorpt_T_max   0.173
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.02
_exptl_absorpt_correction_T_max  0.06
_exptl_absorpt_process_details   SADABS

_exptl_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_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7136
_diffrn_reflns_av_unetI/netI     0.0191
_diffrn_reflns_av_R_equivalents  0.0182
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.838
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             2550
_reflns_number_gt                2475
_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    'SIR97 (Giacovazzo et al, 1997)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_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)+(0.0310P)²+0.8235P] 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         2550
_refine_ls_number_parameters     190
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0220
_refine_ls_R_factor_gt           0.0214
_refine_ls_wR_factor_ref         0.0544
_refine_ls_wR_factor_gt          0.0540
_refine_ls_goodness_of_fit_ref   1.166
_refine_ls_restrained_S_all      1.166
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.43976(2) 0.18447(2) 0.13204(2) 0.02970(7) Uani 1 1 d . . . . .
O2 O 0.0894(4) 0.0714(4) -0.1343(3) 0.0360(6) Uani 1 1 d . . . . .
O3 O 0.3917(5) -0.0533(4) 0.2392(3) 0.0391(7) Uani 1 1 d . . . . .
O1 O 0.3182(4) 0.0853(4) -0.0290(3) 0.0356(6) Uani 1 1 d . . . . .
N1 N 0.0759(4) 0.3166(5) 0.1192(3) 0.0264(6) Uani 1 1 d . . . . .
N2 N -0.3064(4) 0.4731(5) 0.0816(3) 0.0304(7) Uani 1 1 d . . . . .
N3 N -0.2672(5) 0.3149(5) -0.0873(3) 0.0366(8) Uani 1 1 d . . . . .
H3A H -0.3858 0.3703 -0.0975 0.055 Uiso 1 1 calc R U . . .
H3B H -0.1985 0.2375 -0.1372 0.055 Uiso 1 1 calc R U . . .
O4 O 0.3016(7) -0.1785(5) 0.4030(4) 0.0601(11) Uani 1 1 d . . . . .
N4 N 0.3389(5) 0.2574(5) 0.3506(3) 0.0337(7) Uani 1 1 d . . . . .
C3 C -0.1891(5) 0.3494(5) 0.0068(3) 0.0259(7) Uani 1 1 d . . . . .
C2 C 0.0070(5) 0.2687(5) 0.0274(3) 0.0243(7) Uani 1 1 d . . . . .
C5 C -0.0414(6) 0.4391(6) 0.1926(4) 0.0304(8) Uani 1 1 d . . . . .
H5 H 0.0052 0.4728 0.2572 0.036 Uiso 1 1 calc R U . . .
C1 C 0.1457(5) 0.1313(5) -0.0525(3) 0.0274(7) Uani 1 1 d . . . . .
N5 N 0.2069(7) 0.3087(6) 0.5826(4) 0.0460(10) Uani 1 1 d . . . . .
C4 C -0.2323(6) 0.5154(6) 0.1723(4) 0.0315(8) Uani 1 1 d . . . . .
H4 H -0.3112 0.5997 0.2243 0.038 Uiso 1 1 calc R U . . .
N6 N 0.1973(7) 0.0178(6) 0.6006(4) 0.0542(11) Uani 1 1 d . . . . .
H6A H 0.1592 0.0372 0.6732 0.081 Uiso 1 1 calc R U . . .
H6B H 0.2123 -0.0860 0.5721 0.081 Uiso 1 1 calc R U . . .
C6 C 0.3322(6) -0.0495(6) 0.3483(4) 0.0349(9) Uani 1 1 d . . . . .
C7 C 0.3006(6) 0.1234(6) 0.4127(4) 0.0310(8) Uani 1 1 d . . . . .
C8 C 0.2332(6) 0.1484(6) 0.5324(4) 0.0362(9) Uani 1 1 d . . . . .
C10 C 0.3146(7) 0.4139(6) 0.4004(4) 0.0410(10) Uani 1 1 d . . . . .
H10 H 0.3416 0.5077 0.3572 0.049 Uiso 1 1 calc R U . . .
C9 C 0.2487(8) 0.4362(7) 0.5170(4) 0.0485(12) Uani 1 1 d . . . . .
H9 H 0.2331 0.5461 0.5508 0.058 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 O3 2.271(3) . ?
Pb1 O1 2.403(3) . ?
Pb1 O1 2.531(3) 2_655 ?
Pb1 N4 2.585(3) . ?
Pb1 N1 2.608(3) . ?
O2 C1 1.239(5) . ?
O3 C6 1.288(5) . ?
O1 C1 1.279(5) . ?
O1 Pb1 2.531(3) 2_655 ?
N1 C2 1.333(5) . ?
N1 C5 1.342(5) . ?
N2 C4 1.325(5) . ?
N2 C3 1.356(5) . ?
N3 C3 1.346(5) . ?
O4 C6 1.231(6) . ?
N4 C7 1.330(5) . ?
N4 C10 1.331(5) . ?
C3 C2 1.425(5) . ?
C2 C1 1.509(5) . ?
C5 C4 1.388(6) . ?
N5 C9 1.321(7) . ?
N5 C8 1.355(6) . ?
N6 C8 1.332(6) . ?
C6 C7 1.515(6) . ?
C7 C8 1.421(6) . ?
C10 C9 1.384(7) . ?

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
O3 Pb1 O1 84.05(11) . . ?
O3 Pb1 O1 81.26(11) . 2_655 ?
O1 Pb1 O1 66.26(11) . 2_655 ?
O3 Pb1 N4 67.29(11) . . ?
O1 Pb1 N4 135.70(11) . . ?
O1 Pb1 N4 135.42(11) 2_655 . ?
O3 Pb1 N1 82.31(11) . . ?
O1 Pb1 N1 64.12(9) . . ?
O1 Pb1 N1 128.90(9) 2_655 . ?
N4 Pb1 N1 78.62(11) . . ?
C6 O3 Pb1 125.2(3) . . ?
C1 O1 Pb1 126.9(2) . . ?
C1 O1 Pb1 118.2(2) . 2_655 ?
Pb1 O1 Pb1 113.74(11) . 2_655 ?
C2 N1 C5 119.4(3) . . ?
C2 N1 Pb1 116.4(2) . . ?
C5 N1 Pb1 124.0(3) . . ?
C4 N2 C3 117.9(3) . . ?
C7 N4 C10 120.1(4) . . ?
C7 N4 Pb1 113.3(3) . . ?
C10 N4 Pb1 126.5(3) . . ?
N3 C3 N2 116.6(3) . . ?
N3 C3 C2 123.3(3) . . ?
N2 C3 C2 120.1(3) . . ?
N1 C2 C3 120.1(3) . . ?
N1 C2 C1 117.0(3) . . ?
C3 C2 C1 122.9(3) . . ?
N1 C5 C4 120.0(4) . . ?
O2 C1 O1 124.6(4) . . ?
O2 C1 C2 120.0(3) . . ?
O1 C1 C2 115.4(3) . . ?
C9 N5 C8 117.6(4) . . ?
N2 C4 C5 122.6(4) . . ?
O4 C6 O3 123.8(4) . . ?
O4 C6 C7 118.6(4) . . ?
O3 C6 C7 117.7(4) . . ?
N4 C7 C8 119.7(4) . . ?
N4 C7 C6 116.3(4) . . ?
C8 C7 C6 124.0(4) . . ?
N6 C8 N5 117.1(4) . . ?
N6 C8 C7 122.8(4) . . ?
N5 C8 C7 120.1(4) . . ?
N4 C10 C9 119.5(4) . . ?
N5 C9 C10 123.1(4) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H3A N2 0.86 2.22 3.067(5) 167.2 2_465
N3 H3B O2 0.86 2.10 2.731(5) 129.6 .
C5 H5 N4 0.93 2.69 3.282(5) 122.1 .
C5 H5 N5 0.93 2.62 3.235(6) 123.7 2_566
C4 H4 N5 0.93 2.61 3.236(6) 125.2 2_566
N6 H6A O2 0.86 2.22 3.078(5) 174.4 1_556
N6 H6B O4 0.86 2.08 2.716(6) 130.1 .
C10 H10 O4 0.93 2.44 3.147(5) 132.5 1_565

_refine_diff_density_max         2.075
_refine_diff_density_min         -0.725
_refine_diff_density_rms         0.144

_shelxl_version_number           2014-1

_database_code_depnum_ccdc_archive 'CCDC 1017110'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C14 H16 N8 O10 Pb2'
_chemical_formula_weight         870.73

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                   7.6846(4)
_cell_length_b                   8.0250(4)
_cell_length_c                   10.1201(5)
_cell_angle_alpha                102.495(2)
_cell_angle_beta                 99.181(2)
_cell_angle_gamma                112.272(3)
_cell_volume                     543.33(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9207
_cell_measurement_theta_min      2.88
_cell_measurement_theta_max      26.41

_exptl_crystal_description       Block
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.661
_exptl_crystal_F_000             400
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.170
_exptl_absorpt_coefficient_mu    15.544
_shelx_estimated_absorpt_T_min   0.093
_shelx_estimated_absorpt_T_max   0.178
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.018
_exptl_absorpt_correction_T_max  0.065
_exptl_absorpt_process_details   SADABS

_exptl_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_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10973
_diffrn_reflns_av_unetI/netI     0.0169
_diffrn_reflns_av_R_equivalents  0.0228
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.878
_diffrn_reflns_theta_max         26.407
_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 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2225
_reflns_number_gt                2167
_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    'SIR97 (Giacovazzo et al, 1997)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_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)+(0.0258P)²+0.6103P] 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         2225
_refine_ls_number_parameters     154
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0192
_refine_ls_R_factor_gt           0.0187
_refine_ls_wR_factor_ref         0.0462
_refine_ls_wR_factor_gt          0.0458
_refine_ls_goodness_of_fit_ref   1.190
_refine_ls_restrained_S_all      1.190
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.10389(2) 0.25480(2) 0.16115(2) 0.02922(6) Uani 1 1 d . . . . .
O2 O 0.3680(4) 0.0044(4) -0.1473(3) 0.0404(7) Uani 1 1 d . . . . .
O3 O 0.2444(5) 0.1096(4) 0.2924(3) 0.0432(7) Uani 1 1 d . . . . .
O4 O 0.0334(6) 0.1589(6) 0.4021(4) 0.0614(9) Uani 1 1 d . . . . .
O1 O 0.1695(4) 0.0748(4) -0.0328(3) 0.0331(6) Uani 1 1 d . . . . .
O5 O 0.3006(7) 0.5605(6) 0.3878(4) 0.0823(14) Uani 1 1 d . . . . .
N4 N 0.3189(6) 0.7635(6) 0.5840(5) 0.0574(11) Uani 1 1 d . . . . .
H4A H 0.4387 0.7936 0.6242 0.069 Uiso 1 1 calc R U . . .
H4B H 0.2542 0.8140 0.6262 0.069 Uiso 1 1 calc R U . . .
N1 N 0.4647(4) 0.3885(4) 0.1452(3) 0.0283(6) Uani 1 1 d . . . . .
N2 N 0.8364(4) 0.5240(5) 0.1070(4) 0.0346(7) Uani 1 1 d . . . . .
N3 N 0.7424(5) 0.2692(5) -0.0865(4) 0.0390(8) Uani 1 1 d . . . . .
H3A H 0.8591 0.3168 -0.0955 0.047 Uiso 1 1 calc R U . . .
H3B H 0.6565 0.1636 -0.1452 0.047 Uiso 1 1 calc R U . . .
C2 C 0.5033(5) 0.2904(5) 0.0396(3) 0.0246(6) Uani 1 1 d . . . . .
C1 C 0.3373(5) 0.1089(5) -0.0550(4) 0.0271(7) Uani 1 1 d . . . . .
C4 C 0.7915(5) 0.6158(5) 0.2120(4) 0.0368(8) Uani 1 1 d . . . . .
H4 H 0.8887 0.7286 0.2744 0.044 Uiso 1 1 calc R U . . .
C3 C 0.6075(6) 0.5518(6) 0.2329(4) 0.0351(8) Uani 1 1 d . . . . .
H3 H 0.5823 0.6215 0.3074 0.042 Uiso 1 1 calc R U . . .
C6 C 0.1623(7) 0.1074(6) 0.3924(5) 0.0440(10) Uani 1 1 d . . . . .
H6 H 0.2038 0.0631 0.4632 0.053 Uiso 1 1 calc R U . . .
C5 C 0.6946(5) 0.3590(5) 0.0186(4) 0.0277(7) Uani 1 1 d . . . . .
C7 C 0.2385(9) 0.6456(10) 0.4634(5) 0.0628(14) Uani 1 1 d . . . . .
H7 H 0.1091 0.6208 0.4274 0.075 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 O3 2.335(3) . ?
Pb1 O1 2.415(2) . ?
Pb1 O1 2.555(2) 2 ?
Pb1 N1 2.613(3) . ?
Pb1 O5 2.686(4) . ?
O2 C1 1.230(4) . ?
O3 C6 1.275(5) . ?
O4 C6 1.219(6) . ?
O1 C1 1.281(4) . ?
O1 Pb1 2.555(2) 2 ?
O5 C7 1.190(6) . ?
N4 C7 1.258(7) . ?
N4 H4A 0.8600 . ?
N4 H4B 0.8600 . ?
N1 C2 1.328(4) . ?
N1 C3 1.344(5) . ?
N2 C4 1.327(5) . ?
N2 C5 1.350(5) . ?
N3 C5 1.334(5) . ?
N3 H3A 0.8600 . ?
N3 H3B 0.8600 . ?
C2 C5 1.430(5) . ?
C2 C1 1.505(4) . ?
C4 C3 1.378(5) . ?
C4 H4 0.9300 . ?
C3 H3 0.9300 . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Pb1 O1 84.03(10) . . ?
O3 Pb1 O1 86.68(10) . 2 ?
O1 Pb1 O1 65.25(9) . 2 ?
O3 Pb1 N1 76.68(10) . . ?
O1 Pb1 N1 64.03(9) . . ?
O1 Pb1 N1 127.78(8) 2 . ?
O3 Pb1 O5 84.13(15) . . ?
O1 Pb1 O5 138.76(11) . . ?
O1 Pb1 O5 152.58(11) 2 . ?
N1 Pb1 O5 74.82(11) . . ?
C6 O3 Pb1 102.2(3) . . ?
C1 O1 Pb1 126.0(2) . . ?
C1 O1 Pb1 117.1(2) . 2 ?
Pb1 O1 Pb1 114.75(9) . 2 ?
C7 O5 Pb1 128.9(4) . . ?
C7 N4 H4A 120.0 . . ?
C7 N4 H4B 120.0 . . ?
H4A N4 H4B 120.0 . . ?
C2 N1 C3 119.3(3) . . ?
C2 N1 Pb1 116.7(2) . . ?
C3 N1 Pb1 123.9(2) . . ?
C4 N2 C5 117.8(3) . . ?
C5 N3 H3A 120.0 . . ?
C5 N3 H3B 120.0 . . ?
H3A N3 H3B 120.0 . . ?
N1 C2 C5 120.3(3) . . ?
N1 C2 C1 116.8(3) . . ?
C5 C2 C1 122.9(3) . . ?
O2 C1 O1 124.2(3) . . ?
O2 C1 C2 119.7(3) . . ?
O1 C1 C2 116.1(3) . . ?
N2 C4 C3 123.0(3) . . ?
N2 C4 H4 118.5 . . ?
C3 C4 H4 118.5 . . ?
N1 C3 C4 119.8(4) . . ?
N1 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
O4 C6 O3 124.9(4) . . ?
O4 C6 H6 117.5 . . ?
O3 C6 H6 117.5 . . ?
N3 C5 N2 116.9(3) . . ?
N3 C5 C2 123.4(3) . . ?
N2 C5 C2 119.7(3) . . ?
O5 C7 N4 130.7(6) . . ?
O5 C7 H7 114.6 . . ?
N4 C7 H7 114.6 . . ?

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
C3 N1 C2 C5 -0.7(5) . . . . ?
Pb1 N1 C2 C5 176.6(2) . . . . ?
C3 N1 C2 C1 -179.9(3) . . . . ?
Pb1 N1 C2 C1 -2.7(4) . . . . ?
Pb1 O1 C1 O2 172.9(3) . . . . ?
Pb1 O1 C1 O2 10.6(5) 2 . . . ?
Pb1 O1 C1 C2 -7.5(4) . . . . ?
Pb1 O1 C1 C2 -169.8(2) 2 . . . ?
N1 C2 C1 O2 -174.0(3) . . . . ?
C5 C2 C1 O2 6.7(5) . . . . ?
N1 C2 C1 O1 6.4(5) . . . . ?
C5 C2 C1 O1 -172.8(3) . . . . ?
C5 N2 C4 C3 -1.0(6) . . . . ?
C2 N1 C3 C4 0.3(6) . . . . ?
Pb1 N1 C3 C4 -176.7(3) . . . . ?
N2 C4 C3 N1 0.6(7) . . . . ?
Pb1 O3 C6 O4 4.6(5) . . . . ?
C4 N2 C5 N3 179.8(4) . . . . ?
C4 N2 C5 C2 0.6(5) . . . . ?
N1 C2 C5 N3 -178.9(4) . . . . ?
C1 C2 C5 N3 0.3(6) . . . . ?
N1 C2 C5 N2 0.2(5) . . . . ?
C1 C2 C5 N2 179.4(3) . . . . ?
Pb1 O5 C7 N4 164.1(6) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N4 H4A O3 0.86 2.21 3.063(5) 172.7 2_666
N4 H4B O2 0.86 2.28 2.850(5) 124.1 1_566
N4 H4B O4 0.86 2.28 3.016(6) 143.6 2_566
N3 H3A N2 0.86 2.24 3.093(4) 172.9 2_765
N3 H3B O2 0.86 2.09 2.721(4) 129.5 .
C3 H3 O5 0.93 2.35 3.047(6) 131.5 .

_refine_diff_density_max         1.756
_refine_diff_density_min         -0.637
_refine_diff_density_rms         0.146

_shelxl_version_number           2014-1

_database_code_depnum_ccdc_archive 'CCDC 1017111'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_3

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H26 N14 O10 Pb2'
_chemical_formula_weight         1084.97

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                   7.6487(5)
_cell_length_b                   12.2700(7)
_cell_length_c                   18.3447(12)
_cell_angle_alpha                81.365(2)
_cell_angle_beta                 87.259(2)
_cell_angle_gamma                73.959(2)
_cell_volume                     1635.82(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    7391
_cell_measurement_theta_min      2.96
_cell_measurement_theta_max      24.68

_exptl_crystal_description       Block
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.203
_exptl_crystal_F_000             1024
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.290
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    10.355
_shelx_estimated_absorpt_T_min   0.111
_shelx_estimated_absorpt_T_max   0.244
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.07
_exptl_absorpt_correction_T_max  0.14
_exptl_absorpt_process_details   SADABS

_exptl_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_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            18025
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.640
_diffrn_reflns_theta_max         24.700
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             5514
_reflns_number_gt                4373
_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    'SIR97 (Giacovazzo et al, 1997)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_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)+(0.0630P)²+2.3038P] 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         5514
_refine_ls_number_parameters     453
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0384
_refine_ls_wR_factor_ref         0.1102
_refine_ls_wR_factor_gt          0.1015
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_restrained_S_all      1.141
_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 0.08715(4) 0.60810(2) 0.16599(2) 0.03319(12) Uani 1 1 d . . . . .
O9 O 0.3535(12) 0.6403(7) 0.2583(5) 0.079(2) Uani 1 1 d . . . . .
Pb2 Pb 0.57940(4) 0.12174(2) 0.16225(2) 0.03227(12) Uani 1 1 d . . . . .
N2 N -0.5505(8) 0.6481(5) 0.0582(3) 0.0328(14) Uani 1 1 d . . . . .
N8 N -0.0580(8) 0.1487(5) 0.0569(3) 0.0311(14) Uani 1 1 d . . . . .
O5 O 0.4019(8) 0.3155(4) 0.1145(3) 0.0400(13) Uani 1 1 d . . . . .
O6 O 0.1434(8) 0.4340(4) 0.0710(3) 0.0431(14) Uani 1 1 d . . . . .
O1 O -0.0828(8) 0.8054(4) 0.1195(3) 0.0400(13) Uani 1 1 d . . . . .
O2 O -0.3403(9) 0.9289(4) 0.0765(4) 0.0461(15) Uani 1 1 d . . . . .
N1 N -0.2251(8) 0.6281(5) 0.1239(3) 0.0306(14) Uani 1 1 d . . . . .
N3 N -0.5909(9) 0.8413(5) 0.0227(4) 0.0385(16) Uani 1 1 d . . . . .
H3A H -0.6908 0.8439 0.0020 0.058 Uiso 1 1 calc R U . . .
H3B H -0.5564 0.9027 0.0210 0.058 Uiso 1 1 calc R U . . .
O3 O 0.0024(9) 0.4672(5) 0.2540(3) 0.0487(15) Uani 1 1 d . . . . .
N7 N 0.2697(8) 0.1348(5) 0.1210(3) 0.0300(14) Uani 1 1 d . . . . .
N9 N -0.1023(9) 0.3403(5) 0.0196(4) 0.0390(16) Uani 1 1 d . . . . .
H9A H -0.2021 0.3404 -0.0002 0.059 Uiso 1 1 calc R U . . .
H9B H -0.0706 0.4028 0.0165 0.059 Uiso 1 1 calc R U . . .
N10 N 0.4622(9) 0.2208(5) 0.2715(4) 0.0398(16) Uani 1 1 d . . . . .
O7 O 0.4745(8) 0.0048(5) 0.2568(3) 0.0448(14) Uani 1 1 d . . . . .
C1 C -0.2410(11) 0.8296(6) 0.0959(4) 0.0314(17) Uani 1 1 d . . . . .
C2 C -0.3212(10) 0.7312(6) 0.0913(4) 0.0293(16) Uani 1 1 d . . . . .
C3 C -0.2882(11) 0.5373(6) 0.1238(4) 0.0341(17) Uani 1 1 d . . . . .
H3 H -0.2219 0.4656 0.1463 0.041 Uiso 1 1 calc R U . . .
C4 C -0.4510(10) 0.5492(6) 0.0907(4) 0.0337(17) Uani 1 1 d . . . . .
H4 H -0.4925 0.4846 0.0913 0.040 Uiso 1 1 calc R U . . .
C5 C -0.4883(10) 0.7411(6) 0.0577(4) 0.0288(16) Uani 1 1 d . . . . .
N4 N -0.0679(9) 0.6867(5) 0.2767(4) 0.0392(16) Uani 1 1 d . . . . .
C7 C -0.0978(11) 0.6095(7) 0.3313(4) 0.041(2) Uani 1 1 d . . . . .
C6 C -0.0549(13) 0.4874(8) 0.3183(5) 0.047(2) Uani 1 1 d . . . . .
O4 O -0.0781(12) 0.4147(6) 0.3691(4) 0.078(2) Uani 1 1 d . . . . .
C10 C -0.1671(13) 0.6452(8) 0.4012(5) 0.052(2) Uani 1 1 d . . . . .
N5 N -0.1998(12) 0.7562(7) 0.4092(4) 0.060(2) Uani 1 1 d . . . . .
C9 C -0.1651(14) 0.8279(8) 0.3527(5) 0.057(3) Uani 1 1 d . . . . .
H9 H -0.1865 0.9044 0.3587 0.068 Uiso 1 1 calc R U . . .
C8 C -0.0995(13) 0.7964(7) 0.2860(5) 0.050(2) Uani 1 1 d . . . . .
H8 H -0.0774 0.8503 0.2479 0.060 Uiso 1 1 calc R U . . .
N6 N -0.2006(13) 0.5734(7) 0.4586(4) 0.079(3) Uani 1 1 d . . . . .
H6A H -0.2419 0.5985 0.4991 0.118 Uiso 1 1 calc R U . . .
H6B H -0.1810 0.5019 0.4552 0.118 Uiso 1 1 calc R U . . .
C12 C 0.1683(10) 0.2356(6) 0.0885(4) 0.0267(15) Uani 1 1 d . . . . .
C15 C 0.0029(9) 0.2434(6) 0.0548(4) 0.0280(15) Uani 1 1 d . . . . .
C14 C 0.0459(11) 0.0503(6) 0.0903(5) 0.0366(18) Uani 1 1 d . . . . .
H14 H 0.0065 -0.0152 0.0916 0.044 Uiso 1 1 calc R U . . .
C13 C 0.2094(11) 0.0400(6) 0.1232(4) 0.0339(17) Uani 1 1 d . . . . .
H13 H 0.2772 -0.0307 0.1465 0.041 Uiso 1 1 calc R U . . .
C11 C 0.2448(11) 0.3368(6) 0.0911(4) 0.0300(16) Uani 1 1 d . . . . .
C17 C 0.4267(11) 0.1545(7) 0.3306(4) 0.0375(18) Uani 1 1 d . . . . .
C16 C 0.4326(12) 0.0350(7) 0.3201(5) 0.041(2) Uani 1 1 d . . . . .
O8 O 0.3984(11) -0.0310(5) 0.3748(3) 0.0639(19) Uani 1 1 d . . . . .
C20 C 0.3906(13) 0.1976(8) 0.3980(5) 0.048(2) Uani 1 1 d . . . . .
N11 N 0.3867(13) 0.3069(7) 0.4043(4) 0.064(2) Uani 1 1 d . . . . .
C19 C 0.4202(14) 0.3695(7) 0.3438(5) 0.063(3) Uani 1 1 d . . . . .
H19 H 0.4162 0.4453 0.3459 0.076 Uiso 1 1 calc R U . . .
C18 C 0.4610(14) 0.3291(7) 0.2769(5) 0.054(2) Uani 1 1 d . . . . .
H18 H 0.4874 0.3766 0.2359 0.065 Uiso 1 1 calc R U . . .
N12 N 0.3574(14) 0.1325(7) 0.4605(4) 0.075(3) Uani 1 1 d . . . . .
H12A H 0.3356 0.1611 0.5011 0.113 Uiso 1 1 calc R U . . .
H12B H 0.3582 0.0625 0.4597 0.113 Uiso 1 1 calc R U . . .
C21 C 0.3851(16) 0.7264(10) 0.2728(7) 0.074(3) Uani 1 1 d . . . . .
H21 H 0.4185 0.7750 0.2341 0.089 Uiso 1 1 calc R U . . .
C22 C 0.327(2) 0.6871(13) 0.4029(8) 0.102(5) Uani 1 1 d . . . . .
H22A H 0.2237 0.6624 0.3916 0.152 Uiso 1 1 calc R U . . .
H22B H 0.2964 0.7314 0.4429 0.152 Uiso 1 1 calc R U . . .
H22C H 0.4273 0.6213 0.4167 0.152 Uiso 1 1 calc R U . . .
N13 N 0.3759(14) 0.7560(8) 0.3392(7) 0.080(3) Uani 1 1 d . . . . .
H13A H 0.4000 0.8188 0.3445 0.120 Uiso 1 1 calc R U . . .
C23 C 0.9113(17) 0.1732(12) 0.2776(8) 0.082(4) Uani 1 1 d . . . . .
H23 H 0.9233 0.2276 0.2379 0.099 Uiso 1 1 calc R U . . .
O10 O 0.8717(12) 0.0854(8) 0.2642(5) 0.086(3) Uani 1 1 d . . . . .
N14 N 0.9365(13) 0.1924(8) 0.3437(6) 0.073(3) Uani 1 1 d . . . . .
H14A H 0.9677 0.2533 0.3481 0.110 Uiso 1 1 calc R U . . .
C24 C 0.915(2) 0.1163(13) 0.4106(7) 0.105(5) Uani 1 1 d . . . . .
H24A H 0.7975 0.1022 0.4106 0.158 Uiso 1 1 calc R U . . .
H24B H 0.9247 0.1515 0.4529 0.158 Uiso 1 1 calc R U . . .
H24C H 1.0079 0.0451 0.4122 0.158 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 O3 2.387(6) . ?
Pb1 O1 2.454(5) . ?
Pb1 N1 2.481(6) . ?
Pb1 N4 2.487(6) . ?
O9 C21 1.216(13) . ?
Pb2 O7 2.338(5) . ?
Pb2 O5 2.443(5) . ?
Pb2 N7 2.477(6) . ?
Pb2 N10 2.501(6) . ?
N2 C4 1.313(10) . ?
N2 C5 1.351(9) . ?
N8 C14 1.326(10) . ?
N8 C15 1.361(9) . ?
O5 C11 1.241(9) . ?
O6 C11 1.242(9) . ?
O1 C1 1.246(9) . ?
O2 C1 1.254(9) . ?
N1 C3 1.332(9) . ?
N1 C2 1.342(9) . ?
N3 C5 1.348(9) . ?
N3 H3A 0.8600 . ?
N3 H3B 0.8600 . ?
O3 C6 1.273(10) . ?
N7 C12 1.334(9) . ?
N7 C13 1.359(9) . ?
N9 C15 1.330(9) . ?
N9 H9A 0.8600 . ?
N9 H9B 0.8600 . ?
N10 C17 1.320(10) . ?
N10 C18 1.345(11) . ?
O7 C16 1.271(10) . ?
C1 C2 1.512(10) . ?
C2 C5 1.413(10) . ?
C3 C4 1.374(11) . ?
C3 H3 0.9300 . ?
C4 H4 0.9300 . ?
N4 C7 1.328(10) . ?
N4 C8 1.336(10) . ?
C7 C10 1.447(12) . ?
C7 C6 1.496(12) . ?
C6 O4 1.232(11) . ?
C10 N6 1.331(12) . ?
C10 N5 1.344(12) . ?
N5 C9 1.322(12) . ?
C9 C8 1.370(12) . ?
C9 H9 0.9300 . ?
C8 H8 0.9300 . ?
N6 H6A 0.8600 . ?
N6 H6B 0.8600 . ?
C12 C15 1.408(10) . ?
C12 C11 1.520(9) . ?
C14 C13 1.381(11) . ?
C14 H14 0.9300 . ?
C13 H13 0.9300 . ?
C17 C20 1.402(11) . ?
C17 C16 1.495(11) . ?
C16 O8 1.257(10) . ?
C20 N12 1.352(11) . ?
C20 N11 1.356(11) . ?
N11 C19 1.309(12) . ?
C19 C18 1.381(12) . ?
C19 H19 0.9300 . ?
C18 H18 0.9300 . ?
N12 H12A 0.8600 . ?
N12 H12B 0.8600 . ?
C21 N13 1.315(15) . ?
C21 H21 0.9300 . ?
C22 N13 1.435(17) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
N13 H13A 0.8600 . ?
C23 O10 1.256(14) . ?
C23 N14 1.303(15) . ?
C23 H23 0.9300 . ?
N14 C24 1.459(16) . ?
N14 H14A 0.8600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?

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
O3 Pb1 O1 130.4(2) . . ?
O3 Pb1 N1 79.5(2) . . ?
O1 Pb1 N1 65.72(18) . . ?
O3 Pb1 N4 66.9(2) . . ?
O1 Pb1 N4 75.4(2) . . ?
N1 Pb1 N4 84.8(2) . . ?
O7 Pb2 O5 122.9(2) . . ?
O7 Pb2 N7 77.0(2) . . ?
O5 Pb2 N7 65.60(17) . . ?
O7 Pb2 N10 67.1(2) . . ?
O5 Pb2 N10 73.1(2) . . ?
N7 Pb2 N10 92.9(2) . . ?
C4 N2 C5 118.0(7) . . ?
C14 N8 C15 117.4(6) . . ?
C11 O5 Pb2 122.6(4) . . ?
C1 O1 Pb1 122.1(4) . . ?
C3 N1 C2 119.6(7) . . ?
C3 N1 Pb1 121.6(5) . . ?
C2 N1 Pb1 118.1(5) . . ?
C5 N3 H3A 120.0 . . ?
C5 N3 H3B 120.0 . . ?
H3A N3 H3B 120.0 . . ?
C6 O3 Pb1 121.9(5) . . ?
C12 N7 C13 119.4(6) . . ?
C12 N7 Pb2 118.6(4) . . ?
C13 N7 Pb2 121.5(5) . . ?
C15 N9 H9A 120.0 . . ?
C15 N9 H9B 120.0 . . ?
H9A N9 H9B 120.0 . . ?
C17 N10 C18 119.2(7) . . ?
C17 N10 Pb2 115.4(5) . . ?
C18 N10 Pb2 124.5(6) . . ?
C16 O7 Pb2 121.6(5) . . ?
O1 C1 O2 125.5(7) . . ?
O1 C1 C2 117.3(6) . . ?
O2 C1 C2 117.1(7) . . ?
N1 C2 C5 119.1(6) . . ?
N1 C2 C1 115.8(7) . . ?
C5 C2 C1 125.1(6) . . ?
N1 C3 C4 120.2(7) . . ?
N1 C3 H3 119.9 . . ?
C4 C3 H3 119.9 . . ?
N2 C4 C3 122.6(7) . . ?
N2 C4 H4 118.7 . . ?
C3 C4 H4 118.7 . . ?
N3 C5 N2 116.9(7) . . ?
N3 C5 C2 122.6(6) . . ?
N2 C5 C2 120.5(6) . . ?
C7 N4 C8 120.7(8) . . ?
C7 N4 Pb1 115.4(5) . . ?
C8 N4 Pb1 123.3(6) . . ?
N4 C7 C10 119.5(8) . . ?
N4 C7 C6 118.3(7) . . ?
C10 C7 C6 122.3(8) . . ?
O4 C6 O3 124.9(8) . . ?
O4 C6 C7 118.8(8) . . ?
O3 C6 C7 116.3(8) . . ?
N6 C10 N5 117.8(9) . . ?
N6 C10 C7 123.2(9) . . ?
N5 C10 C7 118.9(8) . . ?
C9 N5 C10 118.2(8) . . ?
N5 C9 C8 124.1(9) . . ?
N5 C9 H9 117.9 . . ?
C8 C9 H9 117.9 . . ?
N4 C8 C9 118.6(9) . . ?
N4 C8 H8 120.7 . . ?
C9 C8 H8 120.7 . . ?
C10 N6 H6A 120.0 . . ?
C10 N6 H6B 120.0 . . ?
H6A N6 H6B 120.0 . . ?
N7 C12 C15 120.4(6) . . ?
N7 C12 C11 115.3(6) . . ?
C15 C12 C11 124.3(6) . . ?
N9 C15 N8 116.0(6) . . ?
N9 C15 C12 123.7(6) . . ?
N8 C15 C12 120.4(6) . . ?
N8 C14 C13 123.5(7) . . ?
N8 C14 H14 118.3 . . ?
C13 C14 H14 118.3 . . ?
N7 C13 C14 118.9(7) . . ?
N7 C13 H13 120.5 . . ?
C14 C13 H13 120.5 . . ?
O5 C11 O6 125.6(7) . . ?
O5 C11 C12 117.2(6) . . ?
O6 C11 C12 117.2(7) . . ?
N10 C17 C20 119.5(8) . . ?
N10 C17 C16 115.9(7) . . ?
C20 C17 C16 124.6(7) . . ?
O8 C16 O7 123.3(8) . . ?
O8 C16 C17 118.1(8) . . ?
O7 C16 C17 118.6(7) . . ?
N12 C20 N11 116.0(8) . . ?
N12 C20 C17 121.9(8) . . ?
N11 C20 C17 122.1(8) . . ?
C19 N11 C20 115.8(8) . . ?
N11 C19 C18 123.7(8) . . ?
N11 C19 H19 118.1 . . ?
C18 C19 H19 118.1 . . ?
N10 C18 C19 119.6(8) . . ?
N10 C18 H18 120.2 . . ?
C19 C18 H18 120.2 . . ?
C20 N12 H12A 120.0 . . ?
C20 N12 H12B 120.0 . . ?
H12A N12 H12B 120.0 . . ?
O9 C21 N13 125.0(12) . . ?
O9 C21 H21 117.5 . . ?
N13 C21 H21 117.5 . . ?
N13 C22 H22A 109.5 . . ?
N13 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
N13 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 N13 C22 122.1(10) . . ?
C21 N13 H13A 118.9 . . ?
C22 N13 H13A 118.9 . . ?
O10 C23 N14 123.9(13) . . ?
O10 C23 H23 118.1 . . ?
N14 C23 H23 118.1 . . ?
C23 N14 C24 123.5(11) . . ?
C23 N14 H14A 118.2 . . ?
C24 N14 H14A 118.2 . . ?
N14 C24 H24A 109.5 . . ?
N14 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
N14 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pb1 O1 C1 O2 174.4(6) . . . . ?
Pb1 O1 C1 C2 -4.5(9) . . . . ?
C3 N1 C2 C5 0.2(10) . . . . ?
Pb1 N1 C2 C5 171.1(5) . . . . ?
C3 N1 C2 C1 178.5(6) . . . . ?
Pb1 N1 C2 C1 -10.5(8) . . . . ?
O1 C1 C2 N1 10.0(10) . . . . ?
O2 C1 C2 N1 -169.0(7) . . . . ?
O1 C1 C2 C5 -171.7(7) . . . . ?
O2 C1 C2 C5 9.2(11) . . . . ?
C2 N1 C3 C4 -0.1(11) . . . . ?
Pb1 N1 C3 C4 -170.8(6) . . . . ?
C5 N2 C4 C3 0.1(11) . . . . ?
N1 C3 C4 N2 0.0(12) . . . . ?
C4 N2 C5 N3 178.7(7) . . . . ?
C4 N2 C5 C2 -0.1(10) . . . . ?
N1 C2 C5 N3 -178.8(7) . . . . ?
C1 C2 C5 N3 3.0(11) . . . . ?
N1 C2 C5 N2 -0.1(10) . . . . ?
C1 C2 C5 N2 -178.3(6) . . . . ?
C8 N4 C7 C10 0.7(13) . . . . ?
Pb1 N4 C7 C10 172.6(6) . . . . ?
C8 N4 C7 C6 -178.3(8) . . . . ?
Pb1 N4 C7 C6 -6.3(10) . . . . ?
Pb1 O3 C6 O4 -170.1(8) . . . . ?
Pb1 O3 C6 C7 10.6(11) . . . . ?
N4 C7 C6 O4 178.4(9) . . . . ?
C10 C7 C6 O4 -0.6(14) . . . . ?
N4 C7 C6 O3 -2.2(12) . . . . ?
C10 C7 C6 O3 178.9(8) . . . . ?
N4 C7 C10 N6 180.0(9) . . . . ?
C6 C7 C10 N6 -1.1(15) . . . . ?
N4 C7 C10 N5 0.0(13) . . . . ?
C6 C7 C10 N5 178.9(9) . . . . ?
N6 C10 N5 C9 179.3(10) . . . . ?
C7 C10 N5 C9 -0.7(14) . . . . ?
C10 N5 C9 C8 0.7(16) . . . . ?
C7 N4 C8 C9 -0.7(14) . . . . ?
Pb1 N4 C8 C9 -171.9(7) . . . . ?
N5 C9 C8 N4 -0.1(16) . . . . ?
C13 N7 C12 C15 -1.8(10) . . . . ?
Pb2 N7 C12 C15 170.8(5) . . . . ?
C13 N7 C12 C11 178.1(6) . . . . ?
Pb2 N7 C12 C11 -9.2(8) . . . . ?
C14 N8 C15 N9 178.6(7) . . . . ?
C14 N8 C15 C12 -1.2(10) . . . . ?
N7 C12 C15 N9 -178.0(7) . . . . ?
C11 C12 C15 N9 2.1(11) . . . . ?
N7 C12 C15 N8 1.8(10) . . . . ?
C11 C12 C15 N8 -178.1(6) . . . . ?
C15 N8 C14 C13 0.7(11) . . . . ?
C12 N7 C13 C14 1.3(11) . . . . ?
Pb2 N7 C13 C14 -171.2(6) . . . . ?
N8 C14 C13 N7 -0.7(12) . . . . ?
Pb2 O5 C11 O6 174.7(6) . . . . ?
Pb2 O5 C11 C12 -3.8(9) . . . . ?
N7 C12 C11 O5 8.7(10) . . . . ?
C15 C12 C11 O5 -171.4(7) . . . . ?
N7 C12 C11 O6 -169.9(7) . . . . ?
C15 C12 C11 O6 10.0(11) . . . . ?
C18 N10 C17 C20 -0.7(13) . . . . ?
Pb2 N10 C17 C20 169.1(6) . . . . ?
C18 N10 C17 C16 -179.4(8) . . . . ?
Pb2 N10 C17 C16 -9.5(9) . . . . ?
Pb2 O7 C16 O8 -170.6(7) . . . . ?
Pb2 O7 C16 C17 8.4(11) . . . . ?
N10 C17 C16 O8 -179.5(8) . . . . ?
C20 C17 C16 O8 1.9(14) . . . . ?
N10 C17 C16 O7 1.5(12) . . . . ?
C20 C17 C16 O7 -177.1(8) . . . . ?
N10 C17 C20 N12 -178.5(9) . . . . ?
C16 C17 C20 N12 0.0(15) . . . . ?
N10 C17 C20 N11 1.5(14) . . . . ?
C16 C17 C20 N11 -179.9(9) . . . . ?
N12 C20 N11 C19 179.5(10) . . . . ?
C17 C20 N11 C19 -0.5(15) . . . . ?
C20 N11 C19 C18 -1.2(16) . . . . ?
C17 N10 C18 C19 -0.9(14) . . . . ?
Pb2 N10 C18 C19 -169.8(7) . . . . ?
N11 C19 C18 N10 2.0(17) . . . . ?
O9 C21 N13 C22 0(2) . . . . ?
O10 C23 N14 C24 -3(2) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H3A N8 0.86 2.22 3.082(9) 177.1 2_465
N3 H3B O2 0.86 2.10 2.728(9) 129.0 .
N3 H3B O2 0.86 2.49 3.043(8) 122.6 2_475
N9 H9A N2 0.86 2.18 3.033(9) 174.8 2_465
N9 H9B O6 0.86 2.11 2.727(9) 128.5 .
N9 H9B O6 0.86 2.32 2.953(8) 130.1 2_565
C4 H4 O5 0.93 2.40 3.322(8) 170.6 1_455
C8 H8 O1 0.93 2.50 3.036(11) 116.7 .
N6 H6A N11 0.86 2.33 3.181(11) 170.0 2_566
N6 H6B O4 0.86 2.05 2.679(11) 129.8 .
C14 H14 O1 0.93 2.46 3.374(9) 169.3 1_545
C19 H19 O9 0.93 2.61 3.367(13) 138.7 .
C18 H18 O5 0.93 2.62 3.070(11) 110.5 .
N12 H12A N5 0.86 2.14 2.970(11) 162.9 2_566
N12 H12B O8 0.86 2.03 2.673(10) 130.7 .
N13 H13A O8 0.86 2.00 2.839(10) 164.7 1_565
N14 H14A O4 0.86 2.01 2.806(11) 154.3 1_655


_refine_diff_density_max         2.913
_refine_diff_density_min         -0.663
_refine_diff_density_rms         0.236

_shelxl_version_number           2014-1

_database_code_depnum_ccdc_archive 'CCDC 1017112'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
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#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
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data_4

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H18 N12 O9 Pb2, 2.5(C3 H7 N1 O1)'
_chemical_formula_sum            'C27.50 H35.50 N14.50 O11.50 Pb2'
_chemical_formula_weight         1167.58

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

_space_group_crystal_system      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                   14.468(3)
_cell_length_b                   13.261(2)
_cell_length_c                   19.861(4)
_cell_angle_alpha                90
_cell_angle_beta                 90.964(7)
_cell_angle_gamma                90
_cell_volume                     3809.9(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9564
_cell_measurement_theta_min      2.47
_cell_measurement_theta_max      26.42

_exptl_crystal_description       Block
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.036
_exptl_crystal_F_000             2232
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    8.903
_shelx_estimated_absorpt_T_min   0.163
_shelx_estimated_absorpt_T_max   0.283
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.077
_exptl_absorpt_correction_T_max  0.175
_exptl_absorpt_process_details   SADABS
_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_measurement_device_type  'Bruker APEX-II PHOTON 100 detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            66637
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_av_R_equivalents  0.0886
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.312
_diffrn_reflns_theta_max         26.372
_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 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             7794
_reflns_number_gt                6291
_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    'SIR97 (Giacovazzo et al, 1997)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_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)+(0.0625P)²+5.3545P] 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         7794
_refine_ls_number_parameters     388
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0429
_refine_ls_wR_factor_ref         0.1095
_refine_ls_wR_factor_gt          0.1037
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 -0.054 0.065 1453 417 '10 Dimethylformamide molecules'
_platon_squeeze_details          
;These disordered dimethylformamide molecules could not be 
 modelled reliably,were removed from the model but included in the 
 empirical formulae. This justify the A-level alert in the checkcif report.
 The strategy improved the R1 factor by 29.12%. The electron count suggests 
 the presence of 10 DMF molecules per unit cell (electron count= 400), 
 2.5 DMF molecules per asymmetric unit.Thermogravimetric and elemental 
 analysis data support these results. 
;

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 0.04271(2) 0.21506(2) 0.62691(2) 0.03015(9) Uani 1 1 d . . . . .
Pb2 Pb 0.04634(2) -0.03000(2) 0.75665(2) 0.02921(9) Uani 1 1 d . . . . .
O3 O 0.0673(4) 0.1699(4) 0.7457(2) 0.0357(12) Uani 1 1 d . . . . .
O1 O 0.0862(4) 0.3897(4) 0.6508(2) 0.0351(12) Uani 1 1 d . . . . .
O7 O 0.1069(4) -0.1723(4) 0.8243(3) 0.0419(13) Uani 1 1 d . . . . .
O5 O 0.1045(4) 0.0387(4) 0.6460(2) 0.0383(13) Uani 1 1 d . . . . .
O2 O 0.1886(5) 0.4873(4) 0.7036(3) 0.0491(15) Uani 1 1 d . . . . .
O4 O 0.0885(5) 0.3211(4) 0.7911(2) 0.0516(17) Uani 1 1 d . . . . .
O8 O 0.2245(5) -0.2694(4) 0.8541(3) 0.0522(16) Uani 1 1 d . . . . .
N10 N 0.2193(5) -0.0269(5) 0.7802(3) 0.0363(15) Uani 1 1 d . . . . .
N7 N 0.1214(5) -0.1618(4) 0.6589(3) 0.0350(15) Uani 1 1 d . . . . .
O6 O 0.1132(6) 0.0303(4) 0.5359(3) 0.0562(19) Uani 1 1 d . . . . .
N4 N 0.0795(5) 0.0811(5) 0.8676(3) 0.0372(16) Uani 1 1 d . . . . .
N1 N 0.2139(5) 0.2500(5) 0.6271(3) 0.0363(15) Uani 1 1 d . . . . .
C6 C 0.0808(5) 0.2296(5) 0.7961(3) 0.0286(15) Uani 1 1 d . . . . .
N6 N 0.0987(6) 0.3398(5) 0.9247(3) 0.051(2) Uani 1 1 d . . . . .
H6A H 0.1035 0.3723 0.9621 0.077 Uiso 1 1 calc R U . . .
H6B H 0.0987 0.3719 0.8871 0.077 Uiso 1 1 calc R U . . .
C16 C 0.1904(6) -0.1896(6) 0.8310(4) 0.0355(17) Uani 1 1 d . . . . .
N5 N 0.0916(6) 0.1945(5) 0.9858(3) 0.0451(18) Uani 1 1 d . . . . .
C12 C 0.1250(5) -0.1227(5) 0.5973(3) 0.0308(16) Uani 1 1 d . . . . .
C17 C 0.2578(6) -0.1083(6) 0.8099(4) 0.0390(18) Uani 1 1 d . . . . .
C10 C 0.0913(6) 0.2410(6) 0.9251(3) 0.0355(18) Uani 1 1 d . . . . .
N8 N 0.1541(7) -0.2831(5) 0.5479(4) 0.059(2) Uani 1 1 d . . . . .
C7 C 0.0832(6) 0.1819(5) 0.8647(3) 0.0330(17) Uani 1 1 d . . . . .
N9 N 0.1396(7) -0.1497(6) 0.4770(3) 0.060(2) Uani 1 1 d . . . . .
H9A H 0.1463 -0.1910 0.4440 0.090 Uiso 1 1 calc R U . . .
H9B H 0.1317 -0.0865 0.4693 0.090 Uiso 1 1 calc R U . . .
C2 C 0.2403(6) 0.3398(6) 0.6513(4) 0.0385(18) Uani 1 1 d . . . . .
C3 C 0.2779(7) 0.1845(7) 0.6074(5) 0.050(2) Uani 1 1 d . . . . .
H3 H 0.2598 0.1229 0.5891 0.060 Uiso 1 1 calc R U . . .
C1 C 0.1666(6) 0.4106(5) 0.6707(3) 0.0333(17) Uani 1 1 d . . . . .
C11 C 0.1120(5) -0.0098(5) 0.5918(3) 0.0304(16) Uani 1 1 d . . . . .
C15 C 0.1415(6) -0.1842(6) 0.5408(4) 0.0401(19) Uani 1 1 d . . . . .
C13 C 0.1354(6) -0.2618(6) 0.6638(4) 0.045(2) Uani 1 1 d . . . . .
H13 H 0.1348 -0.2917 0.7061 0.055 Uiso 1 1 calc R U . . .
N2 N 0.3991(6) 0.2950(7) 0.6361(6) 0.079(3) Uani 1 1 d . . . . .
C8 C 0.0822(8) 0.0366(6) 0.9280(4) 0.050(2) Uani 1 1 d . . . . .
H8 H 0.0797 -0.0333 0.9312 0.060 Uiso 1 1 calc R U . . .
C9 C 0.0887(8) 0.0951(6) 0.9859(4) 0.056(3) Uani 1 1 d . . . . .
H9 H 0.0913 0.0621 1.0273 0.067 Uiso 1 1 calc R U . . .
N11 N 0.4087(6) -0.0355(7) 0.8037(5) 0.074(3) Uani 1 1 d . . . . .
C14 C 0.1498(9) -0.3184(7) 0.6114(5) 0.064(3) Uani 1 1 d . . . . .
H14 H 0.1575 -0.3873 0.6182 0.077 Uiso 1 1 calc R U . . .
C18 C 0.2756(7) 0.0486(7) 0.7631(5) 0.055(2) Uani 1 1 d . . . . .
H18 H 0.2509 0.1062 0.7432 0.066 Uiso 1 1 calc R U . . .
C4 C 0.3699(7) 0.2070(8) 0.6139(6) 0.073(3) Uani 1 1 d . . . . .
H4 H 0.4132 0.1585 0.6022 0.087 Uiso 1 1 calc R U . . .
N12 N 0.3959(7) -0.1937(8) 0.8496(6) 0.104(4) Uani 1 1 d . . . . .
H12A H 0.4548 -0.1938 0.8561 0.156 Uiso 1 1 calc R U . . .
H12B H 0.3636 -0.2450 0.8615 0.156 Uiso 1 1 calc R U . . .
C20 C 0.3544(7) -0.1138(8) 0.8212(5) 0.060(3) Uani 1 1 d . . . . .
C5 C 0.3375(7) 0.3616(8) 0.6561(6) 0.062(3) Uani 1 1 d . . . . .
N3 N 0.3706(7) 0.4484(7) 0.6802(6) 0.095(4) Uani 1 1 d . . . . .
H3A H 0.4293 0.4586 0.6820 0.114 Uiso 1 1 calc R U . . .
H3B H 0.3333 0.4942 0.6938 0.114 Uiso 1 1 calc R U . . .
C19 C 0.3676(8) 0.0424(8) 0.7742(7) 0.076(3) Uani 1 1 d . . . . .
H19 H 0.4043 0.0959 0.7603 0.091 Uiso 1 1 calc R U . . .
O9 O 0.1232(6) 0.5520(6) 0.8300(4) 0.076(2) Uani 1 1 d D . . . .
H9O H 0.1490 0.5222 0.7935 0.113 Uiso 1 1 d DR U . . .
H10O H 0.1556 0.6191 0.8523 0.113 Uiso 1 1 d R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 O1 2.444(5) . ?
Pb1 O3 2.454(4) . ?
Pb1 N1 2.519(7) . ?
Pb1 O5 2.530(5) . ?
Pb2 O7 2.469(5) . ?
Pb2 O5 2.536(5) . ?
Pb2 N10 2.539(7) . ?
Pb2 O3 2.677(5) . ?
Pb2 N4 2.688(6) . ?
O3 C6 1.288(8) . ?
O1 C1 1.254(9) . ?
O7 C16 1.235(10) . ?
O5 C11 1.260(8) . ?
O2 C1 1.247(9) . ?
O4 C6 1.224(8) . ?
O8 C16 1.252(9) . ?
N10 C18 1.338(11) . ?
N10 C17 1.346(10) . ?
N7 C12 1.331(9) . ?
N7 C13 1.345(10) . ?
O6 C11 1.231(8) . ?
N4 C8 1.336(9) . ?
N4 C7 1.339(9) . ?
N1 C3 1.332(11) . ?
N1 C2 1.338(10) . ?
C6 C7 1.501(9) . ?
N6 C10 1.314(10) . ?
C16 C17 1.517(11) . ?
N5 C9 1.319(10) . ?
N5 C10 1.353(9) . ?
C12 C15 1.410(10) . ?
C12 C11 1.514(9) . ?
C17 C20 1.414(12) . ?
C10 C7 1.437(9) . ?
N8 C15 1.331(10) . ?
N8 C14 1.347(12) . ?
N9 C15 1.348(10) . ?
C2 C5 1.436(13) . ?
C2 C1 1.477(11) . ?
C3 C4 1.369(14) . ?
C13 C14 1.302(13) . ?
N2 C4 1.314(13) . ?
N2 C5 1.321(13) . ?
C8 C9 1.389(11) . ?
N11 C19 1.324(12) . ?
N11 C20 1.351(12) . ?
C18 C19 1.348(15) . ?
N12 C20 1.339(12) . ?
C5 N3 1.332(12) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Pb1 O3 90.70(16) . . ?
O1 Pb1 N1 64.9(2) . . ?
O3 Pb1 N1 85.24(19) . . ?
O1 Pb1 O5 139.26(18) . . ?
O3 Pb1 O5 65.50(16) . . ?
N1 Pb1 O5 79.9(2) . . ?
O7 Pb2 O5 128.80(19) . . ?
O7 Pb2 N10 64.67(19) . . ?
O5 Pb2 N10 79.2(2) . . ?
O7 Pb2 O3 139.59(17) . . ?
O5 Pb2 O3 62.23(15) . . ?
N10 Pb2 O3 83.50(18) . . ?
O7 Pb2 N4 85.16(19) . . ?
O5 Pb2 N4 117.15(18) . . ?
N10 Pb2 N4 71.2(2) . . ?
O3 Pb2 N4 60.33(16) . . ?
C6 O3 Pb1 127.9(4) . . ?
C6 O3 Pb2 124.1(4) . . ?
Pb1 O3 Pb2 107.77(16) . . ?
C1 O1 Pb1 120.4(5) . . ?
C16 O7 Pb2 122.6(5) . . ?
C11 O5 Pb1 112.3(4) . . ?
C11 O5 Pb2 126.3(5) . . ?
Pb1 O5 Pb2 109.89(19) . . ?
C18 N10 C17 117.5(7) . . ?
C18 N10 Pb2 124.6(6) . . ?
C17 N10 Pb2 117.9(5) . . ?
C12 N7 C13 116.2(6) . . ?
C8 N4 C7 118.7(6) . . ?
C8 N4 Pb2 119.7(5) . . ?
C7 N4 Pb2 121.2(4) . . ?
C3 N1 C2 119.3(8) . . ?
C3 N1 Pb1 124.6(6) . . ?
C2 N1 Pb1 116.1(5) . . ?
O4 C6 O3 124.0(6) . . ?
O4 C6 C7 119.4(6) . . ?
O3 C6 C7 116.6(6) . . ?
O7 C16 O8 125.2(8) . . ?
O7 C16 C17 118.1(7) . . ?
O8 C16 C17 116.8(7) . . ?
C9 N5 C10 117.3(6) . . ?
N7 C12 C15 121.1(6) . . ?
N7 C12 C11 116.4(6) . . ?
C15 C12 C11 122.5(6) . . ?
N10 C17 C20 120.7(8) . . ?
N10 C17 C16 115.3(7) . . ?
C20 C17 C16 123.9(7) . . ?
N6 C10 N5 117.5(6) . . ?
N6 C10 C7 123.0(6) . . ?
N5 C10 C7 119.6(6) . . ?
C15 N8 C14 115.7(7) . . ?
N4 C7 C10 120.7(6) . . ?
N4 C7 C6 117.3(6) . . ?
C10 C7 C6 121.9(6) . . ?
N1 C2 C5 118.5(8) . . ?
N1 C2 C1 117.1(7) . . ?
C5 C2 C1 124.4(7) . . ?
N1 C3 C4 120.7(9) . . ?
O2 C1 O1 125.0(8) . . ?
O2 C1 C2 118.4(8) . . ?
O1 C1 C2 116.6(6) . . ?
O6 C11 O5 123.5(7) . . ?
O6 C11 C12 119.3(6) . . ?
O5 C11 C12 117.1(6) . . ?
N8 C15 N9 115.7(7) . . ?
N8 C15 C12 120.7(7) . . ?
N9 C15 C12 123.4(7) . . ?
C14 C13 N7 122.5(8) . . ?
C4 N2 C5 118.7(9) . . ?
N4 C8 C9 119.8(7) . . ?
N5 C9 C8 123.9(7) . . ?
C19 N11 C20 117.0(9) . . ?
C13 C14 N8 123.9(8) . . ?
N10 C18 C19 121.1(9) . . ?
N2 C4 C3 122.1(10) . . ?
N12 C20 N11 117.3(9) . . ?
N12 C20 C17 122.9(9) . . ?
N11 C20 C17 119.9(8) . . ?
N2 C5 N3 116.4(10) . . ?
N2 C5 C2 120.7(9) . . ?
N3 C5 C2 122.9(10) . . ?
N11 C19 C18 123.7(10) . . ?

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
N6 H6A O6 0.86 1.96 2.806(8) 168.8 4_566
N6 H6B O4 0.86 2.03 2.668(8) 130.7 .
N9 H9A O8 0.86 2.20 2.954(9) 147.0 4
N9 H9B O6 0.86 2.06 2.689(9) 129.6 .
C3 H3 O6 0.93 2.66 3.430(12) 141.2 .
C9 H9 O1 0.93 2.54 3.281(9) 137.2 4_566
C14 H14 O2 0.93 2.41 3.205(11) 143.1 1_545
N12 H12A N2 0.86 2.12 2.978(13) 174.1 2_646
N12 H12B O8 0.86 2.04 2.677(12) 130.2 .
N3 H3A N11 0.86 2.36 3.210(13) 171.6 2_656
N3 H3B O2 0.86 2.11 2.731(12) 128.9 .
O9 H9O O2 0.91 1.94 2.830(9) 165.2 .
O9 H10O O8 1.10 1.78 2.822(9) 156.3 1_565
O9 H10O N9 1.10 2.52 3.200(10) 118.9 4_566

_refine_diff_density_max         3.527
_refine_diff_density_min         -1.104
_refine_diff_density_rms         0.216

_shelxl_version_number           2014/6

_database_code_depnum_ccdc_archive 'CCDC 1017113'
