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

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

data_a
_database_code_depnum_ccdc_archive 'CCDC 1578665'
_audit_update_record             
;
2017-10-08 deposited with the CCDC.
2018-04-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C48 H30 N9 O10 Pb2'
_chemical_formula_sum            'C48 H30 N9 O10 Pb2'
_chemical_formula_weight         1303.16

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

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_Hall  -P1

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

_cell_length_a                   9.3290(7)
_cell_length_b                   10.7880(8)
_cell_length_c                   11.7803(9)
_cell_angle_alpha                109.9250(10)
_cell_angle_beta                 98.2990(10)
_cell_angle_gamma                103.9100(10)
_cell_volume                     1048.14(14)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1945
_cell_measurement_theta_min      1.90
_cell_measurement_theta_max      25.93

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.182
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.048
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.065
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             621
_exptl_absorpt_coefficient_mu    8.097
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.277
_exptl_absorpt_correction_T_max  0.678
_exptl_absorpt_process_details   '(SADABS; Bruker, 2002)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            5690
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_av_sigmaI/netI    0.0558
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.90
_diffrn_reflns_theta_max         25.93
_reflns_number_total             4048
_reflns_number_gt                3496
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'SMART (Bruker, 2002)'
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_reduction        'SHELXS97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXS97 (Sheldrick, 1997)'
_computing_publication_material  SHELXTL

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0308P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4048
_refine_ls_number_parameters     316
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0325
_refine_ls_wR_factor_ref         0.0683
_refine_ls_wR_factor_gt          0.0645
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_restrained_S_all      0.995
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 1.3804(7) 0.2897(6) 0.7464(6) 0.0349(15) Uani 1 1 d . . .
H1 H 1.4102 0.3772 0.8104 0.042 Uiso 1 1 calc R . .
C2 C 1.4521(7) 0.1944(6) 0.7599(6) 0.0342(15) Uani 1 1 d . . .
H2 H 1.5252 0.2167 0.8323 0.041 Uiso 1 1 calc R . .
C3 C 1.4123(7) 0.0666(6) 0.6635(6) 0.0316(14) Uani 1 1 d . . .
H3 H 1.4580 0.0008 0.6701 0.038 Uiso 1 1 calc R . .
C4 C 1.3023(6) 0.0366(6) 0.5555(5) 0.0242(13) Uani 1 1 d . . .
C5 C 1.2512(6) -0.0922(5) 0.4487(5) 0.0230(12) Uani 1 1 d . . .
C6 C 1.1399(6) -0.1168(6) 0.3458(6) 0.0266(13) Uani 1 1 d . . .
C7 C 1.0684(7) -0.0155(6) 0.3373(5) 0.0269(13) Uani 1 1 d . . .
C8 C 0.9603(7) -0.0338(6) 0.2348(6) 0.0336(15) Uani 1 1 d . . .
H8 H 0.9322 -0.1149 0.1635 0.040 Uiso 1 1 calc R . .
C9 C 0.8943(7) 0.0678(6) 0.2382(6) 0.0375(16) Uani 1 1 d . . .
H9 H 0.8238 0.0587 0.1691 0.045 Uiso 1 1 calc R . .
C10 C 0.9367(7) 0.1855(6) 0.3490(6) 0.0322(15) Uani 1 1 d . . .
H10 H 0.8876 0.2519 0.3535 0.039 Uiso 1 1 calc R . .
C11 C 1.1113(6) 0.1096(6) 0.4425(5) 0.0236(13) Uani 1 1 d . . .
C12 C 1.2291(6) 0.1364(5) 0.5508(5) 0.0237(13) Uani 1 1 d . . .
C13 C 1.2016(6) -0.3022(5) 0.3086(5) 0.0251(13) Uani 1 1 d . . .
C14 C 1.2136(7) -0.4415(6) 0.2395(6) 0.0283(14) Uani 1 1 d . . .
C15 C 1.1988(7) -0.4767(6) 0.1138(6) 0.0379(16) Uani 1 1 d . . .
H15 H 1.1783 -0.4159 0.0784 0.045 Uiso 1 1 calc R . .
C16 C 1.2140(8) -0.6012(7) 0.0388(6) 0.050(2) Uani 1 1 d . . .
H16 H 1.2024 -0.6243 -0.0463 0.060 Uiso 1 1 calc R . .
C17 C 1.2462(9) -0.6900(7) 0.0916(6) 0.053(2) Uani 1 1 d . . .
H17 H 1.2588 -0.7727 0.0422 0.063 Uiso 1 1 calc R . .
C18 C 1.2603(7) -0.6573(6) 0.2182(6) 0.0370(16) Uani 1 1 d . . .
H18 H 1.2817 -0.7185 0.2527 0.044 Uiso 1 1 calc R . .
C19 C 1.2427(6) -0.5332(6) 0.2943(5) 0.0255(13) Uani 1 1 d . . .
C20 C 1.2310(6) -0.5183(5) 0.4225(6) 0.0250(13) Uani 1 1 d . . .
C21 C 1.3755(7) 0.9262(6) 1.0301(6) 0.0306(14) Uani 1 1 d . . .
C22 C 1.4259(7) 0.8594(6) 0.9282(5) 0.0278(14) Uani 1 1 d . . .
C23 C 1.5483(7) 0.9329(6) 0.8991(6) 0.0323(15) Uani 1 1 d . . .
H23 H 1.5810 0.8872 0.8303 0.039 Uiso 1 1 calc R . .
C24 C 1.3496(8) 0.7076(7) 0.8472(6) 0.0424(17) Uani 1 1 d . . .
N1 N 1.2724(5) 0.2623(5) 0.6476(5) 0.0269(11) Uani 1 1 d . . .
N2 N 1.0418(5) 0.2078(4) 0.4470(4) 0.0241(11) Uani 1 1 d . . .
N3 N 1.2884(5) -0.2111(4) 0.4242(4) 0.0270(11) Uani 1 1 d . . .
H3A H 1.3544 -0.2263 0.4724 0.032 Uiso 1 1 calc R . .
N4 N 1.1086(5) -0.2491(5) 0.2575(5) 0.0287(12) Uani 1 1 d . . .
N5 N 1.2505(12) 0.8662(11) 1.0592(10) 0.043(3) Uani 0.50 1 d P . .
H5A H 1.1968 0.7818 1.0135 0.051 Uiso 0.50 1 calc PR . .
H5B H 1.2240 0.9123 1.1236 0.051 Uiso 0.50 1 calc PR . .
O1 O 1.1379(4) -0.4596(4) 0.4683(4) 0.0313(10) Uani 1 1 d . . .
O2 O 1.3046(4) -0.5695(4) 0.4807(4) 0.0278(9) Uani 1 1 d . . .
O1W O 1.5089(4) 0.7456(4) 0.5789(4) 0.0333(10) Uani 1 1 d . . .
O3 O 1.3641(5) 0.6623(4) 0.7381(4) 0.0471(13) Uani 1 1 d . . .
O4 O 1.2752(8) 0.6323(5) 0.8907(5) 0.089(2) Uani 1 1 d . . .
Pb Pb 1.14461(3) 0.44646(2) 0.63770(2) 0.02524(8) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.320(7) . ?
C1 C2 1.393(8) . ?
C1 H1 0.9300 . ?
C2 C3 1.376(8) . ?
C2 H2 0.9300 . ?
C3 C4 1.400(8) . ?
C3 H3 0.9300 . ?
C4 C12 1.417(7) . ?
C4 C5 1.435(7) . ?
C5 N3 1.356(7) . ?
C5 C6 1.379(8) . ?
C6 N4 1.379(7) . ?
C6 C7 1.434(8) . ?
C7 C8 1.380(8) . ?
C7 C11 1.404(8) . ?
C8 C9 1.373(8) . ?
C8 H8 0.9300 . ?
C9 C10 1.397(8) . ?
C9 H9 0.9300 . ?
C10 N2 1.312(7) . ?
C10 H10 0.9300 . ?
C11 N2 1.360(7) . ?
C11 C12 1.453(8) . ?
C12 N1 1.362(7) . ?
C13 N4 1.329(7) . ?
C13 N3 1.365(7) . ?
C13 C14 1.486(7) . ?
C14 C15 1.374(9) . ?
C14 C19 1.408(8) . ?
C15 C16 1.387(9) . ?
C15 H15 0.9300 . ?
C16 C17 1.373(10) . ?
C16 H16 0.9300 . ?
C17 C18 1.389(9) . ?
C17 H17 0.9300 . ?
C18 C19 1.397(7) . ?
C18 H18 0.9300 . ?
C19 C20 1.485(8) . ?
C20 O2 1.245(7) . ?
C20 O1 1.271(6) . ?
C21 N5 1.342(12) . ?
C21 C22 1.385(8) . ?
C21 C23 1.399(8) 2_877 ?
C22 C23 1.383(9) . ?
C22 C24 1.509(8) . ?
C23 C21 1.399(8) 2_877 ?
C23 H23 0.9300 . ?
C24 O4 1.232(8) . ?
C24 O3 1.251(8) . ?
N1 Pb 2.577(5) . ?
N2 Pb 2.616(4) . ?
N3 H3A 0.8600 . ?
N5 H5A 0.8600 . ?
N5 H5B 0.8600 . ?
O1 Pb 2.528(4) 1_545 ?
O2 Pb 2.526(4) 1_545 ?
O3 Pb 2.479(4) . ?
Pb O2 2.526(4) 1_565 ?
Pb O1 2.528(4) 1_565 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 123.4(5) . . ?
N1 C1 H1 118.3 . . ?
C2 C1 H1 118.3 . . ?
C3 C2 C1 118.5(6) . . ?
C3 C2 H2 120.7 . . ?
C1 C2 H2 120.7 . . ?
C2 C3 C4 119.3(6) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C3 C4 C12 119.0(5) . . ?
C3 C4 C5 124.7(5) . . ?
C12 C4 C5 116.2(5) . . ?
N3 C5 C6 105.7(5) . . ?
N3 C5 C4 132.1(5) . . ?
C6 C5 C4 122.1(5) . . ?
C5 C6 N4 110.9(5) . . ?
C5 C6 C7 122.5(5) . . ?
N4 C6 C7 126.6(5) . . ?
C8 C7 C11 118.7(5) . . ?
C8 C7 C6 124.6(5) . . ?
C11 C7 C6 116.7(5) . . ?
C9 C8 C7 119.9(6) . . ?
C9 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
C8 C9 C10 117.7(6) . . ?
C8 C9 H9 121.1 . . ?
C10 C9 H9 121.1 . . ?
N2 C10 C9 123.9(5) . . ?
N2 C10 H10 118.1 . . ?
C9 C10 H10 118.1 . . ?
N2 C11 C7 121.1(5) . . ?
N2 C11 C12 118.0(5) . . ?
C7 C11 C12 120.9(5) . . ?
N1 C12 C4 120.0(5) . . ?
N1 C12 C11 118.6(5) . . ?
C4 C12 C11 121.4(5) . . ?
N4 C13 N3 112.4(5) . . ?
N4 C13 C14 121.7(5) . . ?
N3 C13 C14 125.8(5) . . ?
C15 C14 C19 120.2(5) . . ?
C15 C14 C13 115.0(6) . . ?
C19 C14 C13 124.8(5) . . ?
C14 C15 C16 121.2(6) . . ?
C14 C15 H15 119.4 . . ?
C16 C15 H15 119.4 . . ?
C17 C16 C15 119.3(7) . . ?
C17 C16 H16 120.3 . . ?
C15 C16 H16 120.3 . . ?
C16 C17 C18 120.5(6) . . ?
C16 C17 H17 119.7 . . ?
C18 C17 H17 119.7 . . ?
C17 C18 C19 120.7(6) . . ?
C17 C18 H18 119.7 . . ?
C19 C18 H18 119.7 . . ?
C18 C19 C14 118.1(6) . . ?
C18 C19 C20 116.9(5) . . ?
C14 C19 C20 124.2(5) . . ?
O2 C20 O1 120.8(6) . . ?
O2 C20 C19 120.5(5) . . ?
O1 C20 C19 118.6(5) . . ?
N5 C21 C22 123.6(7) . . ?
N5 C21 C23 117.9(7) . 2_877 ?
C22 C21 C23 118.3(6) . 2_877 ?
C23 C22 C21 119.6(5) . . ?
C23 C22 C24 119.0(6) . . ?
C21 C22 C24 121.4(6) . . ?
C22 C23 C21 122.1(6) . 2_877 ?
C22 C23 H23 118.9 . . ?
C21 C23 H23 118.9 2_877 . ?
O4 C24 O3 122.2(6) . . ?
O4 C24 C22 119.1(6) . . ?
O3 C24 C22 118.8(6) . . ?
C1 N1 C12 119.7(5) . . ?
C1 N1 Pb 120.1(4) . . ?
C12 N1 Pb 120.2(4) . . ?
C10 N2 C11 118.5(5) . . ?
C10 N2 Pb 122.0(4) . . ?
C11 N2 Pb 119.1(3) . . ?
C5 N3 C13 107.2(5) . . ?
C5 N3 H3A 126.4 . . ?
C13 N3 H3A 126.4 . . ?
C13 N4 C6 103.9(5) . . ?
C21 N5 H5A 120.0 . . ?
C21 N5 H5B 120.0 . . ?
H5A N5 H5B 120.0 . . ?
C20 O1 Pb 92.8(4) . 1_545 ?
C20 O2 Pb 93.6(3) . 1_545 ?
C24 O3 Pb 101.9(4) . . ?
O3 Pb O2 75.69(14) . 1_565 ?
O3 Pb O1 79.11(15) . 1_565 ?
O2 Pb O1 51.31(12) 1_565 1_565 ?
O3 Pb N1 101.43(16) . . ?
O2 Pb N1 74.72(14) 1_565 . ?
O1 Pb N1 124.51(14) 1_565 . ?
O3 Pb N2 142.75(15) . . ?
O2 Pb N2 67.54(13) 1_565 . ?
O1 Pb N2 82.54(14) 1_565 . ?
N1 Pb N2 63.83(14) . . ?

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 O1W 0.86 1.92 2.780(6) 177.4 1_545

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        25.93
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         0.688
_refine_diff_density_min         -1.031
_refine_diff_density_rms         0.147
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1578669'
_audit_update_record             
;
2017-10-08 deposited with the CCDC.
2018-04-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C48 H25 N8 O9 Pb2'
_chemical_formula_sum            'C48 H25 N8 O9 Pb2'
_chemical_formula_weight         1272.14

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/n  '
_symmetry_space_group_name_Hall  '-P 2yn '

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

_cell_length_a                   9.8473(7)
_cell_length_b                   10.8694(8)
_cell_length_c                   19.4576(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.6750(10)
_cell_angle_gamma                90.00
_cell_volume                     2053.0(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2546
_cell_measurement_theta_min      2.12
_cell_measurement_theta_max      2604

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.162
_exptl_crystal_size_mid          0.137
_exptl_crystal_size_min          0.040
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.058
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1210
_exptl_absorpt_coefficient_mu    8.263
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.273
_exptl_absorpt_correction_T_max  0.719
_exptl_absorpt_process_details   '(SADABS; Bruker, 2002)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            11065
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0478
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.12
_diffrn_reflns_theta_max         26.04
_reflns_number_total             4043
_reflns_number_gt                3174
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'SMART (Bruker, 2002)'
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_reduction        'SHELXS97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXS97 (Sheldrick, 1997)'
_computing_publication_material  SHELXTL

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0195P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4043
_refine_ls_number_parameters     307
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0278
_refine_ls_wR_factor_ref         0.0549
_refine_ls_wR_factor_gt          0.0497
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_restrained_S_all      1.004
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.8578(5) 0.2770(5) 0.9016(3) 0.0399(14) Uani 1 1 d . . .
H1 H 0.7810 0.3130 0.8749 0.048 Uiso 1 1 calc R . .
C2 C 0.9210(5) 0.3375(5) 0.9609(3) 0.0427(15) Uani 1 1 d . . .
H2 H 0.8862 0.4120 0.9739 0.051 Uiso 1 1 calc R . .
C3 C 1.0359(5) 0.2863(5) 1.0007(3) 0.0341(13) Uani 1 1 d . . .
H3 H 1.0802 0.3263 1.0405 0.041 Uiso 1 1 calc R . .
C4 C 1.0855(5) 0.1733(4) 0.9805(3) 0.0266(11) Uani 1 1 d . . .
C5 C 1.1991(5) 0.1061(4) 1.0183(3) 0.0256(11) Uani 1 1 d . . .
C6 C 1.2394(5) -0.0076(5) 0.9962(3) 0.0280(12) Uani 1 1 d . . .
C7 C 1.1707(5) -0.0629(4) 0.9336(3) 0.0285(11) Uani 1 1 d . . .
C8 C 1.2083(5) -0.1766(4) 0.9083(3) 0.0383(14) Uani 1 1 d . . .
H8 H 1.2831 -0.2200 0.9321 0.046 Uiso 1 1 calc R . .
C9 C 1.1340(6) -0.2223(5) 0.8486(3) 0.0425(14) Uani 1 1 d . . .
H9 H 1.1567 -0.2981 0.8314 0.051 Uiso 1 1 calc R . .
C10 C 1.0244(5) -0.1552(4) 0.8135(3) 0.0360(13) Uani 1 1 d . . .
H10 H 0.9745 -0.1879 0.7728 0.043 Uiso 1 1 calc R . .
C11 C 1.0574(5) 0.0001(4) 0.8953(2) 0.0246(11) Uani 1 1 d . . .
C12 C 1.0132(5) 0.1180(4) 0.9193(3) 0.0259(11) Uani 1 1 d . . .
C13 C 1.3742(5) 0.0331(4) 1.0921(3) 0.0270(12) Uani 1 1 d . . .
C14 C 1.4903(5) 0.0199(4) 1.1496(3) 0.0251(11) Uani 1 1 d . . .
C15 C 1.5830(5) -0.0759(4) 1.1427(3) 0.0335(12) Uani 1 1 d . . .
H15 H 1.5655 -0.1271 1.1039 0.040 Uiso 1 1 calc R . .
C16 C 1.6991(5) -0.0960(5) 1.1917(3) 0.0404(15) Uani 1 1 d . . .
H16 H 1.7582 -0.1606 1.1861 0.048 Uiso 1 1 calc R . .
C17 C 1.7275(5) -0.0198(5) 1.2494(3) 0.0376(14) Uani 1 1 d . . .
H17 H 1.8066 -0.0320 1.2823 0.045 Uiso 1 1 calc R . .
C18 C 1.6378(5) 0.0740(4) 1.2579(3) 0.0315(12) Uani 1 1 d . . .
H18 H 1.6575 0.1248 1.2967 0.038 Uiso 1 1 calc R . .
C19 C 1.5181(5) 0.0949(4) 1.2097(3) 0.0261(11) Uani 1 1 d . . .
C20 C 1.4273(5) 0.1957(5) 1.2272(2) 0.0275(11) Uani 1 1 d . . .
C21 C 1.0438(6) -0.0700(5) 0.5592(3) 0.0398(14) Uani 1 1 d . . .
C22 C 0.9371(5) 0.0148(5) 0.5591(3) 0.0320(12) Uani 1 1 d . . .
C23 C 0.8955(6) 0.0837(5) 0.4991(3) 0.0403(14) Uani 1 1 d . . .
H23 H 0.8248 0.1407 0.4983 0.048 Uiso 1 1 calc R . .
C24 C 0.8690(5) 0.0331(5) 0.6211(3) 0.0299(12) Uani 1 1 d . . .
N1 N 0.9013(4) 0.1708(4) 0.8813(2) 0.0310(10) Uani 1 1 d . . .
N2 N 0.9870(4) -0.0465(3) 0.8350(2) 0.0283(10) Uani 1 1 d . . .
N3 N 1.2862(4) 0.1304(4) 1.0793(2) 0.0283(10) Uani 1 1 d . . .
H3A H 1.2856 0.1950 1.1048 0.034 Uiso 1 1 calc R . .
N4 N 1.3480(4) -0.0520(4) 1.0421(2) 0.0319(10) Uani 1 1 d . . .
O1 O 1.3018(3) 0.1732(3) 1.22904(18) 0.0304(8) Uani 1 1 d . . .
O2 O 1.4829(3) 0.2990(3) 1.24348(18) 0.0320(8) Uani 1 1 d . . .
O3 O 0.9085(3) -0.0345(3) 0.67464(18) 0.0337(9) Uani 1 1 d . . .
O4 O 0.7775(4) 0.1139(3) 0.61985(18) 0.0372(9) Uani 1 1 d . . .
O5 O 1.0927(7) -0.1351(6) 0.6129(3) 0.0394(19) Uani 0.50 1 d P . .
H5A H 1.0498 -0.1203 0.6446 0.059 Uiso 0.50 1 calc PR . .
Pb Pb 0.797645(18) 0.072096(17) 0.762349(10) 0.02707(7) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.315(6) . ?
C1 C2 1.382(7) . ?
C1 H1 0.9300 . ?
C2 C3 1.376(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.402(6) . ?
C3 H3 0.9300 . ?
C4 C12 1.416(6) . ?
C4 C5 1.432(6) . ?
C5 N3 1.369(6) . ?
C5 C6 1.388(6) . ?
C6 N4 1.361(6) . ?
C6 C7 1.424(7) . ?
C7 C8 1.403(6) . ?
C7 C11 1.410(6) . ?
C8 C9 1.359(7) . ?
C8 H8 0.9300 . ?
C9 C10 1.384(6) . ?
C9 H9 0.9300 . ?
C10 N2 1.326(6) . ?
C10 H10 0.9300 . ?
C11 N2 1.357(6) . ?
C11 C12 1.455(6) . ?
C12 N1 1.347(6) . ?
C13 N4 1.336(6) . ?
C13 N3 1.363(6) . ?
C13 C14 1.467(6) . ?
C14 C15 1.407(6) . ?
C14 C19 1.413(7) . ?
C15 C16 1.378(7) . ?
C15 H15 0.9300 . ?
C16 C17 1.385(8) . ?
C16 H16 0.9300 . ?
C17 C18 1.377(7) . ?
C17 H17 0.9300 . ?
C18 C19 1.397(6) . ?
C18 H18 0.9300 . ?
C19 C20 1.489(6) . ?
C20 O2 1.266(5) . ?
C20 O1 1.266(5) . ?
C21 O5 1.287(8) . ?
C21 C23 1.376(7) 3_756 ?
C21 C22 1.398(7) . ?
C22 C23 1.389(7) . ?
C22 C24 1.490(7) . ?
C23 C21 1.376(7) 3_756 ?
C23 H23 0.9300 . ?
C24 O4 1.255(6) . ?
C24 O3 1.281(6) . ?
N1 Pb 2.599(4) . ?
N2 Pb 2.500(4) . ?
N3 H3A 0.8600 . ?
O2 Pb 2.377(3) 4_666 ?
O3 Pb 2.465(3) . ?
O5 H5A 0.8200 . ?
Pb O2 2.377(3) 4_565 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 123.1(5) . . ?
N1 C1 H1 118.5 . . ?
C2 C1 H1 118.5 . . ?
C3 C2 C1 119.3(5) . . ?
C3 C2 H2 120.4 . . ?
C1 C2 H2 120.4 . . ?
C2 C3 C4 119.3(5) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C3 C4 C12 117.3(4) . . ?
C3 C4 C5 125.6(5) . . ?
C12 C4 C5 117.0(4) . . ?
N3 C5 C6 105.7(4) . . ?
N3 C5 C4 131.9(4) . . ?
C6 C5 C4 122.4(4) . . ?
N4 C6 C5 110.3(4) . . ?
N4 C6 C7 128.3(4) . . ?
C5 C6 C7 121.4(4) . . ?
C8 C7 C11 118.4(4) . . ?
C8 C7 C6 123.8(4) . . ?
C11 C7 C6 117.9(4) . . ?
C9 C8 C7 119.1(5) . . ?
C9 C8 H8 120.5 . . ?
C7 C8 H8 120.5 . . ?
C8 C9 C10 119.5(5) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 H9 120.3 . . ?
N2 C10 C9 123.3(5) . . ?
N2 C10 H10 118.3 . . ?
C9 C10 H10 118.3 . . ?
N2 C11 C7 121.3(4) . . ?
N2 C11 C12 118.0(4) . . ?
C7 C11 C12 120.7(4) . . ?
N1 C12 C4 122.0(4) . . ?
N1 C12 C11 117.4(4) . . ?
C4 C12 C11 120.6(4) . . ?
N4 C13 N3 111.4(4) . . ?
N4 C13 C14 121.2(4) . . ?
N3 C13 C14 127.2(4) . . ?
C15 C14 C19 117.9(4) . . ?
C15 C14 C13 115.8(4) . . ?
C19 C14 C13 126.3(4) . . ?
C16 C15 C14 121.8(5) . . ?
C16 C15 H15 119.1 . . ?
C14 C15 H15 119.1 . . ?
C15 C16 C17 119.8(5) . . ?
C15 C16 H16 120.1 . . ?
C17 C16 H16 120.1 . . ?
C18 C17 C16 119.6(5) . . ?
C18 C17 H17 120.2 . . ?
C16 C17 H17 120.2 . . ?
C17 C18 C19 121.8(5) . . ?
C17 C18 H18 119.1 . . ?
C19 C18 H18 119.1 . . ?
C18 C19 C14 119.1(4) . . ?
C18 C19 C20 115.9(4) . . ?
C14 C19 C20 125.0(4) . . ?
O2 C20 O1 123.2(4) . . ?
O2 C20 C19 117.3(4) . . ?
O1 C20 C19 119.4(4) . . ?
O5 C21 C23 117.1(6) . 3_756 ?
O5 C21 C22 122.9(6) . . ?
C23 C21 C22 120.0(5) 3_756 . ?
C23 C22 C21 118.2(5) . . ?
C23 C22 C24 120.0(5) . . ?
C21 C22 C24 121.8(5) . . ?
C21 C23 C22 121.8(5) 3_756 . ?
C21 C23 H23 119.1 3_756 . ?
C22 C23 H23 119.1 . . ?
O4 C24 O3 122.4(5) . . ?
O4 C24 C22 119.8(5) . . ?
O3 C24 C22 117.8(5) . . ?
C1 N1 C12 119.1(4) . . ?
C1 N1 Pb 122.1(3) . . ?
C12 N1 Pb 118.4(3) . . ?
C10 N2 C11 118.5(4) . . ?
C10 N2 Pb 120.1(3) . . ?
C11 N2 Pb 121.4(3) . . ?
C13 N3 C5 107.1(4) . . ?
C13 N3 H3A 126.4 . . ?
C5 N3 H3A 126.4 . . ?
C13 N4 C6 105.4(4) . . ?
C20 O2 Pb 104.5(3) . 4_666 ?
C24 O3 Pb 100.6(3) . . ?
C21 O5 H5A 109.5 . . ?
O2 Pb O3 74.30(11) 4_565 . ?
O2 Pb N2 82.67(12) 4_565 . ?
O3 Pb N2 76.94(12) . . ?
O2 Pb N1 72.39(12) 4_565 . ?
O3 Pb N1 131.09(12) . . ?
N2 Pb N1 64.24(12) . . ?

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 O4 0.86 2.10 2.894(5) 153.0 4_666

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.04
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.912
_refine_diff_density_rms         0.129
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1578667'
_audit_update_record             
;
2017-10-08 deposited with the CCDC.
2018-04-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C48 H26 N9 O8 Pb2 '
_chemical_formula_sum            'C48 H26 N9 O8 Pb2 '
_chemical_formula_weight         1271.16

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'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/n  '
_symmetry_space_group_name_Hall  '-P 2yc'

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

_cell_length_a                   9.8904(14)
_cell_length_b                   11.1127(16)
_cell_length_c                   19.284(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.938(3)
_cell_angle_gamma                90.00
_cell_volume                     2073.7(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1750
_cell_measurement_theta_min      2.13
_cell_measurement_theta_max      26.10

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.233
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.039
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.036
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1210
_exptl_absorpt_coefficient_mu    8.179
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.397
_exptl_absorpt_correction_T_max  0.727
_exptl_absorpt_process_details   '(SADABS; Bruker, 2002)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            11163
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_sigmaI/netI    0.0665
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.13
_diffrn_reflns_theta_max         26.10
_reflns_number_total             4095
_reflns_number_gt                2906
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'SMART (Bruker, 2002)'
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_reduction        'SHELXS97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXS97 (Sheldrick, 1997)'
_computing_publication_material  SHELXTL

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0220P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4095
_refine_ls_number_parameters     311
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0365
_refine_ls_wR_factor_ref         0.0694
_refine_ls_wR_factor_gt          0.0616
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_restrained_S_all      0.984
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.8536(7) 0.2606(6) 0.9028(4) 0.0450(18) Uani 1 1 d . . .
H1 H 0.7721 0.2919 0.8760 0.054 Uiso 1 1 calc R . .
C2 C 0.9196(7) 0.3257(6) 0.9614(4) 0.052(2) Uani 1 1 d . . .
H2 H 0.8842 0.3989 0.9729 0.063 Uiso 1 1 calc R . .
C3 C 1.0388(6) 0.2790(6) 1.0021(4) 0.0444(19) Uani 1 1 d . . .
H3 H 1.0857 0.3204 1.0417 0.053 Uiso 1 1 calc R . .
C4 C 1.0888(6) 0.1690(5) 0.9834(3) 0.0324(15) Uani 1 1 d . . .
C5 C 1.2069(6) 0.1081(6) 1.0228(4) 0.0329(16) Uani 1 1 d . . .
C6 C 1.2495(6) -0.0017(6) 1.0024(4) 0.0334(16) Uani 1 1 d . . .
C7 C 1.1817(6) -0.0601(6) 0.9393(3) 0.0357(15) Uani 1 1 d . . .
C8 C 1.2211(7) -0.1698(6) 0.9150(4) 0.0482(19) Uani 1 1 d . . .
H8 H 1.2978 -0.2104 0.9405 0.058 Uiso 1 1 calc R . .
C9 C 1.1467(7) -0.2177(6) 0.8537(4) 0.053(2) Uani 1 1 d . . .
H9 H 1.1724 -0.2909 0.8369 0.063 Uiso 1 1 calc R . .
C10 C 1.0324(7) -0.1561(6) 0.8167(4) 0.0449(18) Uani 1 1 d . . .
H10 H 0.9824 -0.1899 0.7751 0.054 Uiso 1 1 calc R . .
C11 C 1.0625(6) -0.0032(6) 0.8991(3) 0.0326(15) Uani 1 1 d . . .
C12 C 1.0141(6) 0.1114(5) 0.9218(3) 0.0288(15) Uani 1 1 d . . .
C13 C 1.3872(6) 0.0435(6) 1.1007(3) 0.0318(15) Uani 1 1 d . . .
C14 C 1.5026(6) 0.0365(5) 1.1628(4) 0.0338(16) Uani 1 1 d . . .
C15 C 1.6024(7) -0.0515(6) 1.1605(4) 0.0465(19) Uani 1 1 d . . .
C16 C 1.7169(7) -0.0651(7) 1.2139(5) 0.055(2) Uani 1 1 d . . .
H16 H 1.7825 -0.1234 1.2102 0.066 Uiso 1 1 calc R . .
C17 C 1.7347(7) 0.0070(7) 1.2724(5) 0.052(2) Uani 1 1 d . . .
H17 H 1.8102 -0.0041 1.3096 0.063 Uiso 1 1 calc R . .
C18 C 1.6394(6) 0.0965(6) 1.2759(4) 0.0426(19) Uani 1 1 d . . .
H18 H 1.6541 0.1483 1.3146 0.051 Uiso 1 1 calc R . .
C19 C 1.5221(6) 0.1109(5) 1.2228(4) 0.0296(15) Uani 1 1 d . . .
C20 C 1.4250(6) 0.2080(6) 1.2350(3) 0.0315(15) Uani 1 1 d . . .
C21 C 0.9329(8) 0.1034(6) 0.5101(4) 0.052(2) Uani 1 1 d . . .
H21 H 0.8873 0.1743 0.5170 0.063 Uiso 1 1 calc R . .
C22 C 0.9384(6) 0.0115(6) 0.5592(3) 0.0346(16) Uani 1 1 d . . .
C23 C 1.0071(8) -0.0941(6) 0.5492(4) 0.049(2) Uani 1 1 d . . .
C24 C 0.8711(7) 0.0295(6) 0.6213(4) 0.0372(17) Uani 1 1 d . . .
N1 N 0.8978(5) 0.1579(5) 0.8822(3) 0.0398(14) Uani 1 1 d . . .
N2 N 0.9914(5) -0.0525(5) 0.8377(3) 0.0381(13) Uani 1 1 d . . .
N3 N 1.2941(5) 0.1357(4) 1.0853(3) 0.0344(13) Uani 1 1 d . . .
H3A H 1.2912 0.1993 1.1103 0.041 Uiso 1 1 calc R . .
N4 N 1.3637(5) -0.0414(5) 1.0507(3) 0.0350(13) Uani 1 1 d . . .
O1 O 1.4775(4) 0.3116(4) 1.2489(2) 0.0384(11) Uani 1 1 d . . .
O2 O 1.3008(4) 0.1856(4) 1.2335(2) 0.0396(11) Uani 1 1 d . . .
O3 O 0.7854(4) 0.1131(4) 0.6201(2) 0.0440(12) Uani 1 1 d . . .
O4 O 0.9005(4) -0.0421(4) 0.6730(2) 0.0406(11) Uani 1 1 d . . .
Pb Pb 0.79504(2) 0.05904(2) 0.760310(14) 0.03623(9) Uani 1 1 d . . .
N5 N 1.0163(16) -0.1821(12) 0.5931(7) 0.096(6) Uani 0.50 1 d P . .
H5A H 0.9807 -0.1748 0.6300 0.115 Uiso 0.50 1 d PR . .
H5B H 1.0588 -0.2473 0.5864 0.115 Uiso 0.50 1 d PR . .
H15 H 1.590(5) -0.092(4) 1.119(3) 0.007(14) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.312(8) . ?
C1 C2 1.387(9) . ?
C1 H1 0.9300 . ?
C2 C3 1.376(8) . ?
C2 H2 0.9300 . ?
C3 C4 1.394(8) . ?
C3 H3 0.9300 . ?
C4 C12 1.415(8) . ?
C4 C5 1.426(8) . ?
C5 N3 1.364(7) . ?
C5 C6 1.374(8) . ?
C6 N4 1.380(7) . ?
C6 C7 1.420(8) . ?
C7 C8 1.390(9) . ?
C7 C11 1.419(8) . ?
C8 C9 1.365(9) . ?
C8 H8 0.9300 . ?
C9 C10 1.386(8) . ?
C9 H9 0.9300 . ?
C10 N2 1.312(8) . ?
C10 H10 0.9300 . ?
C11 N2 1.361(7) . ?
C11 C12 1.459(8) . ?
C12 N1 1.345(7) . ?
C13 N4 1.334(8) . ?
C13 N3 1.369(7) . ?
C13 C14 1.476(8) . ?
C14 C15 1.396(9) . ?
C14 C19 1.403(9) . ?
C15 C16 1.373(9) . ?
C15 H15 0.90(5) . ?
C16 C17 1.365(11) . ?
C16 H16 0.9300 . ?
C17 C18 1.382(9) . ?
C17 H17 0.9300 . ?
C18 C19 1.389(8) . ?
C18 H18 0.9300 . ?
C19 C20 1.495(8) . ?
C20 O2 1.248(7) . ?
C20 O1 1.269(7) . ?
C21 C22 1.386(9) . ?
C21 C23 1.397(10) 3_756 ?
C21 H21 0.9300 . ?
C22 C23 1.390(9) . ?
C22 C24 1.498(9) . ?
C23 N5 1.285(13) . ?
C23 C21 1.397(10) 3_756 ?
C24 O3 1.255(7) . ?
C24 O4 1.262(7) . ?
N1 Pb 2.603(5) . ?
N2 Pb 2.517(5) . ?
N3 H3A 0.8600 . ?
O1 Pb 2.352(4) 4_666 ?
O3 Pb 2.751(5) . ?
O4 Pb 2.432(4) . ?
Pb O1 2.352(4) 4_565 ?
N5 H5A 0.8600 . ?
N5 H5B 0.8600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 124.8(6) . . ?
N1 C1 H1 117.6 . . ?
C2 C1 H1 117.6 . . ?
C3 C2 C1 118.1(6) . . ?
C3 C2 H2 121.0 . . ?
C1 C2 H2 121.0 . . ?
C2 C3 C4 119.5(6) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
C3 C4 C12 117.5(6) . . ?
C3 C4 C5 125.0(6) . . ?
C12 C4 C5 117.4(6) . . ?
N3 C5 C6 106.1(5) . . ?
N3 C5 C4 131.5(6) . . ?
C6 C5 C4 122.3(6) . . ?
C5 C6 N4 110.3(6) . . ?
C5 C6 C7 122.2(6) . . ?
N4 C6 C7 127.4(6) . . ?
C8 C7 C11 117.8(6) . . ?
C8 C7 C6 125.0(6) . . ?
C11 C7 C6 117.1(6) . . ?
C9 C8 C7 119.7(6) . . ?
C9 C8 H8 120.2 . . ?
C7 C8 H8 120.2 . . ?
C8 C9 C10 119.3(7) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 H9 120.4 . . ?
N2 C10 C9 123.1(6) . . ?
N2 C10 H10 118.4 . . ?
C9 C10 H10 118.4 . . ?
N2 C11 C7 121.1(6) . . ?
N2 C11 C12 118.1(6) . . ?
C7 C11 C12 120.8(6) . . ?
N1 C12 C4 122.7(6) . . ?
N1 C12 C11 117.3(5) . . ?
C4 C12 C11 120.0(5) . . ?
N4 C13 N3 111.3(5) . . ?
N4 C13 C14 122.6(5) . . ?
N3 C13 C14 126.0(6) . . ?
C15 C14 C19 117.5(6) . . ?
C15 C14 C13 116.4(6) . . ?
C19 C14 C13 126.2(5) . . ?
C16 C15 C14 122.2(7) . . ?
C16 C15 H15 123(3) . . ?
C14 C15 H15 114(3) . . ?
C17 C16 C15 120.1(7) . . ?
C17 C16 H16 120.0 . . ?
C15 C16 H16 120.0 . . ?
C16 C17 C18 119.3(7) . . ?
C16 C17 H17 120.3 . . ?
C18 C17 H17 120.3 . . ?
C17 C18 C19 121.4(7) . . ?
C17 C18 H18 119.3 . . ?
C19 C18 H18 119.3 . . ?
C18 C19 C14 119.5(6) . . ?
C18 C19 C20 115.6(6) . . ?
C14 C19 C20 124.9(5) . . ?
O2 C20 O1 122.9(6) . . ?
O2 C20 C19 120.9(6) . . ?
O1 C20 C19 116.1(5) . . ?
C22 C21 C23 122.8(6) . 3_756 ?
C22 C21 H21 118.6 . . ?
C23 C21 H21 118.6 3_756 . ?
C21 C22 C23 118.6(6) . . ?
C21 C22 C24 119.1(6) . . ?
C23 C22 C24 122.4(6) . . ?
N5 C23 C22 121.4(9) . . ?
N5 C23 C21 119.9(8) . 3_756 ?
C22 C23 C21 118.7(7) . 3_756 ?
O3 C24 O4 121.7(7) . . ?
O3 C24 C22 119.7(6) . . ?
O4 C24 C22 118.6(6) . . ?
C1 N1 C12 117.5(6) . . ?
C1 N1 Pb 123.2(4) . . ?
C12 N1 Pb 118.6(4) . . ?
C10 N2 C11 119.0(6) . . ?
C10 N2 Pb 120.0(4) . . ?
C11 N2 Pb 120.9(4) . . ?
C5 N3 C13 107.3(5) . . ?
C5 N3 H3A 126.4 . . ?
C13 N3 H3A 126.4 . . ?
C13 N4 C6 104.9(5) . . ?
C20 O1 Pb 106.6(4) . 4_666 ?
C24 O3 Pb 86.3(4) . . ?
C24 O4 Pb 101.1(4) . . ?
O1 Pb O4 76.75(15) 4_565 . ?
O1 Pb N2 80.99(16) 4_565 . ?
O4 Pb N2 78.10(16) . . ?
O1 Pb N1 70.28(16) 4_565 . ?
O4 Pb N1 132.61(15) . . ?
N2 Pb N1 64.11(17) . . ?
O1 Pb O3 69.30(14) 4_565 . ?
O4 Pb O3 49.73(14) . . ?
N2 Pb O3 123.75(15) . . ?
N1 Pb O3 136.27(16) . . ?
C23 N5 H5A 119.2 . . ?
C23 N5 H5B 120.8 . . ?
H5A N5 H5B 120.0 . . ?

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 O3 0.86 2.09 2.876(7) 150.8 4_666

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        26.10
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.988
_refine_diff_density_min         -0.838
_refine_diff_density_rms         0.141
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1578666'
_audit_update_record             
;
2017-10-08 deposited with the CCDC.
2018-04-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H15 N5 O4 Pb'
_chemical_formula_sum            'C26 H15 N5 O4 Pb'
_chemical_formula_weight         668.62

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

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1   '
_symmetry_space_group_name_Hall  -P1

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

_cell_length_a                   9.4750(5)
_cell_length_b                   10.0435(5)
_cell_length_c                   12.8759(7)
_cell_angle_alpha                80.1830(10)
_cell_angle_beta                 68.8510(10)
_cell_angle_gamma                78.4320(10)
_cell_volume                     1113.08(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4332
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      26.11

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.493
_exptl_crystal_size_mid          0.245
_exptl_crystal_size_min          0.169
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.995
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             640
_exptl_absorpt_coefficient_mu    7.625
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8617
_exptl_absorpt_correction_T_max  0.9015
_exptl_absorpt_process_details   '(SADABS; Bruker, 2002)'


_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       dtprofit.ref
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            6179
_diffrn_reflns_av_R_equivalents  0.0182
_diffrn_reflns_av_sigmaI/netI    0.0348
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.71
_diffrn_reflns_theta_max         26.14
_reflns_number_total             4357
_reflns_number_gt                4077
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'SMART (Bruker, 2002)'
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_reduction        'SAINT '
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXTL

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0303P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4357
_refine_ls_number_parameters     325
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0254
_refine_ls_R_factor_gt           0.0228
_refine_ls_wR_factor_ref         0.0554
_refine_ls_wR_factor_gt          0.0543
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.051
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb Pb 0.622084(14) 0.443922(12) 0.360826(11) 0.02369(6) Uani 1 1 d . . .
C1 C 0.9589(5) 0.3849(4) 0.4119(3) 0.0348(9) Uani 1 1 d . . .
H1 H 0.8881 0.4047 0.4815 0.042 Uiso 1 1 calc R . .
C2 C 1.1137(5) 0.3563(5) 0.4000(4) 0.0386(10) Uani 1 1 d . . .
H2 H 1.1452 0.3587 0.4601 0.046 Uiso 1 1 calc R . .
C3 C 1.2183(5) 0.3250(4) 0.2992(4) 0.0346(9) Uani 1 1 d . . .
H3 H 1.3221 0.3058 0.2899 0.041 Uiso 1 1 calc R . .
C4 C 1.1689(4) 0.3219(4) 0.2091(3) 0.0252(8) Uani 1 1 d . . .
C5 C 1.2676(4) 0.2903(4) 0.1003(3) 0.0251(8) Uani 1 1 d . . .
C6 C 1.2100(4) 0.2943(3) 0.0160(3) 0.0216(7) Uani 1 1 d . . .
C7 C 1.0502(4) 0.3264(3) 0.0302(3) 0.0205(7) Uani 1 1 d . . .
C8 C 0.9862(4) 0.3302(4) -0.0535(3) 0.0241(7) Uani 1 1 d . . .
H8 H 1.0486 0.3095 -0.1251 0.029 Uiso 1 1 calc R . .
C9 C 0.8318(4) 0.3644(4) -0.0286(3) 0.0273(8) Uani 1 1 d . . .
H9 H 0.7874 0.3662 -0.0826 0.033 Uiso 1 1 calc R . .
C10 C 0.7415(4) 0.3968(3) 0.0790(3) 0.0246(7) Uani 1 1 d . . .
H10 H 0.6365 0.4213 0.0947 0.030 Uiso 1 1 calc R . .
C11 C 0.9504(4) 0.3575(3) 0.1375(3) 0.0212(7) Uani 1 1 d . . .
C12 C 1.0097(4) 0.3545(4) 0.2277(3) 0.0234(7) Uani 1 1 d . . .
C13 C 1.4604(4) 0.2377(4) -0.0441(3) 0.0256(8) Uani 1 1 d . . .
C14 C 1.6168(4) 0.1859(4) -0.1147(3) 0.0263(8) Uani 1 1 d . . .
C15 C 1.7000(4) 0.0852(4) -0.0603(4) 0.0338(9) Uani 1 1 d . . .
H15 H 1.6545 0.0560 0.0150 0.041 Uiso 1 1 calc R . .
C16 C 1.8474(5) 0.0291(4) -0.1166(4) 0.0439(11) Uani 1 1 d . . .
H16 H 1.9030 -0.0340 -0.0786 0.053 Uiso 1 1 calc R . .
C17 C 1.9126(5) 0.0669(5) -0.2297(5) 0.0549(14) Uani 1 1 d . . .
H17 H 2.0110 0.0264 -0.2686 0.066 Uiso 1 1 calc R . .
C18 C 1.8325(5) 0.1644(5) -0.2852(4) 0.0458(11) Uani 1 1 d . . .
H18 H 1.8773 0.1886 -0.3616 0.055 Uiso 1 1 calc R . .
C19 C 1.6852(4) 0.2273(4) -0.2287(3) 0.0291(8) Uani 1 1 d . . .
C20 C 1.6135(4) 0.3430(4) -0.2941(3) 0.0279(8) Uani 1 1 d . . .
C21 C 0.6773(4) 0.7288(4) 0.3746(3) 0.0238(7) Uani 1 1 d . . .
C22 C 0.6710(4) 0.8818(4) 0.3655(3) 0.0249(8) Uani 1 1 d . . .
C23 C 0.6409(6) 0.9675(4) 0.2772(4) 0.0417(11) Uani 1 1 d . . .
H23 H 0.6250 0.9316 0.2211 0.050 Uiso 1 1 calc R . .
C24 C 0.6347(6) 1.1061(4) 0.2731(4) 0.0465(12) Uani 1 1 d . . .
H24 H 0.6112 1.1623 0.2144 0.056 Uiso 1 1 calc R . .
C25 C 0.6882(5) 1.0818(4) 0.4345(4) 0.0370(10) Uani 1 1 d . . .
H25 H 0.7042 1.1205 0.4892 0.044 Uiso 1 1 calc R . .
C26 C 0.6942(4) 0.9425(4) 0.4457(3) 0.0299(8) Uani 1 1 d . . .
H26 H 0.7138 0.8891 0.5069 0.036 Uiso 1 1 calc R . .
N1 N 0.9083(4) 0.3852(3) 0.3292(3) 0.0279(7) Uani 1 1 d . . .
N2 N 0.7975(3) 0.3945(3) 0.1599(3) 0.0228(6) Uani 1 1 d . . .
N3 N 1.4247(3) 0.2533(3) 0.0629(3) 0.0285(7) Uani 1 1 d . . .
N4 N 1.3343(3) 0.2608(3) -0.0767(3) 0.0244(6) Uani 1 1 d . . .
H4 H 1.3331 0.2553 -0.1423 0.029 Uiso 1 1 calc R . .
N5 N 0.6604(4) 1.1643(3) 0.3488(3) 0.0397(9) Uani 1 1 d . . .
O1 O 1.5329(3) 0.4432(3) -0.2420(2) 0.0320(6) Uani 1 1 d . . .
O2 O 1.6397(3) 0.3347(3) -0.3949(2) 0.0408(7) Uani 1 1 d . . .
O3 O 0.6570(3) 0.6619(3) 0.4675(2) 0.0316(6) Uani 1 1 d . . .
O4 O 0.7033(3) 0.6775(2) 0.2844(2) 0.0279(6) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb O1 2.478(3) 2_765 ?
Pb O4 2.541(2) . ?
Pb N1 2.552(3) . ?
Pb N2 2.589(3) . ?
Pb N5 2.782(3) 1_545 ?
C1 N1 1.315(5) . ?
C1 C2 1.394(6) . ?
C1 H1 0.9300 . ?
C2 C3 1.361(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.405(5) . ?
C3 H3 0.9300 . ?
C4 C12 1.417(5) . ?
C4 C5 1.423(5) . ?
C5 C6 1.371(5) . ?
C5 N3 1.381(5) . ?
C6 N4 1.375(5) . ?
C6 C7 1.434(5) . ?
C7 C8 1.406(5) . ?
C7 C11 1.410(5) . ?
C8 C9 1.363(5) . ?
C8 H8 0.9300 . ?
C9 C10 1.395(5) . ?
C9 H9 0.9300 . ?
C10 N2 1.325(4) . ?
C10 H10 0.9300 . ?
C11 N2 1.356(4) . ?
C11 C12 1.456(5) . ?
C12 N1 1.356(5) . ?
C13 N3 1.325(5) . ?
C13 N4 1.369(5) . ?
C13 C14 1.474(5) . ?
C14 C19 1.401(6) . ?
C14 C15 1.404(5) . ?
C15 C16 1.374(6) . ?
C15 H15 0.9300 . ?
C16 C17 1.379(7) . ?
C16 H16 0.9300 . ?
C17 C18 1.380(6) . ?
C17 H17 0.9300 . ?
C18 C19 1.395(5) . ?
C18 H18 0.9300 . ?
C19 C20 1.512(5) . ?
C20 O2 1.244(5) . ?
C20 O1 1.265(4) . ?
C21 O3 1.238(4) . ?
C21 O4 1.273(4) . ?
C21 C22 1.512(5) . ?
C22 C23 1.384(6) . ?
C22 C26 1.385(5) . ?
C23 C24 1.374(6) . ?
C23 H23 0.9300 . ?
C24 N5 1.332(6) . ?
C24 H24 0.9300 . ?
C25 N5 1.336(6) . ?
C25 C26 1.373(5) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
N4 H4 0.8600 . ?
N5 Pb 2.782(3) 1_565 ?
O1 Pb 2.478(3) 2_765 ?

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 Pb O4 73.28(8) 2_765 . ?
O1 Pb N1 134.65(10) 2_765 . ?
O4 Pb N1 79.79(9) . . ?
O1 Pb N2 75.93(9) 2_765 . ?
O4 Pb N2 80.33(9) . . ?
N1 Pb N2 63.92(9) . . ?
O1 Pb N5 106.74(10) 2_765 1_545 ?
O4 Pb N5 150.99(10) . 1_545 ?
N1 Pb N5 80.75(10) . 1_545 ?
N2 Pb N5 71.84(10) . 1_545 ?
N1 C1 C2 122.9(4) . . ?
N1 C1 H1 118.5 . . ?
C2 C1 H1 118.5 . . ?
C3 C2 C1 119.1(4) . . ?
C3 C2 H2 120.4 . . ?
C1 C2 H2 120.4 . . ?
C2 C3 C4 119.7(4) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C3 C4 C12 117.6(3) . . ?
C3 C4 C5 124.6(3) . . ?
C12 C4 C5 117.8(3) . . ?
C6 C5 N3 110.8(3) . . ?
C6 C5 C4 120.8(3) . . ?
N3 C5 C4 128.4(3) . . ?
C5 C6 N4 105.9(3) . . ?
C5 C6 C7 123.8(3) . . ?
N4 C6 C7 130.4(3) . . ?
C8 C7 C11 118.1(3) . . ?
C8 C7 C6 125.6(3) . . ?
C11 C7 C6 116.3(3) . . ?
C9 C8 C7 119.3(3) . . ?
C9 C8 H8 120.3 . . ?
C7 C8 H8 120.3 . . ?
C8 C9 C10 119.0(3) . . ?
C8 C9 H9 120.5 . . ?
C10 C9 H9 120.5 . . ?
N2 C10 C9 123.4(3) . . ?
N2 C10 H10 118.3 . . ?
C9 C10 H10 118.3 . . ?
N2 C11 C7 121.7(3) . . ?
N2 C11 C12 117.7(3) . . ?
C7 C11 C12 120.6(3) . . ?
N1 C12 C4 121.3(3) . . ?
N1 C12 C11 118.0(3) . . ?
C4 C12 C11 120.7(3) . . ?
N3 C13 N4 112.4(3) . . ?
N3 C13 C14 122.6(3) . . ?
N4 C13 C14 124.7(3) . . ?
C19 C14 C15 119.0(3) . . ?
C19 C14 C13 125.6(3) . . ?
C15 C14 C13 115.4(4) . . ?
C16 C15 C14 121.1(4) . . ?
C16 C15 H15 119.5 . . ?
C14 C15 H15 119.5 . . ?
C15 C16 C17 119.7(4) . . ?
C15 C16 H16 120.2 . . ?
C17 C16 H16 120.2 . . ?
C16 C17 C18 120.2(4) . . ?
C16 C17 H17 119.9 . . ?
C18 C17 H17 119.9 . . ?
C17 C18 C19 121.0(4) . . ?
C17 C18 H18 119.5 . . ?
C19 C18 H18 119.5 . . ?
C18 C19 C14 118.8(4) . . ?
C18 C19 C20 117.0(4) . . ?
C14 C19 C20 124.1(3) . . ?
O2 C20 O1 124.7(4) . . ?
O2 C20 C19 118.4(3) . . ?
O1 C20 C19 116.9(3) . . ?
O3 C21 O4 124.3(3) . . ?
O3 C21 C22 118.9(3) . . ?
O4 C21 C22 116.8(3) . . ?
C23 C22 C26 117.1(3) . . ?
C23 C22 C21 121.6(3) . . ?
C26 C22 C21 121.3(3) . . ?
C24 C23 C22 119.5(4) . . ?
C24 C23 H23 120.2 . . ?
C22 C23 H23 120.2 . . ?
N5 C24 C23 123.5(4) . . ?
N5 C24 H24 118.2 . . ?
C23 C24 H24 118.2 . . ?
N5 C25 C26 123.2(4) . . ?
N5 C25 H25 118.4 . . ?
C26 C25 H25 118.4 . . ?
C25 C26 C22 119.7(4) . . ?
C25 C26 H26 120.1 . . ?
C22 C26 H26 120.1 . . ?
C1 N1 C12 119.3(3) . . ?
C1 N1 Pb 119.9(3) . . ?
C12 N1 Pb 120.8(2) . . ?
C10 N2 C11 118.4(3) . . ?
C10 N2 Pb 121.9(2) . . ?
C11 N2 Pb 119.6(2) . . ?
C13 N3 C5 104.4(3) . . ?
C13 N4 C6 106.5(3) . . ?
C13 N4 H4 126.8 . . ?
C6 N4 H4 126.8 . . ?
C24 N5 C25 116.9(3) . . ?
C24 N5 Pb 125.8(3) . 1_565 ?
C25 N5 Pb 116.7(3) . 1_565 ?
C20 O1 Pb 102.9(2) . 2_765 ?
C21 O4 Pb 101.2(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
N4 H4 O4 0.86 1.97 2.774(4) 156.3 2_765

_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.860
_refine_diff_density_min         -1.918
_refine_diff_density_rms         0.114
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 1578668'
_audit_update_record             
;
2017-10-08 deposited with the CCDC.
2018-04-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H13 N4 O4 Pb'
_chemical_formula_sum            'C24 H13 N4 O4 Pb'
_chemical_formula_weight         628.57

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/n  '
_symmetry_space_group_name_Hall  '-P 2yc'

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

_cell_length_a                   9.8725(5)
_cell_length_b                   10.8203(5)
_cell_length_c                   19.3515(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.4280(10)
_cell_angle_gamma                90.00
_cell_volume                     2033.05(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6128
_cell_measurement_theta_min      2.14
_cell_measurement_theta_max      26.38

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.187
_exptl_crystal_size_mid          0.143
_exptl_crystal_size_min          0.045
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.054
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1196
_exptl_absorpt_coefficient_mu    8.341
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.249
_exptl_absorpt_correction_T_max  0.687
_exptl_absorpt_process_details   '(SADABS; Bruker, 2002)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            11347
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_av_sigmaI/netI    0.0271
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.14
_diffrn_reflns_theta_max         26.38
_reflns_number_total             4167
_reflns_number_gt                3736
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'SMART (Bruker, 2002)'
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_reduction        'SHELXS97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXS97 (Sheldrick, 1997)'
_computing_publication_material  SHELXTL
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0326P)²+0.4974P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4167
_refine_ls_number_parameters     298
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0267
_refine_ls_R_factor_gt           0.0225
_refine_ls_wR_factor_ref         0.0560
_refine_ls_wR_factor_gt          0.0544
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1455(4) 0.2742(3) 0.59793(19) 0.0263(8) Uani 1 1 d . . .
H1 H 0.2245 0.3091 0.6241 0.032 Uiso 1 1 calc R . .
C2 C 0.0782(4) 0.3365(4) 0.5382(2) 0.0287(9) Uani 1 1 d . . .
H2 H 0.1114 0.4121 0.5256 0.034 Uiso 1 1 calc R . .
C3 C -0.0375(4) 0.2851(3) 0.49828(19) 0.0248(8) Uani 1 1 d . . .
H3 H -0.0833 0.3251 0.4583 0.030 Uiso 1 1 calc R . .
C4 C -0.0854(3) 0.1708(3) 0.51896(18) 0.0178(7) Uani 1 1 d . . .
C5 C -0.2005(4) 0.1032(3) 0.48126(19) 0.0187(7) Uani 1 1 d . . .
C6 C -0.2411(3) -0.0102(3) 0.50341(18) 0.0192(7) Uani 1 1 d . . .
C7 C -0.1705(4) -0.0668(3) 0.56618(19) 0.0196(7) Uani 1 1 d . . .
C8 C -0.2081(4) -0.1806(3) 0.5915(2) 0.0267(8) Uani 1 1 d . . .
H8 H -0.2828 -0.2244 0.5673 0.032 Uiso 1 1 calc R . .
C9 C -0.1328(4) -0.2264(3) 0.6528(2) 0.0300(9) Uani 1 1 d . . .
H9 H -0.1558 -0.3021 0.6702 0.036 Uiso 1 1 calc R . .
C10 C -0.0223(4) -0.1593(3) 0.6887(2) 0.0255(8) Uani 1 1 d . . .
H10 H 0.0271 -0.1914 0.7303 0.031 Uiso 1 1 calc R . .
C11 C -0.0560(3) -0.0044(3) 0.60515(18) 0.0172(7) Uani 1 1 d . . .
C12 C -0.0127(3) 0.1149(3) 0.58022(18) 0.0176(7) Uani 1 1 d . . .
C13 C -0.3783(3) 0.0313(3) 0.40672(18) 0.0185(7) Uani 1 1 d . . .
C14 C -0.4955(3) 0.0195(3) 0.34792(19) 0.0185(7) Uani 1 1 d . . .
C15 C -0.5908(4) -0.0732(3) 0.3555(2) 0.0225(8) Uani 1 1 d . . .
H15 H -0.5742 -0.1245 0.3946 0.027 Uiso 1 1 calc R . .
C16 C -0.7095(4) -0.0900(3) 0.3057(2) 0.0256(8) Uani 1 1 d . . .
H16 H -0.7709 -0.1528 0.3113 0.031 Uiso 1 1 calc R . .
C17 C -0.7366(4) -0.0134(4) 0.2477(2) 0.0266(8) Uani 1 1 d . . .
H17 H -0.8167 -0.0235 0.2146 0.032 Uiso 1 1 calc R . .
C18 C -0.6443(4) 0.0778(3) 0.2393(2) 0.0239(8) Uani 1 1 d . . .
H18 H -0.6631 0.1289 0.2002 0.029 Uiso 1 1 calc R . .
C19 C -0.5227(4) 0.0959(3) 0.2880(2) 0.0193(7) Uani 1 1 d . . .
C20 C -0.4277(3) 0.1958(3) 0.27033(17) 0.0179(7) Uani 1 1 d . . .
C21 C -0.0914(5) -0.0962(4) 1.0008(2) 0.0385(11) Uani 1 1 d . . .
H21 H -0.1530 -0.1611 1.0012 0.046 Uiso 1 1 calc R . .
C22 C -0.0278(5) -0.0795(4) 0.9433(2) 0.0379(11) Uani 1 1 d . . .
H22 H -0.0471 -0.1333 0.9053 0.045 Uiso 1 1 calc R . .
C23 C 0.0636(4) 0.0160(3) 0.94176(19) 0.0225(8) Uani 1 1 d . . .
C24 C 0.1315(4) 0.0350(3) 0.87864(19) 0.0196(7) Uani 1 1 d . . .
N1 N 0.1009(3) 0.1671(3) 0.61882(15) 0.0212(6) Uani 1 1 d . . .
N2 N 0.0161(3) -0.0504(3) 0.66582(16) 0.0194(6) Uani 1 1 d . . .
N3 N -0.2890(3) 0.1281(3) 0.41988(15) 0.0181(6) Uani 1 1 d . . .
H3A H -0.2884 0.1930 0.3943 0.022 Uiso 1 1 calc R . .
N4 N -0.3514(3) -0.0549(3) 0.45643(17) 0.0214(7) Uani 1 1 d . . .
O1 O -0.3045(2) 0.1720(2) 0.27002(13) 0.0217(5) Uani 1 1 d . . .
O2 O -0.4822(2) 0.3009(2) 0.25478(12) 0.0209(5) Uani 1 1 d . . .
O3 O 0.2199(3) 0.1193(2) 0.88019(13) 0.0245(6) Uani 1 1 d . . .
O4 O 0.0960(3) -0.0354(2) 0.82682(13) 0.0230(5) Uani 1 1 d . . .
Pb Pb 0.205311(12) 0.070079(11) 0.739331(6) 0.01759(6) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.328(4) . ?
C1 C2 1.397(5) . ?
C1 H1 0.9300 . ?
C2 C3 1.376(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.408(5) . ?
C3 H3 0.9300 . ?
C4 C12 1.406(5) . ?
C4 C5 1.435(5) . ?
C5 N3 1.368(4) . ?
C5 C6 1.383(5) . ?
C6 N4 1.373(4) . ?
C6 C7 1.425(5) . ?
C7 C8 1.400(5) . ?
C7 C11 1.412(5) . ?
C8 C9 1.373(5) . ?
C8 H8 0.9300 . ?
C9 C10 1.387(5) . ?
C9 H9 0.9300 . ?
C10 N2 1.337(4) . ?
C10 H10 0.9300 . ?
C11 N2 1.352(4) . ?
C11 C12 1.469(5) . ?
C12 N1 1.353(4) . ?
C13 N4 1.331(4) . ?
C13 N3 1.363(4) . ?
C13 C14 1.475(5) . ?
C14 C15 1.400(5) . ?
C14 C19 1.410(5) . ?
C15 C16 1.388(5) . ?
C15 H15 0.9300 . ?
C16 C17 1.381(6) . ?
C16 H16 0.9300 . ?
C17 C18 1.372(5) . ?
C17 H17 0.9300 . ?
C18 C19 1.399(5) . ?
C18 H18 0.9300 . ?
C19 C20 1.511(5) . ?
C20 O1 1.244(4) . ?
C20 O2 1.271(4) . ?
C21 C22 1.386(6) . ?
C21 C23 1.397(5) 3_557 ?
C21 H21 0.9300 . ?
C22 C23 1.376(5) . ?
C22 H22 0.9300 . ?
C23 C21 1.397(5) 3_557 ?
C23 C24 1.510(5) . ?
C24 O4 1.257(4) . ?
C24 O3 1.259(4) . ?
N1 Pb 2.595(3) . ?
N2 Pb 2.500(3) . ?
N3 H3A 0.8600 . ?
O2 Pb 2.380(2) 4_565 ?
O3 Pb 2.755(3) . ?
O4 Pb 2.448(3) . ?
Pb O2 2.380(2) 4_666 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 122.6(3) . . ?
N1 C1 H1 118.7 . . ?
C2 C1 H1 118.7 . . ?
C3 C2 C1 119.4(4) . . ?
C3 C2 H2 120.3 . . ?
C1 C2 H2 120.3 . . ?
C2 C3 C4 118.9(3) . . ?
C2 C3 H3 120.6 . . ?
C4 C3 H3 120.6 . . ?
C12 C4 C3 118.1(3) . . ?
C12 C4 C5 116.5(3) . . ?
C3 C4 C5 125.4(3) . . ?
N3 C5 C6 105.6(3) . . ?
N3 C5 C4 131.6(3) . . ?
C6 C5 C4 122.8(3) . . ?
N4 C6 C5 110.3(3) . . ?
N4 C6 C7 128.3(3) . . ?
C5 C6 C7 121.4(3) . . ?
C8 C7 C11 118.1(3) . . ?
C8 C7 C6 123.9(3) . . ?
C11 C7 C6 118.1(3) . . ?
C9 C8 C7 119.0(3) . . ?
C9 C8 H8 120.5 . . ?
C7 C8 H8 120.5 . . ?
C8 C9 C10 119.8(3) . . ?
C8 C9 H9 120.1 . . ?
C10 C9 H9 120.1 . . ?
N2 C10 C9 122.7(3) . . ?
N2 C10 H10 118.7 . . ?
C9 C10 H10 118.7 . . ?
N2 C11 C7 122.2(3) . . ?
N2 C11 C12 118.0(3) . . ?
C7 C11 C12 119.8(3) . . ?
N1 C12 C4 122.1(3) . . ?
N1 C12 C11 116.5(3) . . ?
C4 C12 C11 121.4(3) . . ?
N4 C13 N3 111.4(3) . . ?
N4 C13 C14 121.5(3) . . ?
N3 C13 C14 127.0(3) . . ?
C15 C14 C19 118.3(3) . . ?
C15 C14 C13 115.5(3) . . ?
C19 C14 C13 126.1(3) . . ?
C16 C15 C14 121.3(4) . . ?
C16 C15 H15 119.3 . . ?
C14 C15 H15 119.3 . . ?
C17 C16 C15 120.0(3) . . ?
C17 C16 H16 120.0 . . ?
C15 C16 H16 120.0 . . ?
C18 C17 C16 119.5(4) . . ?
C18 C17 H17 120.2 . . ?
C16 C17 H17 120.2 . . ?
C17 C18 C19 121.9(4) . . ?
C17 C18 H18 119.1 . . ?
C19 C18 H18 119.1 . . ?
C18 C19 C14 118.9(3) . . ?
C18 C19 C20 116.1(3) . . ?
C14 C19 C20 124.9(3) . . ?
O1 C20 O2 123.8(3) . . ?
O1 C20 C19 120.0(3) . . ?
O2 C20 C19 116.1(3) . . ?
C22 C21 C23 120.4(4) . 3_557 ?
C22 C21 H21 119.8 . . ?
C23 C21 H21 119.8 3_557 . ?
C23 C22 C21 120.6(4) . . ?
C23 C22 H22 119.7 . . ?
C21 C22 H22 119.7 . . ?
C22 C23 C21 119.0(4) . 3_557 ?
C22 C23 C24 120.6(3) . . ?
C21 C23 C24 120.4(3) 3_557 . ?
O4 C24 O3 123.4(3) . . ?
O4 C24 C23 117.5(3) . . ?
O3 C24 C23 119.1(3) . . ?
C1 N1 C12 118.9(3) . . ?
C1 N1 Pb 121.8(2) . . ?
C12 N1 Pb 118.8(2) . . ?
C10 N2 C11 118.4(3) . . ?
C10 N2 Pb 119.9(2) . . ?
C11 N2 Pb 121.6(2) . . ?
C13 N3 C5 107.5(3) . . ?
C13 N3 H3A 126.3 . . ?
C5 N3 H3A 126.3 . . ?
C13 N4 C6 105.2(3) . . ?
C20 O2 Pb 104.4(2) . 4_565 ?
C24 O3 Pb 85.7(2) . . ?
C24 O4 Pb 100.1(2) . . ?
O2 Pb O4 74.71(8) 4_666 . ?
O2 Pb N2 81.90(9) 4_666 . ?
O4 Pb N2 76.88(9) . . ?
O2 Pb N1 71.59(9) 4_666 . ?
O4 Pb N1 131.06(9) . . ?
N2 Pb N1 64.22(9) . . ?
O2 Pb O3 70.43(8) 4_666 . ?
O4 Pb O3 49.96(8) . . ?
N2 Pb O3 124.30(8) . . ?
N1 Pb O3 138.77(8) . . ?

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 O3 0.86 2.05 2.844(4) 152.8 4_565

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.38
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.440
_refine_diff_density_min         -0.679
_refine_diff_density_rms         0.126
