# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_Zn
_audit_block_doi                 10.5517/cc1jm6kx
_database_code_depnum_ccdc_archive 'CCDC 1418639'
_audit_update_record             
;
2016-04-17 deposited with the CCDC.
2016-08-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C9 H7 N4 O7 Zn2'
_chemical_formula_weight         413.97

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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

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

_cell_length_a                   7.794(2)
_cell_length_b                   9.057(3)
_cell_length_c                   9.169(3)
_cell_angle_alpha                90.38(3)
_cell_angle_beta                 91.24(2)
_cell_angle_gamma                107.59(2)
_cell_volume                     616.8(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5771
_cell_measurement_theta_min      3.03
_cell_measurement_theta_max      27.45

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.229
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             410
_exptl_absorpt_coefficient_mu    3.935
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_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  'CCD area detector'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5771
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_sigmaI/netI    0.0637
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.03
_diffrn_reflns_theta_max         27.45
_reflns_number_total             2709
_reflns_number_gt                2197
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0503P)²+1.4544P] 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         2709
_refine_ls_number_parameters     215
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0472
_refine_ls_wR_factor_ref         0.1192
_refine_ls_wR_factor_gt          0.1129
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O4 O 1.1279(9) 0.3935(5) 0.5690(5) 0.0611(13) Uani 1 1 d D . .
H2 H 1.240(4) 0.405(13) 0.567(12) 0.13(5) Uiso 1 1 d D . .
H3 H 0.924(9) 0.229(7) 0.869(5) 0.07(2) Uiso 1 1 d D . .
H1 H 1.106(14) 0.444(11) 0.498(8) 0.13(4) Uiso 1 1 d D . .
H4 H 0.782(7) 0.218(8) 0.784(8) 0.07(2) Uiso 1 1 d D . .
Zn1 Zn 0.99208(7) 0.14166(6) 0.59805(5) 0.02535(17) Uani 1 1 d . . .
Zn2 Zn 0.99124(7) 0.18050(6) 0.23174(5) 0.02440(17) Uani 1 1 d . . .
O1 O 1.1030(4) 0.0983(4) 0.3935(3) 0.0231(7) Uani 1 1 d . . .
O2 O 1.1572(4) -0.0103(4) 0.8978(3) 0.0316(8) Uani 1 1 d . . .
O3 O 1.2240(5) 0.1608(4) 0.7173(4) 0.0363(8) Uani 1 1 d . . .
O5 O 0.7987(7) 0.5751(6) -0.2661(5) 0.0732(16) Uani 1 1 d . . .
O6 O 0.9112(5) 0.6762(4) -0.0592(4) 0.0399(9) Uani 1 1 d . . .
O7 O 0.8705(6) 0.1824(6) 0.7939(4) 0.0479(10) Uani 1 1 d D . .
N1 N 0.7835(5) 0.2167(4) 0.3455(4) 0.0235(8) Uani 1 1 d . . .
N2 N 0.7673(5) 0.1814(5) 0.4866(4) 0.0274(9) Uani 1 1 d . . .
N3 N 0.6073(6) 0.1747(6) 0.5292(4) 0.0408(11) Uani 1 1 d . . .
N4 N 0.5127(6) 0.2060(6) 0.4145(4) 0.0388(11) Uani 1 1 d . . .
C1 C 0.6242(6) 0.2319(5) 0.3033(5) 0.0228(9) Uani 1 1 d . . .
C2 C 0.5867(6) 0.2720(5) 0.1524(5) 0.0234(9) Uani 1 1 d . . .
C3 C 0.7054(6) 0.4003(5) 0.0877(5) 0.0241(9) Uani 1 1 d . . .
H3A H 0.8026 0.4637 0.1416 0.029 Uiso 1 1 calc R . .
C4 C 0.4406(6) 0.1777(5) 0.0730(5) 0.0242(9) Uani 1 1 d . . .
H4A H 0.3617 0.0922 0.1166 0.029 Uiso 1 1 calc R . .
C5 C 0.4120(6) 0.2110(5) -0.0720(5) 0.0226(9) Uani 1 1 d . . .
C6 C 0.5323(6) 0.3379(5) -0.1366(5) 0.0233(9) Uani 1 1 d . . .
H6 H 0.5150 0.3594 -0.2339 0.028 Uiso 1 1 calc R . .
C7 C 0.6791(6) 0.4335(5) -0.0565(5) 0.0233(9) Uani 1 1 d . . .
C8 C 0.8047(6) 0.5686(6) -0.1320(6) 0.0320(11) Uani 1 1 d . . .
C9 C 1.2504(6) 0.1135(6) 0.8409(5) 0.0260(10) 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
O4 Zn1 2.226(5) . ?
O4 H2 0.85(2) . ?
O4 H1 0.84(2) . ?
Zn1 O3 2.053(3) . ?
Zn1 O1 2.076(3) 2_756 ?
Zn1 O7 2.130(4) . ?
Zn1 N2 2.133(4) . ?
Zn1 O1 2.164(3) . ?
Zn1 Zn1 3.1579(15) 2_756 ?
Zn1 Zn2 3.3537(14) 2_756 ?
Zn1 Zn2 3.3795(13) . ?
Zn2 O1 1.966(3) . ?
Zn2 O2 1.991(3) 2_756 ?
Zn2 N1 2.051(4) . ?
Zn2 O6 2.062(4) 2_765 ?
Zn2 O5 2.336(5) 2_765 ?
Zn2 C8 2.537(5) 2_765 ?
Zn2 Zn1 3.3537(14) 2_756 ?
O1 Zn1 2.076(3) 2_756 ?
O2 C9 1.260(6) . ?
O2 Zn2 1.991(3) 2_756 ?
O3 C9 1.250(6) . ?
O5 C8 1.232(7) . ?
O5 Zn2 2.336(5) 2_765 ?
O6 C8 1.250(6) . ?
O6 Zn2 2.062(4) 2_765 ?
O7 H3 0.84(2) . ?
O7 H4 0.85(2) . ?
N1 N2 1.335(5) . ?
N1 C1 1.339(6) . ?
N2 N3 1.299(6) . ?
N3 N4 1.352(6) . ?
N4 C1 1.329(6) . ?
C1 C2 1.478(6) . ?
C2 C4 1.387(6) . ?
C2 C3 1.394(6) . ?
C3 C7 1.382(6) . ?
C3 H3A 0.9300 . ?
C4 C5 1.393(6) . ?
C4 H4A 0.9300 . ?
C5 C6 1.391(6) . ?
C5 C9 1.510(6) 1_454 ?
C6 C7 1.398(6) . ?
C6 H6 0.9300 . ?
C7 C8 1.501(7) . ?
C8 Zn2 2.537(5) 2_765 ?
C9 C5 1.510(6) 1_656 ?

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
Zn1 O4 H2 107(8) . . ?
Zn1 O4 H1 124(8) . . ?
H2 O4 H1 106(10) . . ?
O3 Zn1 O1 95.07(14) . 2_756 ?
O3 Zn1 O7 88.55(15) . . ?
O1 Zn1 O7 95.77(17) 2_756 . ?
O3 Zn1 N2 165.78(16) . . ?
O1 Zn1 N2 98.59(14) 2_756 . ?
O7 Zn1 N2 86.19(16) . . ?
O3 Zn1 O1 94.24(13) . . ?
O1 Zn1 O1 83.74(13) 2_756 . ?
O7 Zn1 O1 177.19(14) . . ?
N2 Zn1 O1 91.15(13) . . ?
O3 Zn1 O4 81.37(19) . . ?
O1 Zn1 O4 171.24(19) 2_756 . ?
O7 Zn1 O4 92.2(2) . . ?
N2 Zn1 O4 85.6(2) . . ?
O1 Zn1 O4 88.53(17) . . ?
O3 Zn1 Zn1 96.25(11) . 2_756 ?
O1 Zn1 Zn1 42.94(9) 2_756 2_756 ?
O7 Zn1 Zn1 138.64(14) . 2_756 ?
N2 Zn1 Zn1 96.43(11) . 2_756 ?
O1 Zn1 Zn1 40.80(8) . 2_756 ?
O4 Zn1 Zn1 129.20(15) . 2_756 ?
O3 Zn1 Zn2 64.38(11) . 2_756 ?
O1 Zn1 Zn2 32.89(8) 2_756 2_756 ?
O7 Zn1 Zn2 83.48(13) . 2_756 ?
N2 Zn1 Zn2 127.89(11) . 2_756 ?
O1 Zn1 Zn2 97.49(9) . 2_756 ?
O4 Zn1 Zn2 145.51(15) . 2_756 ?
Zn1 Zn1 Zn2 62.44(3) 2_756 2_756 ?
O3 Zn1 Zn2 122.05(10) . . ?
O1 Zn1 Zn2 98.58(9) 2_756 . ?
O7 Zn1 Zn2 144.49(11) . . ?
N2 Zn1 Zn2 59.68(11) . . ?
O1 Zn1 Zn2 33.21(8) . . ?
O4 Zn1 Zn2 76.86(13) . . ?
Zn1 Zn1 Zn2 61.62(3) 2_756 . ?
Zn2 Zn1 Zn2 124.06(3) 2_756 . ?
O1 Zn2 O2 111.06(14) . 2_756 ?
O1 Zn2 N1 97.48(14) . . ?
O2 Zn2 N1 97.21(15) 2_756 . ?
O1 Zn2 O6 134.43(14) . 2_765 ?
O2 Zn2 O6 93.07(15) 2_756 2_765 ?
N1 Zn2 O6 117.84(15) . 2_765 ?
O1 Zn2 O5 90.60(15) . 2_765 ?
O2 Zn2 O5 151.15(15) 2_756 2_765 ?
N1 Zn2 O5 98.62(18) . 2_765 ?
O6 Zn2 O5 58.17(15) 2_765 2_765 ?
O1 Zn2 C8 113.20(15) . 2_765 ?
O2 Zn2 C8 122.26(15) 2_756 2_765 ?
N1 Zn2 C8 111.55(16) . 2_765 ?
O6 Zn2 C8 29.29(16) 2_765 2_765 ?
O5 Zn2 C8 28.91(16) 2_765 2_765 ?
O1 Zn2 Zn1 34.98(9) . 2_756 ?
O2 Zn2 Zn1 76.39(10) 2_756 2_756 ?
N1 Zn2 Zn1 97.62(11) . 2_756 ?
O6 Zn2 Zn1 144.15(11) 2_765 2_756 ?
O5 Zn2 Zn1 124.79(13) 2_765 2_756 ?
C8 Zn2 Zn1 141.20(11) 2_765 2_756 ?
O1 Zn2 Zn1 37.08(9) . . ?
O2 Zn2 Zn1 120.93(10) 2_756 . ?
N1 Zn2 Zn1 61.42(10) . . ?
O6 Zn2 Zn1 146.00(11) 2_765 . ?
O5 Zn2 Zn1 87.87(11) 2_765 . ?
C8 Zn2 Zn1 116.79(12) 2_765 . ?
Zn1 Zn2 Zn1 55.94(3) 2_756 . ?
Zn2 O1 Zn1 112.12(14) . 2_756 ?
Zn2 O1 Zn1 109.72(14) . . ?
Zn1 O1 Zn1 96.26(13) 2_756 . ?
C9 O2 Zn2 118.8(3) . 2_756 ?
C9 O3 Zn1 131.9(3) . . ?
C8 O5 Zn2 84.6(3) . 2_765 ?
C8 O6 Zn2 96.9(3) . 2_765 ?
Zn1 O7 H3 126(5) . . ?
Zn1 O7 H4 116(5) . . ?
H3 O7 H4 103(7) . . ?
N2 N1 C1 105.3(4) . . ?
N2 N1 Zn2 119.6(3) . . ?
C1 N1 Zn2 132.6(3) . . ?
N3 N2 N1 110.1(4) . . ?
N3 N2 Zn1 132.0(3) . . ?
N1 N2 Zn1 117.9(3) . . ?
N2 N3 N4 108.6(4) . . ?
C1 N4 N3 105.6(4) . . ?
N4 C1 N1 110.4(4) . . ?
N4 C1 C2 127.3(4) . . ?
N1 C1 C2 122.3(4) . . ?
C4 C2 C3 120.2(4) . . ?
C4 C2 C1 120.3(4) . . ?
C3 C2 C1 119.4(4) . . ?
C7 C3 C2 120.2(4) . . ?
C7 C3 H3A 119.9 . . ?
C2 C3 H3A 119.9 . . ?
C2 C4 C5 120.1(4) . . ?
C2 C4 H4A 120.0 . . ?
C5 C4 H4A 120.0 . . ?
C6 C5 C4 119.4(4) . . ?
C6 C5 C9 119.5(4) . 1_454 ?
C4 C5 C9 121.1(4) . 1_454 ?
C5 C6 C7 120.5(4) . . ?
C5 C6 H6 119.7 . . ?
C7 C6 H6 119.7 . . ?
C3 C7 C6 119.5(4) . . ?
C3 C7 C8 122.3(4) . . ?
C6 C7 C8 118.2(4) . . ?
O5 C8 O6 120.2(5) . . ?
O5 C8 C7 119.6(5) . . ?
O6 C8 C7 120.2(5) . . ?
O5 C8 Zn2 66.5(3) . 2_765 ?
O6 C8 Zn2 53.8(3) . 2_765 ?
C7 C8 Zn2 172.2(4) . 2_765 ?
O3 C9 O2 125.9(4) . . ?
O3 C9 C5 117.0(4) . 1_656 ?
O2 C9 C5 117.1(4) . 1_656 ?

_diffrn_measured_fraction_theta_max 0.961
_diffrn_reflns_theta_full        27.45
_diffrn_measured_fraction_theta_full 0.961
_refine_diff_density_max         1.252
_refine_diff_density_min         -0.928
_refine_diff_density_rms         0.133
####################################################################### 
# 
# 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_Pb-phen
_audit_block_doi                 10.5517/cc1jm8n2
_database_code_depnum_ccdc_archive 'CCDC 1418704'
_audit_update_record             
;
2016-04-17 deposited with the CCDC.
2016-08-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H14 N6 O5 Pb'
_chemical_formula_weight         637.58

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/c

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                   11.2006(16)
_cell_length_b                   11.1967(16)
_cell_length_c                   18.5221(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 121.700(6)
_cell_angle_gamma                90.00
_cell_volume                     1976.3(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    14822
_cell_measurement_theta_min      2.14
_cell_measurement_theta_max      26.38

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.143
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1216
_exptl_absorpt_coefficient_mu    8.588
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14822
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0324
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.14
_diffrn_reflns_theta_max         26.38
_reflns_number_total             4028
_reflns_number_gt                3653
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0232P)²+1.0354P] 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         4028
_refine_ls_number_parameters     310
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0241
_refine_ls_R_factor_gt           0.0208
_refine_ls_wR_factor_ref         0.0525
_refine_ls_wR_factor_gt          0.0513
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
H24 H 1.129(5) 0.387(5) 0.287(4) 0.08(2) Uiso 1 1 d D . .
H25 H 1.201(6) 0.491(4) 0.329(3) 0.073(17) Uiso 1 1 d D . .
O5 O 1.1205(3) 0.4592(4) 0.3185(3) 0.0631(10) Uani 1 1 d . . .
Pb1 Pb 0.951136(11) 0.587618(11) 0.381934(7) 0.02214(6) Uani 1 1 d . . .
O1 O 0.8204(2) 0.6895(3) 0.22608(16) 0.0439(7) Uani 1 1 d . . .
O2 O 0.7215(2) 0.6984(2) 0.30199(15) 0.0314(6) Uani 1 1 d . . .
O3 O 0.2625(3) 0.9208(3) 0.17487(18) 0.0425(8) Uani 1 1 d . . .
O4 O 0.1632(2) 0.9935(2) 0.04467(14) 0.0277(5) Uani 1 1 d . . .
N1 N 1.0994(3) 0.7772(3) 0.38739(18) 0.0292(7) Uani 1 1 d . . .
N2 N 0.9953(3) 0.7494(3) 0.49099(17) 0.0260(6) Uani 1 1 d . . .
N3 N 0.5762(3) 0.8089(3) -0.07529(18) 0.0272(6) Uani 1 1 d . . .
N4 N 0.5324(3) 0.8415(3) -0.15444(18) 0.0281(7) Uani 1 1 d . . .
N5 N 0.4130(3) 0.9000(3) -0.19248(19) 0.0313(7) Uani 1 1 d . . .
N6 N 0.3736(3) 0.9073(3) -0.13665(19) 0.0284(7) Uani 1 1 d . . .
C1 C 0.7187(3) 0.7150(3) 0.2332(2) 0.0255(7) Uani 1 1 d . . .
C2 C 0.5916(3) 0.7707(3) 0.1587(2) 0.0224(7) Uani 1 1 d . . .
C3 C 0.5853(3) 0.7811(3) 0.0821(2) 0.0233(7) Uani 1 1 d . . .
H3 H 0.6569 0.7488 0.0769 0.028 Uiso 1 1 calc R . .
C4 C 0.4744(3) 0.8388(3) 0.0132(2) 0.0210(7) Uani 1 1 d . . .
C5 C 0.4736(3) 0.8510(3) -0.0658(2) 0.0212(7) Uani 1 1 d . . .
C6 C 0.2574(3) 0.9329(3) 0.1071(2) 0.0247(7) Uani 1 1 d . . .
C7 C 0.3701(3) 0.8760(3) 0.0966(2) 0.0206(7) Uani 1 1 d . . .
C8 C 0.9390(3) 0.7423(4) 0.5387(2) 0.0334(8) Uani 1 1 d . . .
H8 H 0.8715 0.6840 0.5256 0.040 Uiso 1 1 calc R . .
C9 C 0.9753(4) 0.8171(4) 0.6067(2) 0.0416(10) Uani 1 1 d . . .
H9 H 0.9302 0.8109 0.6368 0.050 Uiso 1 1 calc R . .
C10 C 1.0788(5) 0.9005(4) 0.6291(3) 0.0417(11) Uani 1 1 d . . .
H23 H 1.1070 0.9494 0.6760 0.050 Uiso 1 1 calc R . .
C11 C 1.1420(4) 0.9117(3) 0.5811(2) 0.0332(9) Uani 1 1 d . . .
C12 C 1.2479(4) 0.9991(4) 0.5987(3) 0.0458(10) Uani 1 1 d . . .
H12 H 1.2800 1.0489 0.6456 0.055 Uiso 1 1 calc R . .
C13 C 1.3013(4) 1.0107(4) 0.5492(3) 0.0452(10) Uani 1 1 d . . .
H13 H 1.3710 1.0670 0.5628 0.054 Uiso 1 1 calc R . .
C14 C 1.2529(4) 0.9381(4) 0.4763(3) 0.0353(9) Uani 1 1 d . . .
C15 C 1.2978(4) 0.9510(4) 0.4181(3) 0.0435(10) Uani 1 1 d . . .
H15 H 1.3642 1.0088 0.4278 0.052 Uiso 1 1 calc R . .
C16 C 1.2454(4) 0.8804(4) 0.3488(3) 0.0422(10) Uani 1 1 d . . .
H16 H 1.2747 0.8898 0.3105 0.051 Uiso 1 1 calc R . .
C17 C 1.1467(4) 0.7932(4) 0.3355(2) 0.0353(9) Uani 1 1 d . . .
H17 H 1.1125 0.7440 0.2882 0.042 Uiso 1 1 calc R . .
C18 C 1.1502(3) 0.8490(3) 0.4564(2) 0.0269(7) Uani 1 1 d . . .
C19 C 1.0948(3) 0.8348(3) 0.5110(2) 0.0261(7) Uani 1 1 d . . .
C20 C 0.4818(3) 0.8174(3) 0.1657(2) 0.0232(7) Uani 1 1 d . . .
H20 H 0.4835 0.8094 0.2162 0.028 Uiso 1 1 calc R . .
C21 C 0.3678(3) 0.8881(3) 0.0214(2) 0.0210(7) Uani 1 1 d . . .
H21 H 0.2947 0.9294 -0.0238 0.025 Uiso 1 1 calc R . .
H1 H 0.582(4) 0.827(4) -0.179(3) 0.046(12) Uiso 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
O5 Pb1 3.064(3) . ?
O5 H24 1.02(5) . ?
O5 H25 0.89(5) . ?
Pb1 O2 2.519(2) . ?
Pb1 O4 2.536(2) 2_645 ?
Pb1 N2 2.560(3) . ?
Pb1 N1 2.664(3) . ?
Pb1 O1 2.708(3) . ?
Pb1 O3 2.770(3) 2_645 ?
Pb1 O4 2.833(2) 4_676 ?
Pb1 C1 2.977(3) . ?
Pb1 C6 2.999(3) 2_645 ?
Pb1 Pb1 4.3755(5) 3_766 ?
O1 C1 1.247(4) . ?
O2 C1 1.272(4) . ?
O3 C6 1.233(4) . ?
O3 Pb1 2.770(2) 2_655 ?
O4 C6 1.276(4) . ?
O4 Pb1 2.536(2) 2_655 ?
O4 Pb1 2.833(2) 4_475 ?
N1 C17 1.332(4) . ?
N1 C18 1.356(4) . ?
N2 C8 1.330(4) . ?
N2 C19 1.364(4) . ?
N3 N4 1.330(4) . ?
N3 C5 1.336(4) . ?
N4 N5 1.313(4) . ?
N4 H1 0.89(4) . ?
N5 N6 1.323(4) . ?
N6 C5 1.352(4) . ?
C1 C2 1.501(4) . ?
C2 C3 1.388(4) . ?
C2 C20 1.404(4) . ?
C3 C4 1.387(4) . ?
C3 H3 0.9300 . ?
C4 C21 1.396(4) . ?
C4 C5 1.465(4) . ?
C6 C7 1.515(4) . ?
C6 Pb1 2.999(3) 2_655 ?
C7 C21 1.386(5) . ?
C7 C20 1.396(4) . ?
C8 C9 1.383(5) . ?
C8 H8 0.9300 . ?
C9 C10 1.372(6) . ?
C9 H9 0.9300 . ?
C10 C11 1.404(6) . ?
C10 H23 0.9300 . ?
C11 C19 1.409(5) . ?
C11 C12 1.436(6) . ?
C12 C13 1.340(6) . ?
C12 H12 0.9300 . ?
C13 C14 1.417(6) . ?
C13 H13 0.9300 . ?
C14 C15 1.415(6) . ?
C14 C18 1.417(5) . ?
C15 C16 1.351(6) . ?
C15 H15 0.9300 . ?
C16 C17 1.397(6) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C18 C19 1.446(5) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Pb1 O5 H24 148(3) . . ?
Pb1 O5 H25 119(3) . . ?
H24 O5 H25 93(3) . . ?
O2 Pb1 O4 82.68(8) . 2_645 ?
O2 Pb1 N2 80.18(8) . . ?
O4 Pb1 N2 79.26(8) 2_645 . ?
O2 Pb1 N1 93.06(8) . . ?
O4 Pb1 N1 142.31(8) 2_645 . ?
N2 Pb1 N1 63.15(9) . . ?
O2 Pb1 O1 49.67(7) . . ?
O4 Pb1 O1 127.15(7) 2_645 . ?
N2 Pb1 O1 108.37(9) . . ?
N1 Pb1 O1 71.46(9) . . ?
O2 Pb1 O3 72.40(9) . 2_645 ?
O4 Pb1 O3 49.04(8) 2_645 2_645 ?
N2 Pb1 O3 123.14(8) . 2_645 ?
N1 Pb1 O3 161.50(9) . 2_645 ?
O1 Pb1 O3 90.22(9) . 2_645 ?
O2 Pb1 O4 144.05(7) . 4_676 ?
O4 Pb1 O4 70.96(7) 2_645 4_676 ?
N2 Pb1 O4 71.39(8) . 4_676 ?
N1 Pb1 O4 93.30(8) . 4_676 ?
O1 Pb1 O4 161.86(7) . 4_676 ?
O3 Pb1 O4 105.19(8) 2_645 4_676 ?
O2 Pb1 C1 25.01(8) . . ?
O4 Pb1 C1 104.64(8) 2_645 . ?
N2 Pb1 C1 95.96(9) . . ?
N1 Pb1 C1 83.00(9) . . ?
O1 Pb1 C1 24.76(8) . . ?
O3 Pb1 C1 79.08(9) 2_645 . ?
O4 Pb1 C1 167.05(8) 4_676 . ?
O2 Pb1 C6 74.53(9) . 2_645 ?
O4 Pb1 C6 24.90(8) 2_645 2_645 ?
N2 Pb1 C6 100.93(9) . 2_645 ?
N1 Pb1 C6 161.74(9) . 2_645 ?
O1 Pb1 C6 108.13(9) . 2_645 ?
O3 Pb1 C6 24.27(8) 2_645 2_645 ?
O4 Pb1 C6 89.46(8) 4_676 2_645 ?
C1 Pb1 C6 90.32(9) . 2_645 ?
O2 Pb1 O5 130.71(9) . . ?
O4 Pb1 O5 126.84(10) 2_645 . ?
N2 Pb1 O5 137.11(9) . . ?
N1 Pb1 O5 83.63(10) . . ?
O1 Pb1 O5 83.43(10) . . ?
O3 Pb1 O5 97.09(9) 2_645 . ?
O4 Pb1 O5 85.17(9) 4_676 . ?
C1 Pb1 O5 106.64(10) . . ?
C6 Pb1 O5 114.59(10) 2_645 . ?
O2 Pb1 Pb1 116.77(5) . 3_766 ?
O4 Pb1 Pb1 37.74(5) 2_645 3_766 ?
N2 Pb1 Pb1 71.66(6) . 3_766 ?
N1 Pb1 Pb1 119.72(6) . 3_766 ?
O1 Pb1 Pb1 164.88(5) . 3_766 ?
O3 Pb1 Pb1 77.86(6) 2_645 3_766 ?
O4 Pb1 Pb1 33.22(4) 4_676 3_766 ?
C1 Pb1 Pb1 141.03(6) . 3_766 ?
C6 Pb1 Pb1 57.87(7) 2_645 3_766 ?
O5 Pb1 Pb1 107.04(8) . 3_766 ?
C1 O1 Pb1 89.8(2) . . ?
C1 O2 Pb1 98.11(19) . . ?
C6 O3 Pb1 88.3(2) . 2_655 ?
C6 O4 Pb1 98.3(2) . 2_655 ?
C6 O4 Pb1 128.8(2) . 4_475 ?
Pb1 O4 Pb1 109.04(7) 2_655 4_475 ?
C17 N1 C18 118.1(3) . . ?
C17 N1 Pb1 123.8(3) . . ?
C18 N1 Pb1 116.9(2) . . ?
C8 N2 C19 117.8(3) . . ?
C8 N2 Pb1 121.3(2) . . ?
C19 N2 Pb1 120.1(2) . . ?
N4 N3 C5 101.7(3) . . ?
N5 N4 N3 114.2(3) . . ?
N5 N4 H1 123(3) . . ?
N3 N4 H1 122(3) . . ?
N4 N5 N6 106.0(3) . . ?
N5 N6 C5 106.4(3) . . ?
O1 C1 O2 122.0(3) . . ?
O1 C1 C2 118.4(3) . . ?
O2 C1 C2 119.6(3) . . ?
O1 C1 Pb1 65.46(18) . . ?
O2 C1 Pb1 56.88(16) . . ?
C2 C1 Pb1 174.3(2) . . ?
C3 C2 C20 119.1(3) . . ?
C3 C2 C1 119.3(3) . . ?
C20 C2 C1 121.6(3) . . ?
C4 C3 C2 121.4(3) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 H3 119.3 . . ?
C3 C4 C21 119.2(3) . . ?
C3 C4 C5 119.7(3) . . ?
C21 C4 C5 121.1(3) . . ?
N3 C5 N6 111.6(3) . . ?
N3 C5 C4 122.9(3) . . ?
N6 C5 C4 125.4(3) . . ?
O3 C6 O4 123.7(3) . . ?
O3 C6 C7 119.2(3) . . ?
O4 C6 C7 117.0(3) . . ?
O3 C6 Pb1 67.43(19) . 2_655 ?
O4 C6 Pb1 56.79(16) . 2_655 ?
C7 C6 Pb1 169.3(2) . 2_655 ?
C21 C7 C20 120.1(3) . . ?
C21 C7 C6 120.7(3) . . ?
C20 C7 C6 119.1(3) . . ?
N2 C8 C9 123.6(4) . . ?
N2 C8 H8 118.2 . . ?
C9 C8 H8 118.2 . . ?
C10 C9 C8 119.0(4) . . ?
C10 C9 H9 120.5 . . ?
C8 C9 H9 120.5 . . ?
C9 C10 C11 119.8(4) . . ?
C9 C10 H23 120.1 . . ?
C11 C10 H23 120.1 . . ?
C10 C11 C19 117.3(4) . . ?
C10 C11 C12 123.2(4) . . ?
C19 C11 C12 119.4(4) . . ?
C13 C12 C11 121.5(4) . . ?
C13 C12 H12 119.3 . . ?
C11 C12 H12 119.3 . . ?
C12 C13 C14 120.8(4) . . ?
C12 C13 H13 119.6 . . ?
C14 C13 H13 119.6 . . ?
C15 C14 C18 116.1(4) . . ?
C15 C14 C13 123.7(4) . . ?
C18 C14 C13 120.2(4) . . ?
C16 C15 C14 120.8(4) . . ?
C16 C15 H15 119.6 . . ?
C14 C15 H15 119.6 . . ?
C15 C16 C17 119.0(4) . . ?
C15 C16 H16 120.5 . . ?
C17 C16 H16 120.5 . . ?
N1 C17 C16 123.0(4) . . ?
N1 C17 H17 118.5 . . ?
C16 C17 H17 118.5 . . ?
N1 C18 C14 122.9(3) . . ?
N1 C18 C19 118.2(3) . . ?
C14 C18 C19 118.9(3) . . ?
N2 C19 C11 122.4(3) . . ?
N2 C19 C18 118.5(3) . . ?
C11 C19 C18 119.1(3) . . ?
C7 C20 C2 119.9(3) . . ?
C7 C20 H20 120.1 . . ?
C2 C20 H20 120.1 . . ?
C7 C21 C4 120.4(3) . . ?
C7 C21 H21 119.8 . . ?
C4 C21 H21 119.8 . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        26.38
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.313
_refine_diff_density_min         -1.210
_refine_diff_density_rms         0.116
####################################################################### 
# 
# 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_Pb
_audit_block_doi                 10.5517/cc1jm8yc
_database_code_depnum_ccdc_archive 'CCDC 1418713'
_audit_update_record             
;
2016-04-17 deposited with the CCDC.
2016-08-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C9 H3 N4 O7 Pb2'
_chemical_formula_weight         693.55

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

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

_cell_length_a                   7.8513(2)
_cell_length_b                   9.1456(2)
_cell_length_c                   10.6941(3)
_cell_angle_alpha                112.083(2)
_cell_angle_beta                 108.443(2)
_cell_angle_gamma                96.4630(10)
_cell_volume                     651.18(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5783
_cell_measurement_theta_min      2.23
_cell_measurement_theta_max      24.99

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.537
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             610
_exptl_absorpt_coefficient_mu    25.864
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5783
_diffrn_reflns_av_R_equivalents  0.1056
_diffrn_reflns_av_sigmaI/netI    0.0721
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.23
_diffrn_reflns_theta_max         24.99
_reflns_number_total             2254
_reflns_number_gt                2071
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0863P)²+3.1416P] 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         2254
_refine_ls_number_parameters     199
_refine_ls_number_restraints     37
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0456
_refine_ls_wR_factor_ref         0.1298
_refine_ls_wR_factor_gt          0.1273
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O7 O 0.4142(17) 0.0428(11) 0.6035(10) 0.053(3) Uani 1 1 d D . .
O6 O 0.4884(11) 0.3700(9) 0.5424(8) 0.0226(17) Uani 1 1 d . . .
Pb1 Pb 0.77038(5) 0.53320(5) 0.58544(4) 0.0196(2) Uani 1 1 d . . .
Pb2 Pb 0.46243(7) 0.38144(5) 0.76366(5) 0.0279(2) Uani 1 1 d D . .
O1 O 0.6071(14) 0.6732(10) 1.0077(9) 0.034(2) Uani 1 1 d . . .
O2 O 0.6588(12) 0.6365(9) 0.8099(8) 0.0301(19) Uani 1 1 d . . .
O3 O 0.7166(14) 1.2521(11) 1.3818(9) 0.035(2) Uani 1 1 d . . .
O4 O 0.7806(14) 1.4508(10) 1.3258(9) 0.034(2) Uani 1 1 d . . .
O5 O 0.8895(14) 0.8238(13) 0.5326(11) 0.048(2) Uani 1 1 d U . .
N3 N 0.8613(15) 1.3479(13) 0.7252(11) 0.029(2) Uani 1 1 d . . .
N4 N 0.7941(15) 1.3305(12) 0.8190(11) 0.028(2) Uani 1 1 d . . .
N2 N 0.9463(16) 1.2333(14) 0.6849(12) 0.033(3) Uani 1 1 d . . .
C1 C 0.8443(15) 1.1983(13) 0.8336(12) 0.020(2) Uani 1 1 d . . .
N1 N 0.9424(17) 1.1424(13) 0.7583(12) 0.032(2) Uani 1 1 d . . .
C8 C 0.7492(16) 1.3014(14) 1.2949(12) 0.021(2) Uani 1 1 d . . .
C9 C 0.6638(15) 0.7288(13) 0.9324(11) 0.019(2) Uani 1 1 d U . .
C6 C 0.7211(15) 0.9088(13) 0.9832(11) 0.018(2) Uani 1 1 d U . .
C7 C 0.7654(16) 0.9729(13) 0.8938(12) 0.020(2) Uani 1 1 d . . .
H7 H 0.7692 0.9027 0.8059 0.024 Uiso 1 1 calc R . .
C5 C 0.7167(15) 1.0176(13) 1.1154(10) 0.019(2) Uani 1 1 d . . .
H5 H 0.6881 0.9775 1.1764 0.023 Uiso 1 1 calc R . .
C2 C 0.8037(14) 1.1403(13) 0.9351(10) 0.018(2) Uani 1 1 d . . .
C3 C 0.7948(16) 1.2418(13) 1.0632(11) 0.022(2) Uani 1 1 d U . .
H3 H 0.8166 1.3534 1.0894 0.027 Uiso 1 1 calc R . .
C4 C 0.7544(15) 1.1828(13) 1.1552(11) 0.019(2) Uani 1 1 d U . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O7 Pb2 2.829(9) . ?
O6 Pb1 2.331(8) . ?
O6 Pb2 2.403(7) . ?
O6 Pb1 2.518(8) 2_666 ?
Pb1 O6 2.518(8) 2_666 ?
Pb1 O3 2.548(9) 1_544 ?
Pb1 O4 2.620(8) 1_544 ?
Pb1 N3 2.668(9) 1_545 ?
Pb1 O2 2.690(7) . ?
Pb1 C8 2.969(11) 1_544 ?
Pb1 O5 3.027(11) . ?
Pb1 Pb1 3.9256(8) 2_666 ?
Pb1 Pb2 4.0103(6) 2_666 ?
Pb2 O2 2.429(8) . ?
Pb2 N4 2.618(10) 1_545 ?
Pb2 O1 2.725(9) . ?
Pb2 O4 2.742(9) 2_677 ?
Pb2 O1 2.869(7) 2_667 ?
Pb2 Pb1 4.0103(6) 2_666 ?
O1 C9 1.260(13) . ?
O1 Pb2 2.869(7) 2_667 ?
O2 C9 1.249(12) . ?
O3 C8 1.254(13) . ?
O3 Pb1 2.548(9) 1_566 ?
O4 C8 1.253(14) . ?
O4 Pb1 2.620(8) 1_566 ?
O4 Pb2 2.742(9) 2_677 ?
N3 N2 1.315(14) . ?
N3 N4 1.321(13) . ?
N3 Pb1 2.668(9) 1_565 ?
N4 C1 1.360(14) . ?
N4 Pb2 2.618(10) 1_565 ?
N2 N1 1.345(14) . ?
C1 N1 1.294(15) . ?
C1 C2 1.475(14) . ?
C8 C4 1.496(14) . ?
C8 Pb1 2.969(11) 1_566 ?
C9 C6 1.487(15) . ?
C6 C7 1.403(14) . ?
C6 C5 1.403(14) . ?
C7 C2 1.390(15) . ?
C7 H7 0.9300 . ?
C5 C4 1.374(15) . ?
C5 H5 0.9300 . ?
C2 C3 1.364(15) . ?
C3 C4 1.384(15) . ?
C3 H3 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Pb1 O6 Pb2 112.8(3) . . ?
Pb1 O6 Pb1 108.0(3) . 2_666 ?
Pb2 O6 Pb1 109.1(3) . 2_666 ?
O6 Pb1 O6 72.0(3) . 2_666 ?
O6 Pb1 O3 72.3(3) . 1_544 ?
O6 Pb1 O3 100.5(3) 2_666 1_544 ?
O6 Pb1 O4 104.9(3) . 1_544 ?
O6 Pb1 O4 76.2(3) 2_666 1_544 ?
O3 Pb1 O4 49.7(3) 1_544 1_544 ?
O6 Pb1 N3 74.6(3) . 1_545 ?
O6 Pb1 N3 145.7(3) 2_666 1_545 ?
O3 Pb1 N3 75.7(3) 1_544 1_545 ?
O4 Pb1 N3 120.0(3) 1_544 1_545 ?
O6 Pb1 O2 65.7(3) . . ?
O6 Pb1 O2 85.9(2) 2_666 . ?
O3 Pb1 O2 133.1(3) 1_544 . ?
O4 Pb1 O2 161.8(3) 1_544 . ?
N3 Pb1 O2 73.9(3) 1_545 . ?
O6 Pb1 C8 89.2(3) . 1_544 ?
O6 Pb1 C8 89.1(3) 2_666 1_544 ?
O3 Pb1 C8 24.8(3) 1_544 1_544 ?
O4 Pb1 C8 24.9(3) 1_544 1_544 ?
N3 Pb1 C8 97.5(3) 1_545 1_544 ?
O2 Pb1 C8 154.8(3) . 1_544 ?
O6 Pb1 O5 136.0(3) . . ?
O6 Pb1 O5 64.0(3) 2_666 . ?
O3 Pb1 O5 116.2(3) 1_544 . ?
O4 Pb1 O5 66.6(3) 1_544 . ?
N3 Pb1 O5 148.5(3) 1_545 . ?
O2 Pb1 O5 108.4(3) . . ?
C8 Pb1 O5 91.4(3) 1_544 . ?
O6 Pb1 Pb1 37.58(18) . 2_666 ?
O6 Pb1 Pb1 34.38(17) 2_666 2_666 ?
O3 Pb1 Pb1 86.3(2) 1_544 2_666 ?
O4 Pb1 Pb1 90.0(2) 1_544 2_666 ?
N3 Pb1 Pb1 111.8(2) 1_545 2_666 ?
O2 Pb1 Pb1 73.12(19) . 2_666 ?
C8 Pb1 Pb1 89.0(2) 1_544 2_666 ?
O5 Pb1 Pb1 98.42(19) . 2_666 ?
O6 Pb1 Pb2 92.17(17) . 2_666 ?
O6 Pb1 Pb2 34.48(16) 2_666 2_666 ?
O3 Pb1 Pb2 80.6(2) 1_544 2_666 ?
O4 Pb1 Pb2 42.8(2) 1_544 2_666 ?
N3 Pb1 Pb2 155.4(2) 1_545 2_666 ?
O2 Pb1 Pb2 119.91(18) . 2_666 ?
C8 Pb1 Pb2 61.0(2) 1_544 2_666 ?
O5 Pb1 Pb2 51.15(19) . 2_666 ?
Pb1 Pb1 Pb2 59.588(11) 2_666 2_666 ?
O6 Pb2 O2 69.1(3) . . ?
O6 Pb2 N4 83.2(3) . 1_545 ?
O2 Pb2 N4 76.5(3) . 1_545 ?
O6 Pb2 O1 118.4(2) . . ?
O2 Pb2 O1 49.8(2) . . ?
N4 Pb2 O1 89.7(3) 1_545 . ?
O6 Pb2 O4 75.8(2) . 2_677 ?
O2 Pb2 O4 75.1(3) . 2_677 ?
N4 Pb2 O4 149.2(3) 1_545 2_677 ?
O1 Pb2 O4 80.9(3) . 2_677 ?
O6 Pb2 O7 78.4(3) . . ?
O2 Pb2 O7 137.2(3) . . ?
N4 Pb2 O7 72.7(3) 1_545 . ?
O1 Pb2 O7 154.7(3) . . ?
O4 Pb2 O7 123.4(3) 2_677 . ?
O6 Pb2 O1 168.5(3) . 2_667 ?
O2 Pb2 O1 122.3(3) . 2_667 ?
N4 Pb2 O1 97.6(3) 1_545 2_667 ?
O1 Pb2 O1 73.2(3) . 2_667 ?
O4 Pb2 O1 107.5(3) 2_677 2_667 ?
O7 Pb2 O1 90.9(3) . 2_667 ?
O6 Pb2 Pb1 36.38(19) . 2_666 ?
O2 Pb2 Pb1 73.7(2) . 2_666 ?
N4 Pb2 Pb1 118.87(19) 1_545 2_666 ?
O1 Pb2 Pb1 108.43(17) . 2_666 ?
O4 Pb2 Pb1 40.44(16) 2_677 2_666 ?
O7 Pb2 Pb1 96.2(2) . 2_666 ?
O1 Pb2 Pb1 143.3(2) 2_667 2_666 ?
C9 O1 Pb2 86.6(6) . . ?
C9 O1 Pb2 166.2(8) . 2_667 ?
Pb2 O1 Pb2 106.8(3) . 2_667 ?
C9 O2 Pb2 100.8(6) . . ?
C9 O2 Pb1 157.1(7) . . ?
Pb2 O2 Pb1 100.7(3) . . ?
C8 O3 Pb1 96.8(7) . 1_566 ?
C8 O4 Pb1 93.4(6) . 1_566 ?
C8 O4 Pb2 128.5(8) . 2_677 ?
Pb1 O4 Pb2 96.8(3) 1_566 2_677 ?
N2 N3 N4 109.6(9) . . ?
N2 N3 Pb1 123.1(7) . 1_565 ?
N4 N3 Pb1 125.7(7) . 1_565 ?
N3 N4 C1 104.2(9) . . ?
N3 N4 Pb2 110.3(7) . 1_565 ?
C1 N4 Pb2 127.2(8) . 1_565 ?
N3 N2 N1 109.1(9) . . ?
N1 C1 N4 111.7(9) . . ?
N1 C1 C2 125.9(10) . . ?
N4 C1 C2 122.2(9) . . ?
C1 N1 N2 105.3(10) . . ?
O3 C8 O4 120.0(10) . . ?
O3 C8 C4 120.3(10) . . ?
O4 C8 C4 119.7(9) . . ?
O3 C8 Pb1 58.5(6) . 1_566 ?
O4 C8 Pb1 61.7(6) . 1_566 ?
C4 C8 Pb1 175.1(8) . 1_566 ?
O2 C9 O1 121.5(10) . . ?
O2 C9 C6 118.7(9) . . ?
O1 C9 C6 119.5(9) . . ?
C7 C6 C5 118.4(10) . . ?
C7 C6 C9 120.4(9) . . ?
C5 C6 C9 120.9(9) . . ?
C2 C7 C6 120.7(10) . . ?
C2 C7 H7 119.7 . . ?
C6 C7 H7 119.7 . . ?
C4 C5 C6 120.5(9) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C3 C2 C7 119.1(9) . . ?
C3 C2 C1 123.2(10) . . ?
C7 C2 C1 117.6(9) . . ?
C2 C3 C4 121.7(10) . . ?
C2 C3 H3 119.2 . . ?
C4 C3 H3 119.2 . . ?
C5 C4 C3 119.6(9) . . ?
C5 C4 C8 121.6(9) . . ?
C3 C4 C8 118.8(10) . . ?

_diffrn_measured_fraction_theta_max 0.983
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max         2.475
_refine_diff_density_min         -3.353
_refine_diff_density_rms         0.447
