# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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 1049263'
_audit_update_record             
;
2015-02-13 deposited with the CCDC.
2015-04-24 downloaded from the CCDC.
;
#=====================================================================  

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C10 H7 N7 O3 Pb'
_chemical_formula_sum            'C10 H7 N7 O3 Pb'
_chemical_formula_weight         480.42

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           orthorhombic
_symmetry_space_group_name_H-M   Pbca
_symmetry_space_group_name_hall  '-P 2ac 2ab'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   12.941(4)
_cell_length_b                   6.9454(18)
_cell_length_c                   26.594(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2390.3(11)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7160
_cell_measurement_theta_min      2.1961
_cell_measurement_theta_max      27.4816

_exptl_crystal_description       Prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    2.670
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1776
_exptl_absorpt_coefficient_mu    14.142
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6452
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   ?

_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  'Saturn70 (4x4 bin mode)'
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean 28.5714
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18867
_diffrn_reflns_av_R_equivalents  0.0614
_diffrn_reflns_av_sigmaI/netI    0.0406
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         2.20
_diffrn_reflns_theta_max         27.50
_reflns_number_total             2724
_reflns_number_gt                2203
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0730P)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         2724
_refine_ls_number_parameters     190
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0272
_refine_ls_wR_factor_ref         0.1134
_refine_ls_wR_factor_gt          0.0788
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_restrained_S_all      0.998
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.136501(19) 0.23525(4) 0.685583(9) 0.01336(13) Uani 1 1 d . . .
N7 N 0.1272(5) -0.2016(10) 0.7347(2) 0.0223(14) Uani 1 1 d . . .
N5 N 0.8544(4) 0.1017(9) 0.5941(2) 0.0132(12) Uani 1 1 d . . .
N4 N 0.3592(4) 0.2052(10) 0.5595(2) 0.0167(13) Uani 1 1 d . . .
N2 N 0.2594(4) 0.1252(8) 0.62103(18) 0.0148(12) Uani 1 1 d U . .
C2 C 0.5289(5) 0.1063(8) 0.5945(2) 0.0125(13) Uani 1 1 d . . .
C4 C 0.6904(5) 0.1182(10) 0.5493(2) 0.0167(14) Uani 1 1 d . . .
H4A H 0.7260 0.1310 0.5191 0.020 Uiso 1 1 calc R . .
C6 C 0.6906(5) 0.0816(10) 0.6386(2) 0.0157(14) Uani 1 1 d . . .
H6A H 0.7267 0.0654 0.6685 0.019 Uiso 1 1 calc R . .
C5 C 0.7437(5) 0.0997(9) 0.5936(2) 0.0107(12) Uani 1 1 d . . .
N3 N 0.2617(5) 0.2110(8) 0.5768(2) 0.0154(12) Uani 1 1 d . . .
C7 C 0.5835(5) 0.0877(11) 0.6390(2) 0.0193(15) Uani 1 1 d . . .
H7A H 0.5482 0.0793 0.6693 0.023 Uiso 1 1 calc R . .
C3 C 0.5836(5) 0.1178(10) 0.5496(2) 0.0163(14) Uani 1 1 d . . .
H3A H 0.5479 0.1254 0.5193 0.020 Uiso 1 1 calc R . .
O3 O 0.1772(4) -0.1145(8) 0.7015(2) 0.0320(13) Uani 1 1 d . . .
C1 C 0.4154(5) 0.1202(10) 0.5950(2) 0.0145(14) Uani 1 1 d . . .
C11 C 0.9154(5) 0.1070(11) 0.6353(3) 0.0201(15) Uani 1 1 d . . .
H11A H 0.8912 0.1024 0.6682 0.024 Uiso 1 1 calc R . .
O1 O 0.0451(5) -0.1360(9) 0.7492(2) 0.0471(17) Uani 1 1 d . . .
N1 N 0.3556(4) 0.0635(8) 0.6337(2) 0.0153(12) Uani 1 1 d . . .
N6 N 1.0138(4) 0.1196(8) 0.6228(2) 0.0157(12) Uani 1 1 d . . .
C10 C 1.0168(5) 0.1297(10) 0.5714(2) 0.0175(15) Uani 1 1 d . . .
H10A H 1.0763 0.1442 0.5521 0.021 Uiso 1 1 calc R . .
C9 C 0.9195(5) 0.1152(10) 0.5530(2) 0.0168(14) Uani 1 1 d . . .
H9A H 0.9002 0.1145 0.5193 0.020 Uiso 1 1 calc R . .
O2 O 0.1651(6) -0.3527(9) 0.7516(2) 0.0430(16) 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 N6 2.440(5) 1_455 ?
Pb1 N2 2.462(5) . ?
Pb1 O3 2.522(5) . ?
Pb1 O3 2.661(6) 8_665 ?
Pb1 N1 2.666(6) 8_665 ?
N7 O1 1.220(8) . ?
N7 O2 1.242(9) . ?
N7 O3 1.250(8) . ?
N5 C11 1.350(8) . ?
N5 C9 1.383(8) . ?
N5 C5 1.432(8) . ?
N4 C1 1.331(8) . ?
N4 N3 1.344(8) . ?
N2 N3 1.318(7) . ?
N2 N1 1.360(7) . ?
C2 C3 1.391(9) . ?
C2 C7 1.385(9) . ?
C2 C1 1.472(9) . ?
C4 C5 1.372(8) . ?
C4 C3 1.381(9) . ?
C6 C7 1.386(9) . ?
C6 C5 1.385(9) . ?
O3 Pb1 2.661(6) 8_655 ?
C1 N1 1.347(8) . ?
C11 N6 1.318(8) . ?
N1 Pb1 2.666(6) 8_655 ?
N6 C10 1.370(8) . ?
N6 Pb1 2.440(5) 1_655 ?
C10 C9 1.354(9) . ?

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
N6 Pb1 N2 80.86(19) 1_455 . ?
N6 Pb1 O3 86.22(19) 1_455 . ?
N2 Pb1 O3 71.52(18) . . ?
N6 Pb1 O3 145.86(18) 1_455 8_665 ?
N2 Pb1 O3 69.36(19) . 8_665 ?
O3 Pb1 O3 99.30(12) . 8_665 ?
N6 Pb1 N1 87.25(18) 1_455 8_665 ?
N2 Pb1 N1 83.11(18) . 8_665 ?
O3 Pb1 N1 154.50(18) . 8_665 ?
O3 Pb1 N1 73.30(16) 8_665 8_665 ?
O1 N7 O2 122.9(7) . . ?
O1 N7 O3 119.6(7) . . ?
O2 N7 O3 117.4(7) . . ?
C11 N5 C9 106.4(5) . . ?
C11 N5 C5 126.4(5) . . ?
C9 N5 C5 127.0(5) . . ?
C1 N4 N3 106.4(5) . . ?
N3 N2 N1 110.0(5) . . ?
N3 N2 Pb1 119.8(4) . . ?
N1 N2 Pb1 121.1(4) . . ?
C3 C2 C7 118.6(6) . . ?
C3 C2 C1 120.8(6) . . ?
C7 C2 C1 120.5(6) . . ?
C5 C4 C3 119.9(6) . . ?
C7 C6 C5 120.0(6) . . ?
C4 C5 C6 120.0(6) . . ?
C4 C5 N5 120.7(5) . . ?
C6 C5 N5 119.3(5) . . ?
N2 N3 N4 108.3(6) . . ?
C6 C7 C2 120.5(6) . . ?
C4 C3 C2 120.9(6) . . ?
N7 O3 Pb1 118.5(5) . . ?
N7 O3 Pb1 113.1(5) . 8_655 ?
Pb1 O3 Pb1 122.7(2) . 8_655 ?
N4 C1 N1 111.0(6) . . ?
N4 C1 C2 124.6(6) . . ?
N1 C1 C2 124.1(6) . . ?
N6 C11 N5 111.3(6) . . ?
C1 N1 N2 104.1(5) . . ?
C1 N1 Pb1 128.6(4) . 8_655 ?
N2 N1 Pb1 115.6(4) . 8_655 ?
C11 N6 C10 106.4(6) . . ?
C11 N6 Pb1 118.6(4) . 1_655 ?
C10 N6 Pb1 130.4(4) . 1_655 ?
C9 C10 N6 109.2(6) . . ?
C10 C9 N5 106.7(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
N6 Pb1 N2 N3 64.6(5) 1_455 . . . ?
O3 Pb1 N2 N3 153.6(5) . . . . ?
O3 Pb1 N2 N3 -98.4(5) 8_665 . . . ?
N1 Pb1 N2 N3 -23.7(4) 8_665 . . . ?
N6 Pb1 N2 N1 -151.7(5) 1_455 . . . ?
O3 Pb1 N2 N1 -62.6(5) . . . . ?
O3 Pb1 N2 N1 45.3(5) 8_665 . . . ?
N1 Pb1 N2 N1 120.0(5) 8_665 . . . ?
C3 C4 C5 C6 -0.3(10) . . . . ?
C3 C4 C5 N5 -179.3(6) . . . . ?
C7 C6 C5 C4 -1.8(10) . . . . ?
C7 C6 C5 N5 177.2(6) . . . . ?
C11 N5 C5 C4 171.9(7) . . . . ?
C9 N5 C5 C4 -2.2(10) . . . . ?
C11 N5 C5 C6 -7.2(10) . . . . ?
C9 N5 C5 C6 178.8(7) . . . . ?
N1 N2 N3 N4 0.7(7) . . . . ?
Pb1 N2 N3 N4 148.1(4) . . . . ?
C1 N4 N3 N2 -2.1(8) . . . . ?
C5 C6 C7 C2 1.8(10) . . . . ?
C3 C2 C7 C6 0.3(9) . . . . ?
C1 C2 C7 C6 -177.7(6) . . . . ?
C5 C4 C3 C2 2.5(9) . . . . ?
C7 C2 C3 C4 -2.4(9) . . . . ?
C1 C2 C3 C4 175.5(6) . . . . ?
O1 N7 O3 Pb1 18.6(9) . . . . ?
O2 N7 O3 Pb1 -160.9(5) . . . . ?
O1 N7 O3 Pb1 172.6(5) . . . 8_655 ?
O2 N7 O3 Pb1 -6.9(9) . . . 8_655 ?
N6 Pb1 O3 N7 -91.2(6) 1_455 . . . ?
N2 Pb1 O3 N7 -172.8(6) . . . . ?
O3 Pb1 O3 N7 122.8(5) 8_665 . . . ?
N1 Pb1 O3 N7 -166.7(5) 8_665 . . . ?
N6 Pb1 O3 Pb1 117.5(3) 1_455 . . 8_655 ?
N2 Pb1 O3 Pb1 35.8(2) . . . 8_655 ?
O3 Pb1 O3 Pb1 -28.6(4) 8_665 . . 8_655 ?
N1 Pb1 O3 Pb1 42.0(6) 8_665 . . 8_655 ?
N3 N4 C1 N1 2.8(8) . . . . ?
N3 N4 C1 C2 -171.7(6) . . . . ?
C3 C2 C1 N4 -23.5(10) . . . . ?
C7 C2 C1 N4 154.3(7) . . . . ?
C3 C2 C1 N1 162.6(6) . . . . ?
C7 C2 C1 N1 -19.5(10) . . . . ?
C9 N5 C11 N6 -1.0(8) . . . . ?
C5 N5 C11 N6 -176.1(6) . . . . ?
N4 C1 N1 N2 -2.4(8) . . . . ?
C2 C1 N1 N2 172.2(6) . . . . ?
N4 C1 N1 Pb1 138.2(5) . . . 8_655 ?
C2 C1 N1 Pb1 -47.2(9) . . . 8_655 ?
N3 N2 N1 C1 1.0(7) . . . . ?
Pb1 N2 N1 C1 -145.9(4) . . . . ?
N3 N2 N1 Pb1 -145.6(4) . . . 8_655 ?
Pb1 N2 N1 Pb1 67.6(5) . . . 8_655 ?
N5 C11 N6 C10 2.1(8) . . . . ?
N5 C11 N6 Pb1 160.4(5) . . . 1_655 ?
C11 N6 C10 C9 -2.4(8) . . . . ?
Pb1 N6 C10 C9 -157.1(5) 1_655 . . . ?
N6 C10 C9 N5 1.8(8) . . . . ?
C11 N5 C9 C10 -0.5(8) . . . . ?
C5 N5 C9 C10 174.5(6) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         2.039
_refine_diff_density_min         -2.041
_refine_diff_density_rms         0.380
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2
_database_code_depnum_ccdc_archive 'CCDC 1049264'
_audit_update_record             
;
2015-02-13 deposited with the CCDC.
2015-04-24 downloaded from the CCDC.
;
#=====================================================================  

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C20 H14 N12 Pb'
_chemical_formula_sum            'C20 H14 N12 Pb'
_chemical_formula_weight         629.62

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'
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   P21/c
_symmetry_space_group_name_hall  '-P 2ybc '
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.1322(11)
_cell_length_b                   7.3687(4)
_cell_length_c                   21.000(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.060(5)
_cell_angle_gamma                90.00
_cell_volume                     1952.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5133
_cell_measurement_theta_min      2.0182
_cell_measurement_theta_max      27.4797

_exptl_crystal_description       Prism
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    2.142
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1200
_exptl_absorpt_coefficient_mu    8.679
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6293
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   ?

_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  'Saturn70 (4x4 bin mode)'
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean 13.6612
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15014
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_av_sigmaI/netI    0.0459
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.02
_diffrn_reflns_theta_max         27.50
_reflns_number_total             4483
_reflns_number_gt                4012
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0920P)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         4483
_refine_ls_number_parameters     298
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0417
_refine_ls_wR_factor_ref         0.1276
_refine_ls_wR_factor_gt          0.1121
_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
Pb1 Pb 0.131306(16) 0.30661(3) 0.068224(11) 0.02555(12) Uani 1 1 d . . .
N12 N 0.0483(5) 0.7252(10) 0.0631(4) 0.0413(15) Uani 1 1 d . . .
N11 N 0.1423(5) 0.6742(9) 0.0545(4) 0.0448(17) Uani 1 1 d . . .
N22 N 0.3027(4) 0.3376(8) 0.1504(3) 0.0347(13) Uani 1 1 d . . .
N13 N 0.0527(5) 0.8975(9) 0.0790(3) 0.0400(14) Uani 1 1 d . . .
N23 N 0.3190(5) 0.2681(10) 0.2102(3) 0.0380(13) Uani 1 1 d . . .
C11 C 0.3137(5) 0.8239(8) 0.0642(3) 0.0275(13) Uani 1 1 d . . .
C10 C 0.2032(6) 0.8189(7) 0.0670(4) 0.0282(14) Uani 1 1 d . . .
C26 C 0.6535(5) 0.2286(9) 0.2475(3) 0.0294(13) Uani 1 1 d . . .
H26A H 0.6289 0.1573 0.2766 0.035 Uiso 1 1 calc R . .
C14 C 0.5225(5) 0.8296(8) 0.0581(3) 0.0262(12) Uani 1 1 d . . .
C21 C 0.5822(5) 0.3360(8) 0.2013(3) 0.0286(13) Uani 1 1 d . . .
N21 N 0.3944(4) 0.3763(8) 0.1375(3) 0.0341(12) Uani 1 1 d . . .
C20 C 0.4680(5) 0.3289(8) 0.1932(3) 0.0253(12) Uani 1 1 d . . .
C12 C 0.3911(5) 0.9146(9) 0.1121(3) 0.0322(13) Uani 1 1 d . . .
H12A H 0.3731 0.9737 0.1466 0.039 Uiso 1 1 calc R . .
C22 C 0.6219(5) 0.4431(8) 0.1593(3) 0.0332(14) Uani 1 1 d . . .
H22A H 0.5757 0.5170 0.1286 0.040 Uiso 1 1 calc R . .
N24 N 0.4232(5) 0.2616(9) 0.2386(3) 0.0346(12) Uani 1 1 d . . .
C13 C 0.4964(5) 0.9178(9) 0.1089(3) 0.0299(12) Uani 1 1 d . . .
H13A H 0.5480 0.9792 0.1410 0.036 Uiso 1 1 calc R . .
C15 C 0.4456(5) 0.7393(11) 0.0096(4) 0.0368(15) Uani 1 1 d . . .
H15A H 0.4637 0.6806 -0.0249 0.044 Uiso 1 1 calc R . .
C18 C 0.7161(5) 0.9067(10) 0.0990(4) 0.0382(15) Uani 1 1 d . . .
H18A H 0.7163 0.9723 0.1368 0.046 Uiso 1 1 calc R . .
N15 N 0.6296(4) 0.8273(7) 0.0552(3) 0.0274(11) Uani 1 1 d . . .
C16 C 0.3418(6) 0.7373(11) 0.0129(4) 0.0375(15) Uani 1 1 d . . .
H16A H 0.2902 0.6772 -0.0196 0.045 Uiso 1 1 calc R . .
C19 C 0.8003(5) 0.8706(12) 0.0762(4) 0.0412(16) Uani 1 1 d . . .
H19A H 0.8693 0.9086 0.0960 0.049 Uiso 1 1 calc R . .
N14 N 0.1504(4) 0.9600(8) 0.0824(3) 0.0326(12) Uani 1 1 d . . .
N16 N 0.7683(5) 0.7678(9) 0.0185(3) 0.0369(13) Uani 1 1 d . . .
C17 C 0.6660(6) 0.7467(11) 0.0082(3) 0.0339(14) Uani 1 1 d . . .
H17A H 0.6233 0.6832 -0.0276 0.041 Uiso 1 1 calc R . .
C25 C 0.7601(6) 0.2261(10) 0.2507(3) 0.0345(14) Uani 1 1 d . . .
H25A H 0.8066 0.1540 0.2821 0.041 Uiso 1 1 calc R . .
C24 C 0.7974(6) 0.3293(9) 0.2079(3) 0.0311(14) Uani 1 1 d . . .
N25 N 0.9057(5) 0.3220(7) 0.2078(3) 0.0328(13) Uani 1 1 d . . .
C23 C 0.7290(5) 0.4426(9) 0.1622(3) 0.0324(13) Uani 1 1 d . . .
H23A H 0.7546 0.5164 0.1341 0.039 Uiso 1 1 calc R . .
C28 C 0.9920(6) 0.2857(11) 0.2612(4) 0.0436(19) Uani 1 1 d . . .
H28A H 0.9914 0.2651 0.3048 0.052 Uiso 1 1 calc R . .
C27 C 0.9438(7) 0.3407(13) 0.1548(4) 0.049(2) Uani 1 1 d . . .
H27A H 0.9019 0.3652 0.1122 0.058 Uiso 1 1 calc R . .
C29 C 1.0783(6) 0.2865(11) 0.2369(4) 0.0406(17) Uani 1 1 d . . .
H29A H 1.1478 0.2669 0.2621 0.049 Uiso 1 1 calc R . .
N26 N 1.0479(6) 0.3198(9) 0.1708(4) 0.0473(18) 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 N22 2.439(6) . ?
Pb1 N14 2.575(6) 1_545 ?
Pb1 N16 2.586(6) 3_665 ?
Pb1 N26 2.674(7) 1_455 ?
Pb1 N11 2.732(7) . ?
N12 N13 1.309(11) . ?
N12 N11 1.349(10) . ?
N11 C10 1.315(9) . ?
N22 N23 1.318(10) . ?
N22 N21 1.336(8) . ?
N13 N14 1.346(7) . ?
N23 N24 1.334(8) . ?
C11 C16 1.386(10) . ?
C11 C12 1.388(9) . ?
C11 C10 1.469(9) . ?
C10 N14 1.338(8) . ?
C26 C25 1.384(9) . ?
C26 C21 1.392(9) . ?
C14 C13 1.372(9) . ?
C14 C15 1.390(9) . ?
C14 N15 1.425(8) . ?
C21 C22 1.387(9) . ?
C21 C20 1.464(9) . ?
N21 C20 1.341(8) . ?
C20 N24 1.346(9) . ?
C12 C13 1.402(8) . ?
C22 C23 1.392(9) . ?
C15 C16 1.384(10) . ?
C18 C19 1.347(10) . ?
C18 N15 1.378(8) . ?
N15 C17 1.347(9) . ?
C19 N16 1.392(10) . ?
N14 Pb1 2.575(6) 1_565 ?
N16 C17 1.309(9) . ?
N16 Pb1 2.586(6) 3_665 ?
C25 C24 1.368(10) . ?
C24 C23 1.396(9) . ?
C24 N25 1.424(9) . ?
N25 C27 1.346(10) . ?
N25 C28 1.382(10) . ?
C28 C29 1.366(11) . ?
C27 N26 1.324(11) . ?
C29 N26 1.358(11) . ?
N26 Pb1 2.674(7) 1_655 ?

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
N22 Pb1 N14 88.29(19) . 1_545 ?
N22 Pb1 N16 88.1(2) . 3_665 ?
N14 Pb1 N16 79.55(19) 1_545 3_665 ?
N22 Pb1 N26 86.0(2) . 1_455 ?
N14 Pb1 N26 89.53(19) 1_545 1_455 ?
N16 Pb1 N26 167.7(2) 3_665 1_455 ?
N22 Pb1 N11 85.2(2) . . ?
N14 Pb1 N11 171.5(2) 1_545 . ?
N16 Pb1 N11 94.8(2) 3_665 . ?
N26 Pb1 N11 95.4(2) 1_455 . ?
N13 N12 N11 109.1(6) . . ?
C10 N11 N12 106.0(6) . . ?
C10 N11 Pb1 146.0(5) . . ?
N12 N11 Pb1 100.7(5) . . ?
N23 N22 N21 111.0(6) . . ?
N23 N22 Pb1 120.8(5) . . ?
N21 N22 Pb1 125.7(5) . . ?
N12 N13 N14 108.6(5) . . ?
N22 N23 N24 108.5(6) . . ?
C16 C11 C12 119.1(6) . . ?
C16 C11 C10 119.8(6) . . ?
C12 C11 C10 121.1(6) . . ?
N11 C10 N14 110.5(7) . . ?
N11 C10 C11 124.5(6) . . ?
N14 C10 C11 125.0(5) . . ?
C25 C26 C21 121.2(6) . . ?
C13 C14 C15 120.6(6) . . ?
C13 C14 N15 120.1(6) . . ?
C15 C14 N15 119.3(6) . . ?
C22 C21 C26 117.9(6) . . ?
C22 C21 C20 119.9(6) . . ?
C26 C21 C20 122.0(6) . . ?
N22 N21 C20 103.8(6) . . ?
N21 C20 N24 111.4(6) . . ?
N21 C20 C21 124.1(6) . . ?
N24 C20 C21 124.4(6) . . ?
C11 C12 C13 120.5(6) . . ?
C21 C22 C23 121.6(6) . . ?
N23 N24 C20 105.3(6) . . ?
C14 C13 C12 119.4(6) . . ?
C16 C15 C14 119.6(6) . . ?
C19 C18 N15 106.6(6) . . ?
C17 N15 C18 106.4(5) . . ?
C17 N15 C14 126.3(6) . . ?
C18 N15 C14 127.4(6) . . ?
C15 C16 C11 120.7(6) . . ?
C18 C19 N16 109.7(6) . . ?
C10 N14 N13 105.7(6) . . ?
C10 N14 Pb1 141.6(4) . 1_565 ?
N13 N14 Pb1 105.8(4) . 1_565 ?
C17 N16 C19 104.9(6) . . ?
C17 N16 Pb1 123.9(5) . 3_665 ?
C19 N16 Pb1 129.7(5) . 3_665 ?
N16 C17 N15 112.5(6) . . ?
C24 C25 C26 120.1(7) . . ?
C25 C24 C23 120.4(7) . . ?
C25 C24 N25 121.3(6) . . ?
C23 C24 N25 118.3(6) . . ?
C27 N25 C28 106.4(6) . . ?
C27 N25 C24 126.6(6) . . ?
C28 N25 C24 126.9(6) . . ?
C22 C23 C24 118.8(6) . . ?
C29 C28 N25 105.9(7) . . ?
N26 C27 N25 111.9(7) . . ?
N26 C29 C28 110.1(7) . . ?
C27 N26 C29 105.7(7) . . ?
C27 N26 Pb1 115.2(6) . 1_655 ?
C29 N26 Pb1 138.4(5) . 1_655 ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         3.134
_refine_diff_density_min         -2.223
_refine_diff_density_rms         0.313

