# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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 1909534'
loop_
_audit_author_name
_audit_author_address
'Xiaoshuo Wu'
;Nanjing Tech University
China
;
_audit_update_record             
;
2019-08-12 deposited with the CCDC.	2019-08-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H10 N4 O4 Pb'
_chemical_formula_weight         481.43

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   Pccn

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

_cell_length_a                   11.5834(5)
_cell_length_b                   12.4815(5)
_cell_length_c                   9.1984(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1329.89(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5289
_cell_measurement_theta_min      2.3988
_cell_measurement_theta_max      27.4665

_exptl_crystal_description       block
_exptl_crystal_colour            'light yellow'
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.405
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             896
_exptl_absorpt_coefficient_mu    12.709
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.237
_exptl_absorpt_correction_T_max  0.319
_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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9839
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_sigmaI/netI    0.0237
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.40
_diffrn_reflns_theta_max         25.50
_reflns_number_total             1227
_reflns_number_gt                955
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker 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 > 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)+(0.0483P)²+0.4107P] 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         1227
_refine_ls_number_parameters     96
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0286
_refine_ls_R_factor_gt           0.0194
_refine_ls_wR_factor_ref         0.0695
_refine_ls_wR_factor_gt          0.0656
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_restrained_S_all      0.999
_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
Pb1 Pb 0.7500 0.2500 0.08902(2) 0.02127(14) Uani 1 2 d S . .
O1 O 0.8753(3) 0.2161(3) 0.3075(3) 0.0279(7) Uani 1 1 d . . .
O2 O 0.5665(3) 0.3768(2) 0.1171(3) 0.0385(8) Uani 1 1 d . . .
N1 N 0.8341(3) 0.4524(3) 0.1130(4) 0.0296(9) Uani 1 1 d . . .
N2 N 0.9599(3) 0.4375(3) 0.3037(4) 0.0324(9) Uani 1 1 d . . .
H2A H 0.9323 0.3746 0.3191 0.039 Uiso 1 1 calc R . .
H2B H 1.0139 0.4621 0.3586 0.039 Uiso 1 1 calc R . .
C1 C 0.7908(5) 0.5104(4) 0.0030(5) 0.0361(11) Uani 1 1 d . . .
H1 H 0.7318 0.4801 -0.0519 0.043 Uiso 1 1 calc R . .
C2 C 0.9189(3) 0.4973(3) 0.1940(4) 0.0231(8) Uani 1 1 d . . .
C4 C 0.5570(3) 0.3508(3) 0.2483(4) 0.0239(9) Uani 1 1 d . . .
C5 C 0.4628(4) 0.3995(3) 0.3378(3) 0.0208(9) Uani 1 1 d . . .
C6 C 0.4162(4) 0.3439(4) 0.4532(4) 0.0313(10) Uani 1 1 d . . .
H6 H 0.4441 0.2762 0.4770 0.038 Uiso 1 1 calc R . .
C7 C 0.3271(4) 0.3896(4) 0.5338(5) 0.0390(12) Uani 1 1 d . . .
H7 H 0.2933 0.3527 0.6107 0.047 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pb1 0.0226(2) 0.02008(19) 0.0211(2) 0.000 0.000 0.00092(9)
O1 0.0301(18) 0.0191(13) 0.0347(15) -0.0017(15) -0.0022(16) 0.0094(15)
O2 0.042(2) 0.045(2) 0.0282(16) 0.0014(15) 0.0073(15) 0.0160(16)
N1 0.029(2) 0.025(2) 0.0346(19) 0.0029(17) -0.0052(17) -0.0091(17)
N2 0.039(2) 0.026(2) 0.0325(18) 0.0101(17) -0.0114(18) -0.0089(18)
C1 0.030(2) 0.036(3) 0.043(3) 0.000(2) -0.013(2) -0.007(2)
C2 0.025(2) 0.021(2) 0.0232(18) -0.0009(18) 0.0045(18) -0.0007(18)
C4 0.024(2) 0.018(2) 0.030(2) -0.0034(17) 0.0005(18) -0.0006(18)
C5 0.018(2) 0.022(2) 0.022(2) -0.0006(15) -0.0024(15) 0.0006(19)
C6 0.034(3) 0.023(2) 0.037(2) 0.007(2) 0.007(2) 0.008(2)
C7 0.036(3) 0.042(3) 0.039(3) 0.013(2) 0.013(2) 0.001(2)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 O1 2.515(3) . ?
Pb1 O1 2.515(3) 2_655 ?
Pb1 O2 2.662(3) 2_655 ?
Pb1 O2 2.662(3) . ?
Pb1 N1 2.716(3) 2_655 ?
Pb1 N1 2.716(3) . ?
O1 C4 1.267(5) 2_655 ?
O2 C4 1.255(4) . ?
N1 C1 1.342(6) . ?
N1 C2 1.355(5) . ?
N2 C2 1.342(5) . ?
C1 C7 1.361(7) 4_565 ?
C2 C5 1.415(6) 4_565 ?
C4 O1 1.267(5) 2_655 ?
C4 C5 1.497(6) . ?
C5 C6 1.378(5) . ?
C5 C2 1.415(6) 4_465 ?
C6 C7 1.394(6) . ?
C7 C1 1.361(7) 4_465 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Pb1 O1 73.92(15) . 2_655 ?
O1 Pb1 O2 50.33(10) . 2_655 ?
O1 Pb1 O2 118.91(10) 2_655 2_655 ?
O1 Pb1 O2 118.91(10) . . ?
O1 Pb1 O2 50.33(10) 2_655 . ?
O2 Pb1 O2 168.87(13) 2_655 . ?
O1 Pb1 N1 89.15(11) . 2_655 ?
O1 Pb1 N1 83.38(11) 2_655 2_655 ?
O2 Pb1 N1 74.06(10) 2_655 2_655 ?
O2 Pb1 N1 105.00(10) . 2_655 ?
O1 Pb1 N1 83.38(11) . . ?
O1 Pb1 N1 89.15(11) 2_655 . ?
O2 Pb1 N1 105.00(10) 2_655 . ?
O2 Pb1 N1 74.06(10) . . ?
N1 Pb1 N1 170.67(16) 2_655 . ?
C4 O1 Pb1 97.2(2) 2_655 . ?
C4 O2 Pb1 90.5(2) . . ?
C1 N1 C2 117.5(4) . . ?
C1 N1 Pb1 107.8(3) . . ?
C2 N1 Pb1 133.6(3) . . ?
N1 C1 C7 124.6(4) . 4_565 ?
N2 C2 N1 116.1(4) . . ?
N2 C2 C5 122.3(4) . 4_565 ?
N1 C2 C5 121.6(4) . 4_565 ?
O2 C4 O1 121.9(4) . 2_655 ?
O2 C4 C5 119.2(4) . . ?
O1 C4 C5 118.8(3) 2_655 . ?
C6 C5 C2 118.5(4) . 4_465 ?
C6 C5 C4 120.3(4) . . ?
C2 C5 C4 121.2(3) 4_465 . ?
C5 C6 C7 119.6(4) . . ?
C1 C7 C6 118.2(4) 4_465 . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.646
_refine_diff_density_min         -1.676
_refine_diff_density_rms         0.251
####################################################################### 
# 
# 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 1909535'
loop_
_audit_author_name
_audit_author_address
'Xiaoshuo Wu'
;Nanjing Tech University
China
;
_audit_update_record             
;
2019-04-11 deposited with the CCDC.	2019-08-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H16 N2 O6 Pb'
_chemical_formula_weight         587.55

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           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                   16.1564(10)
_cell_length_b                   15.4233(10)
_cell_length_c                   8.1906(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.808(2)
_cell_angle_gamma                90.00
_cell_volume                     2026.6(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    303(2)
_cell_measurement_reflns_used    9450
_cell_measurement_theta_min      2.9795
_cell_measurement_theta_max      27.4663

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.926
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1120
_exptl_absorpt_coefficient_mu    8.364
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.452
_exptl_absorpt_correction_T_max  0.605
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      303(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            43712
_diffrn_reflns_av_R_equivalents  0.0461
_diffrn_reflns_av_sigmaI/netI    0.0230
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.83
_diffrn_reflns_theta_max         27.50
_reflns_number_total             4637
_reflns_number_gt                4063
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker 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 > 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)+(0.0455P)²+9.5671P] 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         4637
_refine_ls_number_parameters     262
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0357
_refine_ls_wR_factor_ref         0.0960
_refine_ls_wR_factor_gt          0.0924
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_restrained_S_all      1.101
_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
Pb1 Pb 0.750366(13) 0.213336(13) 0.23622(2) 0.02823(9) Uani 1 1 d . . .
N1 N 0.9861(3) 0.5614(4) 0.1989(7) 0.0424(12) Uani 1 1 d . . .
N2 N 0.4146(4) 0.4469(4) 0.2910(8) 0.0550(16) Uani 1 1 d . . .
O2 O 0.8106(3) 0.3222(3) 0.0440(5) 0.0416(10) Uani 1 1 d . . .
O1 O 0.8645(3) 0.3323(3) 0.3026(5) 0.0427(11) Uani 1 1 d . . .
O3 O 0.6328(3) 0.3328(4) 0.1807(5) 0.0535(14) Uani 1 1 d . . .
O4 O 0.6761(3) 0.3076(3) 0.4400(5) 0.0429(11) Uani 1 1 d . . .
C14 C 0.4372(5) 0.3798(5) 0.5596(9) 0.0504(17) Uani 1 1 d . . .
C19 C 0.3895(4) 0.4308(5) 0.4392(9) 0.0455(15) Uani 1 1 d . . .
C13 C 0.5149(4) 0.3487(5) 0.5213(8) 0.0440(15) Uani 1 1 d . . .
H13 H 0.5486 0.3157 0.5978 0.053 Uiso 1 1 calc R . .
C12 C 0.5405(4) 0.3667(4) 0.3730(7) 0.0366(13) Uani 1 1 d . . .
C9 C 0.9438(4) 0.6150(4) 0.0856(8) 0.0394(14) Uani 1 1 d . . .
C2 C 0.8827(4) 0.4516(4) 0.1282(7) 0.0314(12) Uani 1 1 d . . .
C10 C 0.9561(4) 0.4839(4) 0.2191(8) 0.0382(13) Uani 1 1 d . . .
H10 H 0.9847 0.4480 0.2977 0.046 Uiso 1 1 calc R . .
C3 C 0.8399(4) 0.5046(4) 0.0147(7) 0.0365(13) Uani 1 1 d . . .
H3 H 0.7920 0.4846 -0.0482 0.044 Uiso 1 1 calc R . .
C8 C 0.9755(5) 0.6991(5) 0.0633(10) 0.0537(19) Uani 1 1 d . . .
H8 H 1.0256 0.7164 0.1219 0.064 Uiso 1 1 calc R . .
C5 C 0.8257(6) 0.6498(5) -0.1181(10) 0.062(2) Uani 1 1 d . . .
H5 H 0.7764 0.6337 -0.1810 0.074 Uiso 1 1 calc R . .
C4 C 0.8683(4) 0.5900(4) -0.0073(8) 0.0399(14) Uani 1 1 d . . .
C1 C 0.8515(3) 0.3629(4) 0.1597(6) 0.0299(11) Uani 1 1 d . . .
C6 C 0.8573(7) 0.7314(6) -0.1326(12) 0.074(3) Uani 1 1 d . . .
H6 H 0.8282 0.7715 -0.2023 0.089 Uiso 1 1 calc R . .
C7 C 0.9323(7) 0.7547(6) -0.0441(11) 0.070(3) Uani 1 1 d . . .
H7 H 0.9538 0.8097 -0.0584 0.084 Uiso 1 1 calc R . .
C20 C 0.4868(5) 0.4160(5) 0.2609(9) 0.0499(17) Uani 1 1 d . . .
H20 H 0.5038 0.4275 0.1585 0.060 Uiso 1 1 calc R . .
C15 C 0.4078(6) 0.3653(7) 0.7128(12) 0.079(3) Uani 1 1 d . . .
H15 H 0.4390 0.3322 0.7927 0.095 Uiso 1 1 calc R . .
C16 C 0.3334(7) 0.4000(9) 0.7435(14) 0.096(4) Uani 1 1 d . . .
H16 H 0.3138 0.3896 0.8439 0.115 Uiso 1 1 calc R . .
C17 C 0.2868(6) 0.4507(7) 0.6259(14) 0.078(3) Uani 1 1 d . . .
H17 H 0.2373 0.4756 0.6503 0.094 Uiso 1 1 calc R . .
C18 C 0.3126(5) 0.4642(5) 0.4757(11) 0.059(2) Uani 1 1 d . . .
H18 H 0.2792 0.4958 0.3966 0.071 Uiso 1 1 calc R . .
C11 C 0.6217(4) 0.3345(4) 0.3289(7) 0.0335(12) Uani 1 1 d . . .
O5 O 0.8572(3) 0.1028(4) 0.1232(6) 0.0509(12) Uani 1 1 d . . .
H5A H 0.9015 0.0965 0.1943 0.076 Uiso 1 1 d R . .
H5B H 0.8768 0.1246 0.0373 0.076 Uiso 1 1 d R . .
O6 O 0.6398(4) 0.1061(4) 0.3596(7) 0.079(2) Uani 1 1 d . . .
H6A H 0.6028 0.1362 0.3990 0.119 Uiso 1 1 d R . .
H6B H 0.6168 0.0737 0.2835 0.119 Uiso 1 1 d R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pb1 0.03290(13) 0.03068(13) 0.02078(11) 0.00058(7) 0.00184(8) 0.00024(9)
N1 0.038(3) 0.045(3) 0.043(3) -0.008(2) 0.002(2) -0.012(2)
N2 0.049(4) 0.062(4) 0.053(4) 0.007(3) 0.001(3) 0.023(3)
O2 0.054(3) 0.042(2) 0.027(2) -0.0013(18) -0.0039(18) -0.016(2)
O1 0.051(3) 0.042(3) 0.033(2) 0.0003(18) -0.0057(19) -0.013(2)
O3 0.062(3) 0.076(4) 0.024(2) 0.007(2) 0.009(2) 0.030(3)
O4 0.036(2) 0.060(3) 0.031(2) -0.002(2) -0.0022(18) 0.013(2)
C14 0.042(4) 0.065(5) 0.045(4) 0.003(3) 0.009(3) 0.006(3)
C19 0.039(4) 0.042(4) 0.054(4) -0.008(3) 0.001(3) 0.009(3)
C13 0.035(3) 0.059(4) 0.037(3) 0.007(3) 0.000(2) 0.010(3)
C12 0.036(3) 0.042(3) 0.030(3) -0.002(2) 0.000(2) 0.009(3)
C9 0.040(3) 0.046(4) 0.034(3) -0.008(3) 0.012(2) -0.010(3)
C2 0.032(3) 0.034(3) 0.029(3) -0.006(2) 0.005(2) -0.003(2)
C10 0.034(3) 0.041(3) 0.038(3) -0.003(3) -0.002(2) -0.003(3)
C3 0.035(3) 0.041(3) 0.033(3) -0.003(2) -0.002(2) -0.007(3)
C8 0.062(5) 0.049(4) 0.051(4) -0.007(3) 0.012(3) -0.021(4)
C5 0.071(5) 0.054(5) 0.057(4) 0.018(4) -0.008(4) -0.009(4)
C4 0.047(4) 0.038(3) 0.035(3) -0.001(2) 0.006(3) -0.005(3)
C1 0.029(3) 0.033(3) 0.027(2) -0.003(2) 0.002(2) 0.001(2)
C6 0.099(8) 0.053(5) 0.067(6) 0.021(4) -0.001(5) -0.007(5)
C7 0.105(8) 0.043(4) 0.063(5) 0.009(4) 0.015(5) -0.027(5)
C20 0.052(4) 0.058(4) 0.040(3) 0.008(3) 0.006(3) 0.020(3)
C15 0.059(5) 0.116(8) 0.067(5) 0.022(6) 0.025(4) 0.021(5)
C16 0.071(7) 0.145(11) 0.079(7) 0.016(7) 0.042(6) 0.026(7)
C17 0.046(5) 0.091(7) 0.102(8) -0.009(6) 0.027(5) 0.013(5)
C18 0.044(4) 0.051(4) 0.081(6) -0.006(4) 0.008(4) 0.012(3)
C11 0.036(3) 0.034(3) 0.029(3) -0.001(2) -0.002(2) 0.003(2)
O5 0.043(3) 0.071(3) 0.039(2) 0.007(2) 0.003(2) 0.015(2)
O6 0.105(5) 0.094(5) 0.041(3) -0.017(3) 0.015(3) -0.062(4)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 O2 2.570(4) . ?
Pb1 O4 2.596(4) 4_565 ?
Pb1 O4 2.610(5) . ?
Pb1 O1 2.612(4) . ?
Pb1 O3 2.647(5) . ?
Pb1 O2 2.649(4) 4_566 ?
Pb1 O5 2.669(5) . ?
Pb1 O6 2.716(5) . ?
N1 C10 1.308(8) . ?
N1 C9 1.364(9) . ?
N2 C20 1.311(9) . ?
N2 C19 1.348(9) . ?
O2 C1 1.258(7) . ?
O2 Pb1 2.649(4) 4_565 ?
O1 C1 1.257(7) . ?
O3 C11 1.248(7) . ?
O4 C11 1.258(7) . ?
O4 Pb1 2.596(4) 4_566 ?
C14 C15 1.411(11) . ?
C14 C13 1.414(9) . ?
C14 C19 1.416(10) . ?
C19 C18 1.410(10) . ?
C13 C12 1.358(9) . ?
C13 H13 0.9300 . ?
C12 C20 1.409(8) . ?
C12 C11 1.486(8) . ?
C9 C4 1.413(9) . ?
C9 C8 1.415(9) . ?
C2 C3 1.363(8) . ?
C2 C10 1.413(8) . ?
C2 C1 1.491(8) . ?
C10 H10 0.9300 . ?
C3 C4 1.413(9) . ?
C3 H3 0.9300 . ?
C8 C7 1.359(12) . ?
C8 H8 0.9300 . ?
C5 C6 1.369(11) . ?
C5 C4 1.414(10) . ?
C5 H5 0.9300 . ?
C6 C7 1.384(13) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C20 H20 0.9300 . ?
C15 C16 1.365(12) . ?
C15 H15 0.9300 . ?
C16 C17 1.390(14) . ?
C16 H16 0.9300 . ?
C17 C18 1.361(13) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
O5 H5A 0.8734 . ?
O5 H5B 0.8722 . ?
O6 H6A 0.8500 . ?
O6 H6B 0.8500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Pb1 O4 71.05(14) . 4_565 ?
O2 Pb1 O4 105.32(17) . . ?
O4 Pb1 O4 118.03(17) 4_565 . ?
O2 Pb1 O1 50.20(13) . . ?
O4 Pb1 O1 121.24(14) 4_565 . ?
O4 Pb1 O1 80.94(16) . . ?
O2 Pb1 O3 75.88(16) . . ?
O4 Pb1 O3 71.53(16) 4_565 . ?
O4 Pb1 O3 49.24(13) . . ?
O1 Pb1 O3 91.21(19) . . ?
O2 Pb1 O2 126.51(17) . 4_566 ?
O4 Pb1 O2 160.12(16) 4_565 4_566 ?
O4 Pb1 O2 69.60(14) . 4_566 ?
O1 Pb1 O2 77.09(15) . 4_566 ?
O3 Pb1 O2 118.84(13) . 4_566 ?
O2 Pb1 O5 84.11(16) . . ?
O4 Pb1 O5 80.96(16) 4_565 . ?
O4 Pb1 O5 160.54(14) . . ?
O1 Pb1 O5 92.94(16) . . ?
O3 Pb1 O5 149.96(14) . . ?
O2 Pb1 O5 91.06(14) 4_566 . ?
O2 Pb1 O6 159.89(18) . . ?
O4 Pb1 O6 91.18(15) 4_565 . ?
O4 Pb1 O6 74.24(19) . . ?
O1 Pb1 O6 146.03(15) . . ?
O3 Pb1 O6 89.9(2) . . ?
O2 Pb1 O6 72.75(17) 4_566 . ?
O5 Pb1 O6 102.8(2) . . ?
C10 N1 C9 118.5(5) . . ?
C20 N2 C19 118.1(6) . . ?
C1 O2 Pb1 93.9(3) . . ?
C1 O2 Pb1 157.1(4) . 4_565 ?
Pb1 O2 Pb1 108.97(15) . 4_565 ?
C1 O1 Pb1 92.0(3) . . ?
C11 O3 Pb1 91.8(4) . . ?
C11 O4 Pb1 157.3(4) . 4_566 ?
C11 O4 Pb1 93.2(4) . . ?
Pb1 O4 Pb1 109.37(16) 4_566 . ?
C15 C14 C13 123.0(7) . . ?
C15 C14 C19 119.6(7) . . ?
C13 C14 C19 117.3(6) . . ?
N2 C19 C18 119.3(7) . . ?
N2 C19 C14 122.2(6) . . ?
C18 C19 C14 118.4(7) . . ?
C12 C13 C14 120.1(6) . . ?
C12 C13 H13 120.0 . . ?
C14 C13 H13 120.0 . . ?
C13 C12 C20 117.7(6) . . ?
C13 C12 C11 121.3(5) . . ?
C20 C12 C11 121.0(6) . . ?
N1 C9 C4 122.1(6) . . ?
N1 C9 C8 119.0(6) . . ?
C4 C9 C8 118.9(7) . . ?
C3 C2 C10 118.3(6) . . ?
C3 C2 C1 120.9(5) . . ?
C10 C2 C1 120.8(5) . . ?
N1 C10 C2 123.7(6) . . ?
N1 C10 H10 118.1 . . ?
C2 C10 H10 118.1 . . ?
C2 C3 C4 120.0(6) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C7 C8 C9 119.7(8) . . ?
C7 C8 H8 120.1 . . ?
C9 C8 H8 120.1 . . ?
C6 C5 C4 119.8(8) . . ?
C6 C5 H5 120.1 . . ?
C4 C5 H5 120.1 . . ?
C3 C4 C9 117.2(6) . . ?
C3 C4 C5 123.3(6) . . ?
C9 C4 C5 119.4(6) . . ?
O1 C1 O2 121.9(5) . . ?
O1 C1 C2 118.9(5) . . ?
O2 C1 C2 119.1(5) . . ?
C5 C6 C7 120.3(8) . . ?
C5 C6 H6 119.8 . . ?
C7 C6 H6 119.8 . . ?
C8 C7 C6 121.8(8) . . ?
C8 C7 H7 119.1 . . ?
C6 C7 H7 119.1 . . ?
N2 C20 C12 124.5(6) . . ?
N2 C20 H20 117.7 . . ?
C12 C20 H20 117.7 . . ?
C16 C15 C14 119.9(9) . . ?
C16 C15 H15 120.1 . . ?
C14 C15 H15 120.1 . . ?
C15 C16 C17 120.6(9) . . ?
C15 C16 H16 119.7 . . ?
C17 C16 H16 119.7 . . ?
C18 C17 C16 120.9(8) . . ?
C18 C17 H17 119.5 . . ?
C16 C17 H17 119.5 . . ?
C17 C18 C19 120.5(8) . . ?
C17 C18 H18 119.8 . . ?
C19 C18 H18 119.8 . . ?
O3 C11 O4 121.8(6) . . ?
O3 C11 C12 118.4(5) . . ?
O4 C11 C12 119.7(5) . . ?
Pb1 O5 H5A 110.6 . . ?
Pb1 O5 H5B 110.2 . . ?
H5A O5 H5B 103.5 . . ?
Pb1 O6 H6A 109.4 . . ?
Pb1 O6 H6B 109.6 . . ?
H6A O6 H6B 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         2.161
_refine_diff_density_min         -2.681
_refine_diff_density_rms         0.184
