# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1423047'
_audit_update_record             
;
2016-02-28 deposited with the CCDC.
2016-04-04 downloaded from the CCDC.
;
_audit_creation_date             2016-02-24
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2015.11.10 svn.r3248 for OlexSys, GUI svn.r5133)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C7 H7 N3 O7 Pb'
_chemical_formula_sum            'C7 H7 N3 O7 Pb'
_chemical_formula_weight         452.35
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -4.0753 8.5060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   4.53460(10)
_cell_length_b                   20.2191(6)
_cell_length_c                   11.4766(3)
_cell_angle_alpha                90
_cell_angle_beta                 97.340(3)
_cell_angle_gamma                90
_cell_volume                     1043.62(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1966
_cell_measurement_temperature    150
_cell_measurement_theta_max      70.725
_cell_measurement_theta_min      4.373
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    31.843
_exptl_absorpt_correction_T_max  0.0942
_exptl_absorpt_correction_T_min  0.0176
_exptl_absorpt_correction_type   Sphere
_exptl_absorpt_process_details   
;
C.W.Dwiggins Jr. Acta Cryst.(1975), A31,146-148.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.879
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_crystal_size_rad          0.1100
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0492
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       3
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3501
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.725
_diffrn_reflns_theta_min         4.373
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  
;
Goniometer Xcalibur, detector: Ruby
Oxford Diffraction (2007). Oxford Diffraction Ltd.,
Xcalibur CCD system
;
_diffrn_measurement_method       'w\ scan'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1875
_reflns_number_total             1966
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_refine_diff_density_max         2.976
_refine_diff_density_min         -3.066
_refine_diff_density_rms         0.464
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         1966
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_gt           0.0726
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1572P)²+0.1683P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1886
_refine_ls_wR_factor_ref         0.1909
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C5(H5A,H5B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.30550(8) 0.01196(2) 0.67610(3) 0.0399(3) Uani 1 1 d . . . . .
O1 O 0.5683(17) 0.0862(4) 0.8178(6) 0.0463(16) Uani 1 1 d . . . . .
O2 O 0.7151(16) 0.0586(3) 0.5643(6) 0.0442(15) Uani 1 1 d . . . . .
O3 O 0.0771(15) 0.1273(3) 0.6379(6) 0.0433(14) Uani 1 1 d . . . . .
O4 O 0.4245(18) -0.0933(4) 0.8119(7) 0.0509(16) Uani 1 1 d . . . . .
O5 O 0.7180(19) -0.0954(3) 0.6771(6) 0.0484(15) Uani 1 1 d . . . . .
O6 O 0.7094(18) -0.1781(4) 0.7966(7) 0.0541(18) Uani 1 1 d . . . . .
O7 O 0.945(2) 0.0137(3) 0.8296(7) 0.0453(19) Uani 1 1 d . . . . .
N3 N 0.7726(19) 0.2720(4) 0.9958(6) 0.0403(16) Uani 1 1 d . . . . .
N2 N 0.9265(19) 0.1752(4) 0.9545(6) 0.0401(16) Uani 1 1 d . . . . .
N1 N 0.6184(18) -0.1228(4) 0.7608(7) 0.0412(16) Uani 1 1 d . . . . .
C1 C 0.822(2) 0.0649(5) 0.8612(8) 0.041(2) Uani 1 1 d . . . . .
C2 C 0.996(2) 0.1039(4) 0.9604(8) 0.0402(18) Uani 1 1 d . . . . .
H2A H 0.9506 0.0865 1.0350 0.048 Uiso 1 1 calc R . . . .
H2B H 1.2066 0.0978 0.9573 0.048 Uiso 1 1 calc R . . . .
C3 C 1.018(2) 0.2172(5) 0.8733(8) 0.044(2) Uani 1 1 d . . . . .
H3 H 1.1260 0.2057 0.8128 0.053 Uiso 1 1 calc R . . . .
C4 C 0.921(2) 0.2790(5) 0.8967(8) 0.045(2) Uani 1 1 d . . . . .
H4 H 0.9486 0.3176 0.8556 0.054 Uiso 1 1 calc R . . . .
C5 C 0.619(2) 0.3247(5) 1.0485(8) 0.0411(19) Uani 1 1 d . . . . .
H5A H 0.5402 0.3077 1.1173 0.049 Uiso 1 1 calc R . . . .
H5B H 0.4528 0.3395 0.9930 0.049 Uiso 1 1 calc R . . . .
C6 C 0.781(2) 0.2083(4) 1.0287(9) 0.0419(19) Uani 1 1 d . . . . .
H6 H 0.6996 0.1906 1.0922 0.050 Uiso 1 1 calc R . . . .
C7 C 0.824(2) 0.1155(4) 0.5850(8) 0.0388(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 O1 2.412(7) . ?
Pb1 O2 2.568(7) . ?
Pb1 O3 2.566(7) . ?
Pb1 O4 2.652(7) . ?
Pb1 O7 2.553(8) 1_455 ?
O1 C1 1.269(13) . ?
O2 C7 1.262(11) . ?
O3 C7 1.252(12) 1_455 ?
O4 N1 1.267(11) . ?
O5 N1 1.242(11) . ?
O6 N1 1.243(11) . ?
O7 Pb1 2.553(8) 1_655 ?
O7 C1 1.250(12) . ?
N3 C4 1.401(13) . ?
N3 C5 1.447(12) . ?
N3 C6 1.341(12) . ?
N2 C2 1.475(10) . ?
N2 C3 1.363(13) . ?
N2 C6 1.324(13) . ?
C1 C2 1.519(13) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 H3 0.9300 . ?
C3 C4 1.360(13) . ?
C4 H4 0.9300 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C7 1.549(12) 4_566 ?
C6 H6 0.9300 . ?
C7 O3 1.252(12) 1_655 ?
C7 C5 1.549(12) 4_565 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Pb1 O2 77.4(2) . . ?
O1 Pb1 O3 72.8(2) . . ?
O1 Pb1 O4 93.3(3) . . ?
O1 Pb1 O7 80.3(2) . 1_455 ?
O2 Pb1 O4 118.8(2) . . ?
O3 Pb1 O2 83.3(2) . . ?
O3 Pb1 O4 151.3(2) . . ?
O7 Pb1 O2 155.2(2) 1_455 . ?
O7 Pb1 O3 79.9(2) 1_455 . ?
O7 Pb1 O4 72.9(2) 1_455 . ?
C1 O1 Pb1 113.5(6) . . ?
C7 O2 Pb1 122.0(6) . . ?
C7 O3 Pb1 103.6(5) 1_455 . ?
N1 O4 Pb1 101.9(5) . . ?
C1 O7 Pb1 124.1(6) . 1_655 ?
C4 N3 C5 124.9(8) . . ?
C6 N3 C4 109.0(8) . . ?
C6 N3 C5 126.0(8) . . ?
C3 N2 C2 124.1(8) . . ?
C6 N2 C2 125.8(8) . . ?
C6 N2 C3 110.0(8) . . ?
O5 N1 O4 119.4(8) . . ?
O5 N1 O6 121.2(9) . . ?
O6 N1 O4 119.4(8) . . ?
O1 C1 C2 118.4(8) . . ?
O7 C1 O1 125.6(9) . . ?
O7 C1 C2 116.0(9) . . ?
N2 C2 C1 112.7(8) . . ?
N2 C2 H2A 109.1 . . ?
N2 C2 H2B 109.1 . . ?
C1 C2 H2A 109.1 . . ?
C1 C2 H2B 109.1 . . ?
H2A C2 H2B 107.8 . . ?
N2 C3 H3 126.1 . . ?
C4 C3 N2 107.8(8) . . ?
C4 C3 H3 126.1 . . ?
N3 C4 H4 127.2 . . ?
C3 C4 N3 105.5(8) . . ?
C3 C4 H4 127.2 . . ?
N3 C5 H5A 109.1 . . ?
N3 C5 H5B 109.1 . . ?
N3 C5 C7 112.6(8) . 4_566 ?
H5A C5 H5B 107.8 . . ?
C7 C5 H5A 109.1 4_566 . ?
C7 C5 H5B 109.1 4_566 . ?
N3 C6 H6 126.1 . . ?
N2 C6 N3 107.7(9) . . ?
N2 C6 H6 126.1 . . ?
O2 C7 C5 117.0(9) . 4_565 ?
O3 C7 O2 125.2(9) 1_655 . ?
O3 C7 C5 117.6(8) 1_655 4_565 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pb1 O1 C1 O7 6.0(13) . . . . ?
Pb1 O1 C1 C2 -173.9(6) . . . . ?
Pb1 O2 C7 O3 106.8(9) . . . 1_655 ?
Pb1 O2 C7 C5 -69.4(9) . . . 4_565 ?
Pb1 O4 N1 O5 6.8(9) . . . . ?
Pb1 O4 N1 O6 -174.4(7) . . . . ?
Pb1 O7 C1 O1 93.1(12) 1_655 . . . ?
Pb1 O7 C1 C2 -87.1(10) 1_655 . . . ?
O1 C1 C2 N2 -29.0(13) . . . . ?
O7 C1 C2 N2 151.1(9) . . . . ?
N2 C3 C4 N3 0.7(12) . . . . ?
C2 N2 C3 C4 -178.2(9) . . . . ?
C2 N2 C6 N3 178.0(9) . . . . ?
C3 N2 C2 C1 -72.4(12) . . . . ?
C3 N2 C6 N3 0.8(11) . . . . ?
C4 N3 C5 C7 -56.9(12) . . . 4_566 ?
C4 N3 C6 N2 -0.4(12) . . . . ?
C5 N3 C4 C3 -176.6(9) . . . . ?
C5 N3 C6 N2 176.0(8) . . . . ?
C6 N3 C4 C3 -0.2(13) . . . . ?
C6 N3 C5 C7 127.3(10) . . . 4_566 ?
C6 N2 C2 C1 110.8(10) . . . . ?
C6 N2 C3 C4 -0.9(11) . . . . ?

_shelx_SHELXL_version_number     2014/8
__computing_data_collection      
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55
;
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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 1423048'
_audit_update_record             
;
2016-03-29 deposited with the CCDC.
2016-04-04 downloaded from the CCDC.
;
_audit_creation_date             2016-03-29
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2016.02.24 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C84 H64 Br4.75 Cl2.27 N18 O21.25 Pb6, 12.2(O), 0.5(N O3)'
_chemical_formula_sum            'C84 H64 Br4.74 Cl2.29 N18.50 O34.95 Pb6'
_chemical_formula_weight         3594.25
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -4.0753 8.5060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   31.6333(7)
_cell_length_b                   19.2972(5)
_cell_length_c                   19.7693(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     12067.9(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    11652
_cell_measurement_temperature    150
_cell_measurement_theta_max      70.883
_cell_measurement_theta_min      3.200
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    18.905
_exptl_absorpt_correction_T_max  01235
_exptl_absorpt_correction_T_min  0.0351
_exptl_absorpt_correction_type   Sphere
_exptl_absorpt_process_details   
;
C.W.Dwiggins Jr Acta Cryst.(1975) A31,146-148) 
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.978
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             6695
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_exptl_crystal_size_rad          0.1400
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0567
_diffrn_reflns_av_unetI/netI     0.0657
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            33506
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.883
_diffrn_reflns_theta_min         3.200
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  
;
Goniometer Xcalibur, detector: Ruby
Oxford Diffraction (2007). Oxford Diffraction Ltd.,
Xcalibur CCD system
;
_diffrn_measurement_method       'w\ scan'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8728
_reflns_number_total             11802
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55
;
_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2011 (Burla et al., 2007)'
_refine_diff_density_max         2.539
_refine_diff_density_min         -1.441
_refine_diff_density_rms         0.196
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     746
_refine_ls_number_reflns         11802
_refine_ls_number_restraints     814
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0475
_refine_ls_restrained_S_all      0.986
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0732P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1288
_refine_ls_wR_factor_ref         0.1410
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Shared sites
{Br6, Cl3}
{Br4, Cl4}
{Br5, Cl5}
{Br2, Cl2}
{Br1, Cl1}
{Br3, Cl6}
3. Restrained distances
 O9-O11
 2.2 with sigma of 0.02
 O5-N13 \\sim O3-N13 \\sim O2-N13
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(O11) \\sim Ueq, Uanis(O16) \\sim Ueq, Uanis(O20) \\sim Ueq, Uanis(O23)
\\sim Ueq, Uanis(O24) \\sim Ueq, Uanis(O27) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(Br6) = Uanis(Cl3)
Uanis(Br4) = Uanis(Cl4)
Uanis(Br5) = Uanis(Cl5)
Uanis(Br1) = Uanis(Cl1)
Uanis(Br2) = Uanis(Cl2)
Uanis(Br3) = Uanis(Cl6)
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(Cl1)=0.5*(1-FVAR(2))
 Sof(Br1)=0.5*FVAR(2)
 Fixed Sof: Br2(0.415) Br3(0.325) Br4(0.25) Br5(0.8) Br6(0.255) Cl2(0.085)
 Cl3(0.18) Cl4(0.25) Cl5(0.2) Cl6(0.25) O11(0.125) O16(0.6) O20(0.35) O23(0.5)
 O27(0.15) O2(0.25) O3(0.25) O5(0.25) N13(0.25)
7.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C12(H12A,H12B), C33(H33A,H33B), C44(H44A,H44B)
7.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C13(H13), C14(H14),
 C15(H15), C17(H17), C18(H18), C20(H20), C21(H21), C25(H25), C26(H26), C28(H28),
  C29(H29), C30(H30), C31(H31), C32(H32), C36(H36), C37(H37), C39(H39),
 C40(H40), C41(H41), C42(H42), C43(H43)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.43388(2) 0.2500 0.19106(3) 0.03968(14) Uani 1 2 d S TU P . .
Pb2 Pb 0.29762(2) 0.2500 0.37026(3) 0.03047(12) Uani 1 2 d S TU P . .
Pb3 Pb 0.40016(2) 0.2500 0.48935(3) 0.04461(16) Uani 1 2 d S TU P . .
Pb4 Pb 0.18805(2) 0.13432(2) 0.32781(2) 0.03225(10) Uani 1 1 d . U . . .
Pb5 Pb 0.14838(2) 0.2500 0.15017(3) 0.04704(16) Uani 1 2 d S TU P . .
Br1 Br 0.43725(5) 0.2500 0.04840(11) 0.0462(7) Uani 0.660(11) 2 d S TU P A 1
Br2 Br 0.39067(5) 0.2500 0.33582(10) 0.0526(5) Uani 0.83 2 d S TU P A 1
Br3 Br 0.21620(5) 0.2500 0.44433(9) 0.0385(4) Uani 0.65 2 d S TU P A 1
Br4 Br 0.11784(6) 0.2500 0.29164(12) 0.0443(5) Uani 0.5 2 d S TU P B 1
Br5 Br 0.17700(5) 0.09986(9) 0.18832(7) 0.0598(4) Uani 0.8 1 d . U . B 1
Br6 Br 0.18215(8) 0.2500 0.00649(14) 0.0506(6) Uani 0.51 2 d S TU P B 1
Cl1 Cl 0.43725(5) 0.2500 0.04840(11) 0.0462(7) Uani 0.340(11) 2 d S TU P A 2
Cl2 Cl 0.39067(5) 0.2500 0.33582(10) 0.0526(5) Uani 0.17 2 d S TU P A 2
Cl3 Cl 0.18215(8) 0.2500 0.00649(14) 0.0506(6) Uani 0.36 2 d S TU P B 2
Cl4 Cl 0.11784(6) 0.2500 0.29164(12) 0.0443(5) Uani 0.5 2 d S TU P B 2
Cl5 Cl 0.17700(5) 0.09986(9) 0.18832(7) 0.0598(4) Uani 0.2 1 d . U . B 2
Cl6 Cl 0.21620(5) 0.2500 0.44433(9) 0.0385(4) Uani 0.5 2 d S TU P A 2
O1A O 0.3782(2) 0.1745(4) 0.1741(4) 0.0486(17) Uani 1 1 d . U . . .
O1B O 0.4279(2) 0.1011(4) 0.2056(4) 0.0526(19) Uani 1 1 d . U . . .
O4A O 0.3335(2) 0.1784(4) 0.4755(4) 0.0467(16) Uani 1 1 d . U . . .
O4B O 0.3818(3) 0.1169(4) 0.5271(5) 0.064(2) Uani 1 1 d . U . . .
O6A O 0.2741(2) 0.1273(3) 0.3360(4) 0.0391(15) Uani 1 1 d . U . . .
O6B O 0.23458(19) 0.0326(3) 0.3337(3) 0.0356(14) Uani 1 1 d . U . . .
O7 O 0.1477(2) 0.0967(4) 0.4419(4) 0.055(2) Uani 1 1 d . U . . .
O8 O 0.1331(2) 0.0426(4) 0.3469(4) 0.0555(19) Uani 1 1 d . U . . .
O9 O 0.3730(3) 0.2500 0.6140(6) 0.068(3) Uani 1 2 d DS TU P A .
O10 O 0.4398(3) 0.2500 0.6168(6) 0.062(3) Uani 1 2 d S TU P A .
O11 O 0.4023(12) 0.2500 0.7114(13) 0.061(9) Uani 0.25 2 d DS TU P A .
O12 O 0.2925(3) 0.2500 0.2319(5) 0.041(2) Uani 1 2 d S TU P A .
O13 O 0.2397(3) 0.2500 0.1620(5) 0.053(3) Uani 1 2 d S TU P A .
O14 O 0.2292(3) 0.2500 0.2689(5) 0.045(2) Uani 1 2 d S TU P A .
O16 O 0.0673(6) 0.0593(11) 0.2350(12) 0.127(8) Uani 0.6 1 d . U . . .
O26 O 0.0671(3) 0.1519(7) 0.6268(6) 0.104(4) Uani 1 1 d . U . . .
O20 O 0.4054(5) -0.2500 0.2690(8) 0.062(4) Uani 0.7 2 d S TU P C 1
O21 O 0.1453(2) 0.1767(4) 0.5575(4) 0.0480(18) Uani 1 1 d . U . . .
O22 O 0.0192(5) -0.2500 0.3902(8) 0.100(5) Uani 1 2 d S TU P . .
O23 O 0.1370(5) -0.0862(9) 0.2763(10) 0.067(5) Uani 0.5 1 d . U . . .
O24 O 0.0865(5) -0.0589(9) 0.1517(7) 0.157(6) Uani 1 1 d . U . . .
O25 O 0.4675(3) 0.1568(7) 0.4561(6) 0.103(4) Uani 1 1 d . U . . .
O27 O 0.3029(15) -0.2500 0.241(2) 0.061(11) Uani 0.3 2 d S TU P D 1
N1 N -0.0464(2) -0.1879(4) 0.5579(4) 0.0332(15) Uani 1 1 d . U . . .
N2 N 0.0019(2) -0.1091(4) 0.5419(4) 0.0343(15) Uani 1 1 d . U . . .
N3 N 0.1890(2) -0.1877(4) 0.5333(4) 0.0386(17) Uani 1 1 d . U . . .
N4 N 0.2254(2) -0.0955(4) 0.5087(4) 0.0373(17) Uani 1 1 d . U . . .
N5 N 0.2652(2) -0.0964(4) 0.1746(4) 0.0347(16) Uani 1 1 d . U . . .
N6 N 0.4141(2) -0.1052(4) 0.3871(5) 0.0431(19) Uani 1 1 d . U . . .
N7 N 0.4528(2) -0.1878(4) 0.4305(5) 0.046(2) Uani 1 1 d . U . . .
N8 N 0.4048(4) 0.2500 0.6468(8) 0.067(4) Uani 1 2 d S TU P . .
N9 N 0.2330(2) -0.1875(4) 0.1403(4) 0.0337(16) Uani 1 1 d . U . . .
N10 N 0.2514(3) 0.2500 0.2264(5) 0.0205(16) Uani 1 2 d S TU P . .
C1 C -0.0721(4) -0.2500 0.5460(8) 0.039(3) Uani 1 2 d S TU P . .
H1A H -0.0963 -0.2500 0.5762 0.047 Uiso 1 2 calc RS T P . .
H1B H -0.0825 -0.2500 0.4998 0.047 Uiso 1 2 calc RS T P . .
C2 C -0.0200(3) -0.1593(5) 0.5116(5) 0.040(2) Uani 1 1 d . U . . .
H2 H -0.0176 -0.1725 0.4665 0.048 Uiso 1 1 calc R . . . .
C3 C -0.0095(3) -0.1072(5) 0.6091(5) 0.040(2) Uani 1 1 d . U . . .
H3 H 0.0016 -0.0773 0.6414 0.047 Uiso 1 1 calc R . . . .
C4 C -0.0399(3) -0.1565(5) 0.6204(6) 0.043(2) Uani 1 1 d . U . . .
H4 H -0.0532 -0.1668 0.6611 0.051 Uiso 1 1 calc R . . . .
C5 C 0.0405(4) -0.0784(7) 0.4424(6) 0.064(3) Uani 1 1 d . U . . .
H5 H 0.0250 -0.1109 0.4183 0.076 Uiso 1 1 calc R . . . .
C6 C 0.0716(4) -0.0376(6) 0.4097(6) 0.056(3) Uani 1 1 d . U . . .
H6 H 0.0759 -0.0424 0.3634 0.067 Uiso 1 1 calc R . . . .
C7 C 0.0952(3) 0.0084(5) 0.4452(5) 0.0369(18) Uani 1 1 d . U . . .
C8 C 0.0886(3) 0.0160(6) 0.5135(5) 0.045(2) Uani 1 1 d . U . . .
H8 H 0.1047 0.0474 0.5381 0.053 Uiso 1 1 calc R . . . .
C9 C 0.0581(3) -0.0231(5) 0.5453(6) 0.045(2) Uani 1 1 d . U . . .
H9 H 0.0540 -0.0181 0.5916 0.054 Uiso 1 1 calc R . . . .
C10 C 0.0338(3) -0.0691(5) 0.5098(5) 0.0364(19) Uani 1 1 d . U . . .
C11 C 0.1276(3) 0.0533(5) 0.4106(5) 0.0376(19) Uani 1 1 d . U . . .
C12 C 0.1745(4) -0.2500 0.5683(7) 0.039(3) Uani 1 2 d S TU P . .
H12A H 0.1438 -0.2500 0.5703 0.047 Uiso 1 2 calc RS T P . .
H12B H 0.1851 -0.2500 0.6143 0.047 Uiso 1 2 calc RS T P . .
C13 C 0.2230(3) -0.1503(5) 0.5483(5) 0.0364(19) Uani 1 1 d . U . . .
H13 H 0.2424 -0.1613 0.5820 0.044 Uiso 1 1 calc R . . . .
C14 C 0.1690(4) -0.1559(6) 0.4806(6) 0.054(3) Uani 1 1 d . U . . .
H14 H 0.1443 -0.1709 0.4596 0.065 Uiso 1 1 calc R . . . .
C15 C 0.1912(3) -0.0991(6) 0.4643(6) 0.051(3) Uani 1 1 d . U . . .
H15 H 0.1849 -0.0679 0.4298 0.061 Uiso 1 1 calc R . . . .
C16 C 0.2554(3) -0.0408(5) 0.5107(5) 0.0357(19) Uani 1 1 d . U . . .
C17 C 0.2407(3) 0.0274(5) 0.5009(5) 0.0355(19) Uani 1 1 d . U . . .
H17 H 0.2121 0.0368 0.4954 0.043 Uiso 1 1 calc R . . . .
C18 C 0.2706(3) 0.0796(5) 0.4999(4) 0.0348(19) Uani 1 1 d . U . . .
H18 H 0.2620 0.1248 0.4910 0.042 Uiso 1 1 calc R . . . .
C19 C 0.3125(3) 0.0668(5) 0.5118(5) 0.0358(19) Uani 1 1 d . U . . .
C20 C 0.3262(3) -0.0008(5) 0.5251(5) 0.039(2) Uani 1 1 d . U . . .
H20 H 0.3546 -0.0095 0.5342 0.047 Uiso 1 1 calc R . . . .
C21 C 0.2974(3) -0.0541(5) 0.5246(5) 0.0360(19) Uani 1 1 d . U . . .
H21 H 0.3061 -0.0992 0.5336 0.043 Uiso 1 1 calc R . . . .
C22 C 0.3446(3) 0.1230(5) 0.5032(5) 0.043(2) Uani 1 1 d . U . . .
C23 C 0.2703(3) 0.0616(5) 0.3383(5) 0.0329(18) Uani 1 1 d . U . . .
C24 C 0.3080(3) 0.0193(5) 0.3497(5) 0.0343(18) Uani 1 1 d . U . . .
C25 C 0.3041(3) -0.0535(5) 0.3535(5) 0.0361(19) Uani 1 1 d . U . . .
H25 H 0.2778 -0.0742 0.3479 0.043 Uiso 1 1 calc R . . . .
C26 C 0.3396(3) -0.0943(5) 0.3655(5) 0.036(2) Uani 1 1 d . U . . .
H26 H 0.3369 -0.1422 0.3684 0.044 Uiso 1 1 calc R . . . .
C27 C 0.3783(3) -0.0641(5) 0.3730(5) 0.038(2) Uani 1 1 d . U . . .
C28 C 0.3836(3) 0.0076(5) 0.3665(5) 0.041(2) Uani 1 1 d . U . . .
H28 H 0.4102 0.0276 0.3710 0.049 Uiso 1 1 calc R . . . .
C29 C 0.3488(3) 0.0479(5) 0.3534(5) 0.038(2) Uani 1 1 d . U . . .
H29 H 0.3523 0.0953 0.3467 0.046 Uiso 1 1 calc R . . . .
C30 C 0.4549(4) -0.0961(7) 0.3667(9) 0.079(5) Uani 1 1 d . U . . .
H30 H 0.4648 -0.0605 0.3392 0.095 Uiso 1 1 calc R . . . .
C31 C 0.4784(4) -0.1480(6) 0.3933(8) 0.064(3) Uani 1 1 d . U . . .
H31 H 0.5072 -0.1547 0.3869 0.077 Uiso 1 1 calc R . . . .
C32 C 0.4137(3) -0.1597(5) 0.4278(6) 0.043(2) Uani 1 1 d . U . . .
H32 H 0.3901 -0.1760 0.4511 0.051 Uiso 1 1 calc R . . . .
C33 C 0.4637(5) -0.2500 0.4705(9) 0.053(4) Uani 1 2 d S TU P . .
H33A H 0.4481 -0.2500 0.5128 0.063 Uiso 1 2 calc RS T P . .
H33B H 0.4937 -0.2500 0.4809 0.063 Uiso 1 2 calc RS T P . .
C34 C 0.3910(3) 0.1146(6) 0.1890(6) 0.043(2) Uani 1 1 d . U . . .
C35 C 0.3584(3) 0.0583(5) 0.1855(5) 0.0350(19) Uani 1 1 d . U . . .
C36 C 0.3153(3) 0.0764(5) 0.1813(5) 0.0321(18) Uani 1 1 d . U . . .
H36 H 0.3073 0.1227 0.1810 0.039 Uiso 1 1 calc R . . . .
C37 C 0.2849(3) 0.0250(5) 0.1778(5) 0.0351(19) Uani 1 1 d . U . . .
H37 H 0.2564 0.0361 0.1742 0.042 Uiso 1 1 calc R . . . .
C38 C 0.2979(3) -0.0428(5) 0.1796(4) 0.0304(17) Uani 1 1 d . U . . .
C39 C 0.3399(3) -0.0622(5) 0.1852(5) 0.036(2) Uani 1 1 d . U . . .
H39 H 0.3476 -0.1087 0.1872 0.043 Uiso 1 1 calc R . . . .
C40 C 0.3697(3) -0.0116(5) 0.1879(5) 0.037(2) Uani 1 1 d . U . . .
H40 H 0.3981 -0.0237 0.1913 0.045 Uiso 1 1 calc R . . . .
C41 C 0.2688(3) -0.1528(5) 0.1361(5) 0.0330(18) Uani 1 1 d . U . . .
H41 H 0.2924 -0.1654 0.1108 0.040 Uiso 1 1 calc R . . . .
C42 C 0.2264(3) -0.0955(5) 0.2033(6) 0.044(2) Uani 1 1 d . U . . .
H42 H 0.2158 -0.0615 0.2321 0.052 Uiso 1 1 calc R . . . .
C43 C 0.2060(3) -0.1527(5) 0.1827(6) 0.042(2) Uani 1 1 d . U . . .
H43 H 0.1788 -0.1661 0.1949 0.050 Uiso 1 1 calc R . . . .
C44 C 0.2238(4) -0.2500 0.1016(7) 0.035(3) Uani 1 2 d S TU P . .
H44A H 0.2406 -0.2500 0.0606 0.043 Uiso 1 2 calc RS T P . .
H44B H 0.1942 -0.2500 0.0886 0.043 Uiso 1 2 calc RS T P . .
O2 O 0.3432(13) -0.2500 0.2032(13) 0.101(9) Uani 0.5 2 d DS TU P E 2
O3 O 0.2849(16) -0.2500 0.2696(18) 0.126(13) Uani 0.5 2 d DS TU P E 2
O5 O 0.3609(13) -0.2500 0.3064(12) 0.092(9) Uani 0.5 2 d DS TU P E 2
N13 N 0.3270(12) -0.2500 0.2647(15) 0.102(9) Uani 0.5 2 d DS TU P E 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 Br1 2.822(2) . ?
Pb1 Br2 3.1716(19) . ?
Pb1 Cl1 2.822(2) . ?
Pb1 O1A 2.311(7) 8_565 ?
Pb1 O1A 2.311(7) . ?
Pb2 Br2 3.0212(17) . ?
Pb2 Br3 2.9629(17) . ?
Pb2 Cl2 3.0212(17) . ?
Pb2 Cl6 2.9629(17) . ?
Pb2 O4A 2.742(7) . ?
Pb2 O4A 2.742(7) 8_565 ?
Pb2 O6A 2.573(6) 8_565 ?
Pb2 O6A 2.573(6) . ?
Pb2 O12 2.740(10) . ?
Pb3 Br2 3.050(2) . ?
Pb3 Cl2 3.050(2) . ?
Pb3 O4A 2.536(7) . ?
Pb3 O4A 2.536(7) 8_565 ?
Pb3 O4B 2.736(8) . ?
Pb3 O4B 2.736(8) 8_565 ?
Pb3 O9 2.610(12) . ?
Pb4 Br4 3.2289(16) . ?
Pb4 Br5 2.8581(14) . ?
Pb4 Cl5 2.8581(14) . ?
Pb4 O6A 2.732(7) . ?
Pb4 O6B 2.457(6) . ?
Pb4 O7 2.692(7) . ?
Pb4 O8 2.509(7) . ?
Pb5 Br4 2.959(2) . ?
Pb5 Br5 3.1278(16) 8_565 ?
Pb5 Br5 3.1278(16) . ?
Pb5 Br6 3.035(3) . ?
Pb5 Cl3 3.035(3) . ?
Pb5 Cl4 2.959(2) . ?
Br4 Pb4 3.2289(16) 8_565 ?
O1A C34 1.258(13) . ?
O1B C34 1.242(12) . ?
O4A C22 1.253(12) . ?
O4B C22 1.274(13) . ?
O6A C23 1.275(11) . ?
O6B C23 1.264(11) . ?
O7 C11 1.221(11) . ?
O8 C11 1.289(12) . ?
O9 N8 1.197(16) . ?
O10 N8 1.258(16) . ?
O11 N8 1.28(3) . ?
O12 N10 1.304(12) . ?
O13 N10 1.325(14) . ?
O14 N10 1.096(13) . ?
N1 C1 1.467(10) . ?
N1 C2 1.356(12) . ?
N1 C4 1.393(13) . ?
N2 C2 1.334(12) . ?
N2 C3 1.377(13) . ?
N2 C10 1.420(11) . ?
N3 C12 1.461(11) . ?
N3 C13 1.330(12) . ?
N3 C14 1.366(13) . ?
N4 C13 1.318(12) . ?
N4 C15 1.395(12) . ?
N4 C16 1.421(12) . ?
N5 C38 1.465(11) . ?
N5 C41 1.333(12) . ?
N5 C42 1.352(11) . ?
N6 C27 1.411(11) . ?
N6 C30 1.363(14) . ?
N6 C32 1.324(13) . ?
N7 C31 1.336(14) . ?
N7 C32 1.353(12) . ?
N7 C33 1.479(12) . ?
N9 C41 1.320(11) . ?
N9 C43 1.372(12) . ?
N9 C44 1.457(10) . ?
C1 N1 1.467(10) 8 ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?
C3 C4 1.371(13) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C5 C6 1.417(14) . ?
C5 C10 1.361(15) . ?
C6 H6 0.9300 . ?
C6 C7 1.356(14) . ?
C7 C8 1.372(14) . ?
C7 C11 1.506(13) . ?
C8 H8 0.9300 . ?
C8 C9 1.377(13) . ?
C9 H9 0.9300 . ?
C9 C10 1.368(13) . ?
C12 N3 1.461(11) 8 ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C14 C15 1.341(15) . ?
C15 H15 0.9300 . ?
C16 C17 1.408(12) . ?
C16 C21 1.380(13) . ?
C17 H17 0.9300 . ?
C17 C18 1.382(13) . ?
C18 H18 0.9300 . ?
C18 C19 1.369(13) . ?
C19 C20 1.399(13) . ?
C19 C22 1.496(14) . ?
C20 H20 0.9300 . ?
C20 C21 1.376(13) . ?
C21 H21 0.9300 . ?
C23 C24 1.463(13) . ?
C24 C25 1.412(13) . ?
C24 C29 1.404(12) . ?
C25 H25 0.9300 . ?
C25 C26 1.392(13) . ?
C26 H26 0.9300 . ?
C26 C27 1.365(13) . ?
C27 C28 1.399(13) . ?
C28 H28 0.9300 . ?
C28 C29 1.374(13) . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?
C30 C31 1.354(16) . ?
C31 H31 0.9300 . ?
C32 H32 0.9300 . ?
C33 N7 1.479(12) 8 ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 C35 1.498(13) . ?
C35 C36 1.410(12) . ?
C35 C40 1.396(13) . ?
C36 H36 0.9300 . ?
C36 C37 1.384(12) . ?
C37 H37 0.9300 . ?
C37 C38 1.372(12) . ?
C38 C39 1.386(12) . ?
C39 H39 0.9300 . ?
C39 C40 1.358(13) . ?
C40 H40 0.9300 . ?
C41 H41 0.9300 . ?
C42 H42 0.9300 . ?
C42 C43 1.341(14) . ?
C43 H43 0.9300 . ?
C44 N9 1.457(10) 8 ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?
O2 N13 1.32(3) . ?
O3 N13 1.34(3) . ?
O5 N13 1.35(3) . ?

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
Br1 Pb1 Br2 156.64(5) . . ?
O1A Pb1 Br1 83.35(19) . . ?
O1A Pb1 Br1 83.36(19) 8_565 . ?
O1A Pb1 Br2 78.58(19) 8_565 . ?
O1A Pb1 Br2 78.58(19) . . ?
O1A Pb1 Cl1 83.35(19) . . ?
O1A Pb1 Cl1 83.36(19) 8_565 . ?
O1A Pb1 O1A 78.2(4) 8_565 . ?
Br3 Pb2 Br2 163.41(5) . . ?
Cl6 Pb2 Cl2 163.41(5) . . ?
O4A Pb2 Br2 76.58(15) 8_565 . ?
O4A Pb2 Br2 76.59(15) . . ?
O4A Pb2 Br3 89.12(15) 8_565 . ?
O4A Pb2 Br3 89.12(15) . . ?
O4A Pb2 Cl2 76.58(15) 8_565 . ?
O4A Pb2 Cl2 76.59(15) . . ?
O4A Pb2 Cl6 89.12(15) 8_565 . ?
O4A Pb2 Cl6 89.12(15) . . ?
O4A Pb2 O4A 60.5(3) . 8_565 ?
O6A Pb2 Br2 102.82(14) 8_565 . ?
O6A Pb2 Br2 102.82(14) . . ?
O6A Pb2 Br3 83.05(15) 8_565 . ?
O6A Pb2 Br3 83.05(15) . . ?
O6A Pb2 Cl2 102.82(14) 8_565 . ?
O6A Pb2 Cl2 102.82(14) . . ?
O6A Pb2 Cl6 83.05(15) . . ?
O6A Pb2 Cl6 83.05(15) 8_565 . ?
O6A Pb2 O4A 141.5(2) 8_565 . ?
O6A Pb2 O4A 81.7(2) 8_565 8_565 ?
O6A Pb2 O4A 141.5(2) . 8_565 ?
O6A Pb2 O4A 81.7(2) . . ?
O6A Pb2 O6A 134.0(3) . 8_565 ?
O6A Pb2 O12 73.76(17) . . ?
O6A Pb2 O12 73.76(17) 8_565 . ?
O12 Pb2 Br2 80.38(19) . . ?
O12 Pb2 Br3 116.21(19) . . ?
O12 Pb2 Cl2 80.38(19) . . ?
O12 Pb2 Cl6 116.21(19) . . ?
O12 Pb2 O4A 141.42(19) . . ?
O12 Pb2 O4A 141.42(19) . 8_565 ?
O4A Pb3 Br2 79.07(17) . . ?
O4A Pb3 Br2 79.07(17) 8_565 . ?
O4A Pb3 Cl2 79.07(17) 8_565 . ?
O4A Pb3 Cl2 79.07(17) . . ?
O4A Pb3 O4A 66.0(3) 8_565 . ?
O4A Pb3 O4B 48.9(2) 8_565 8_565 ?
O4A Pb3 O4B 48.9(2) . . ?
O4A Pb3 O4B 111.3(2) . 8_565 ?
O4A Pb3 O4B 111.3(2) 8_565 . ?
O4A Pb3 O9 80.1(3) . . ?
O4A Pb3 O9 80.1(3) 8_565 . ?
O4B Pb3 Br2 104.51(19) 8_565 . ?
O4B Pb3 Br2 104.51(19) . . ?
O4B Pb3 Cl2 104.51(19) 8_565 . ?
O4B Pb3 Cl2 104.51(19) . . ?
O4B Pb3 O4B 139.5(4) 8_565 . ?
O9 Pb3 Br2 155.1(2) . . ?
O9 Pb3 Cl2 155.1(2) . . ?
O9 Pb3 O4B 70.9(2) . . ?
O9 Pb3 O4B 70.9(2) . 8_565 ?
Br5 Pb4 Br4 82.13(5) . . ?
O6A Pb4 Br4 137.17(13) . . ?
O6A Pb4 Br5 99.65(15) . . ?
O6A Pb4 Cl5 99.65(15) . . ?
O6B Pb4 Br4 167.17(15) . . ?
O6B Pb4 Br5 86.14(15) . . ?
O6B Pb4 Cl5 86.14(15) . . ?
O6B Pb4 O6A 50.21(19) . . ?
O6B Pb4 O7 91.7(2) . . ?
O6B Pb4 O8 81.0(2) . . ?
O7 Pb4 Br4 92.64(19) . . ?
O7 Pb4 Br5 133.47(15) . . ?
O7 Pb4 Cl5 133.47(15) . . ?
O7 Pb4 O6A 114.2(2) . . ?
O8 Pb4 Br4 92.6(2) . . ?
O8 Pb4 Br5 84.03(18) . . ?
O8 Pb4 Cl5 84.03(18) . . ?
O8 Pb4 O6A 130.3(2) . . ?
O8 Pb4 O7 49.9(2) . . ?
Br4 Pb5 Br5 82.33(3) . . ?
Br4 Pb5 Br5 82.33(3) . 8_565 ?
Br4 Pb5 Br6 178.44(7) . . ?
Br5 Pb5 Br5 135.73(6) . 8_565 ?
Br6 Pb5 Br5 97.11(3) . 8_565 ?
Br6 Pb5 Br5 97.11(3) . . ?
Cl4 Pb5 Cl3 178.44(7) . . ?
Pb2 Br2 Pb1 128.55(6) . . ?
Pb2 Br2 Pb3 82.62(5) . . ?
Pb3 Br2 Pb1 148.82(6) . . ?
Pb4 Br4 Pb4 87.47(5) 8_565 . ?
Pb5 Br4 Pb4 89.13(4) . 8_565 ?
Pb5 Br4 Pb4 89.13(4) . . ?
Pb4 Br5 Pb5 93.01(4) . . ?
Pb2 Cl2 Pb3 82.62(5) . . ?
C34 O1A Pb1 107.4(6) . . ?
Pb3 O4A Pb2 98.7(2) . . ?
C22 O4A Pb2 151.4(7) . . ?
C22 O4A Pb3 100.6(6) . . ?
C22 O4B Pb3 90.5(6) . . ?
Pb2 O6A Pb4 104.9(2) . . ?
C23 O6A Pb2 159.1(7) . . ?
C23 O6A Pb4 87.5(5) . . ?
C23 O6B Pb4 100.7(5) . . ?
C11 O7 Pb4 90.4(6) . . ?
C11 O8 Pb4 97.3(6) . . ?
N8 O9 Pb3 103.6(9) . . ?
N10 O12 Pb2 98.2(7) . . ?
C2 N1 C1 124.4(10) . . ?
C2 N1 C4 109.3(8) . . ?
C4 N1 C1 125.5(10) . . ?
C2 N2 C3 108.5(8) . . ?
C2 N2 C10 124.4(9) . . ?
C3 N2 C10 127.0(8) . . ?
C13 N3 C12 126.6(9) . . ?
C13 N3 C14 107.5(9) . . ?
C14 N3 C12 125.9(9) . . ?
C13 N4 C15 106.9(8) . . ?
C13 N4 C16 128.1(8) . . ?
C15 N4 C16 125.0(8) . . ?
C41 N5 C38 123.6(8) . . ?
C41 N5 C42 109.1(8) . . ?
C42 N5 C38 127.2(8) . . ?
C30 N6 C27 129.0(10) . . ?
C32 N6 C27 123.9(9) . . ?
C32 N6 C30 107.0(9) . . ?
C31 N7 C32 107.6(9) . . ?
C31 N7 C33 128.3(11) . . ?
C32 N7 C33 124.1(11) . . ?
O9 N8 O10 119.0(14) . . ?
O9 N8 O11 119(2) . . ?
O10 N8 O11 122(2) . . ?
C41 N9 C43 108.8(8) . . ?
C41 N9 C44 123.9(9) . . ?
C43 N9 C44 127.1(9) . . ?
O12 N10 O13 111.0(10) . . ?
O14 N10 O12 125.0(11) . . ?
O14 N10 O13 124.0(10) . . ?
N1 C1 N1 109.5(10) 8 . ?
N1 C1 H1A 109.8 . . ?
N1 C1 H1A 109.8 8 . ?
N1 C1 H1B 109.8 8 . ?
N1 C1 H1B 109.8 . . ?
H1A C1 H1B 108.2 . . ?
N1 C2 H2 125.9 . . ?
N2 C2 N1 108.2(9) . . ?
N2 C2 H2 125.9 . . ?
N2 C3 H3 125.6 . . ?
C4 C3 N2 108.8(9) . . ?
C4 C3 H3 125.6 . . ?
N1 C4 H4 127.4 . . ?
C3 C4 N1 105.1(9) . . ?
C3 C4 H4 127.4 . . ?
C6 C5 H5 120.6 . . ?
C10 C5 H5 120.6 . . ?
C10 C5 C6 118.9(11) . . ?
C5 C6 H6 119.7 . . ?
C7 C6 C5 120.6(11) . . ?
C7 C6 H6 119.7 . . ?
C6 C7 C8 119.7(10) . . ?
C6 C7 C11 121.0(10) . . ?
C8 C7 C11 119.3(9) . . ?
C7 C8 H8 120.1 . . ?
C7 C8 C9 119.9(10) . . ?
C9 C8 H8 120.1 . . ?
C8 C9 H9 119.5 . . ?
C10 C9 C8 120.9(10) . . ?
C10 C9 H9 119.5 . . ?
C5 C10 N2 118.4(9) . . ?
C5 C10 C9 120.0(10) . . ?
C9 C10 N2 121.6(9) . . ?
O7 C11 O8 122.4(9) . . ?
O7 C11 C7 121.2(10) . . ?
O8 C11 C7 116.4(8) . . ?
N3 C12 N3 110.7(11) . 8 ?
N3 C12 H12A 109.5 . . ?
N3 C12 H12A 109.5 8 . ?
N3 C12 H12B 109.5 8 . ?
N3 C12 H12B 109.5 . . ?
H12A C12 H12B 108.1 . . ?
N3 C13 H13 124.8 . . ?
N4 C13 N3 110.4(9) . . ?
N4 C13 H13 124.8 . . ?
N3 C14 H14 126.0 . . ?
C15 C14 N3 108.0(10) . . ?
C15 C14 H14 126.0 . . ?
N4 C15 H15 126.4 . . ?
C14 C15 N4 107.2(10) . . ?
C14 C15 H15 126.4 . . ?
C17 C16 N4 117.9(8) . . ?
C21 C16 N4 120.7(8) . . ?
C21 C16 C17 121.3(9) . . ?
C16 C17 H17 121.4 . . ?
C18 C17 C16 117.2(9) . . ?
C18 C17 H17 121.4 . . ?
C17 C18 H18 119.1 . . ?
C19 C18 C17 121.8(9) . . ?
C19 C18 H18 119.1 . . ?
C18 C19 C20 120.2(9) . . ?
C18 C19 C22 120.4(9) . . ?
C20 C19 C22 119.1(9) . . ?
C19 C20 H20 120.4 . . ?
C21 C20 C19 119.3(9) . . ?
C21 C20 H20 120.4 . . ?
C16 C21 H21 120.0 . . ?
C20 C21 C16 120.0(9) . . ?
C20 C21 H21 120.0 . . ?
O4A C22 O4B 120.0(10) . . ?
O4A C22 C19 118.6(9) . . ?
O4B C22 C19 121.2(9) . . ?
O6A C23 C24 118.8(8) . . ?
O6B C23 O6A 121.6(9) . . ?
O6B C23 C24 119.6(8) . . ?
C25 C24 C23 119.4(8) . . ?
C29 C24 C23 122.5(9) . . ?
C29 C24 C25 118.0(9) . . ?
C24 C25 H25 120.0 . . ?
C26 C25 C24 120.0(9) . . ?
C26 C25 H25 120.0 . . ?
C25 C26 H26 119.9 . . ?
C27 C26 C25 120.1(9) . . ?
C27 C26 H26 119.9 . . ?
C26 C27 N6 120.1(9) . . ?
C26 C27 C28 121.3(9) . . ?
C28 C27 N6 118.6(9) . . ?
C27 C28 H28 120.6 . . ?
C29 C28 C27 118.8(9) . . ?
C29 C28 H28 120.6 . . ?
C24 C29 H29 119.2 . . ?
C28 C29 C24 121.6(9) . . ?
C28 C29 H29 119.2 . . ?
N6 C30 H30 126.0 . . ?
C31 C30 N6 108.0(11) . . ?
C31 C30 H30 126.0 . . ?
N7 C31 C30 107.8(10) . . ?
N7 C31 H31 126.1 . . ?
C30 C31 H31 126.1 . . ?
N6 C32 N7 109.4(9) . . ?
N6 C32 H32 125.3 . . ?
N7 C32 H32 125.3 . . ?
N7 C33 N7 108.5(13) . 8 ?
N7 C33 H33A 110.0 8 . ?
N7 C33 H33A 110.0 . . ?
N7 C33 H33B 110.0 . . ?
N7 C33 H33B 110.0 8 . ?
H33A C33 H33B 108.4 . . ?
O1A C34 C35 115.7(9) . . ?
O1B C34 O1A 123.9(10) . . ?
O1B C34 C35 120.4(10) . . ?
C36 C35 C34 119.2(9) . . ?
C40 C35 C34 121.6(8) . . ?
C40 C35 C36 119.2(9) . . ?
C35 C36 H36 120.0 . . ?
C37 C36 C35 119.9(9) . . ?
C37 C36 H36 120.0 . . ?
C36 C37 H37 120.9 . . ?
C38 C37 C36 118.2(8) . . ?
C38 C37 H37 120.9 . . ?
C37 C38 N5 117.3(8) . . ?
C37 C38 C39 123.2(9) . . ?
C39 C38 N5 119.5(8) . . ?
C38 C39 H39 120.8 . . ?
C40 C39 C38 118.4(9) . . ?
C40 C39 H39 120.8 . . ?
C35 C40 H40 119.4 . . ?
C39 C40 C35 121.1(9) . . ?
C39 C40 H40 119.4 . . ?
N5 C41 H41 126.1 . . ?
N9 C41 N5 107.8(8) . . ?
N9 C41 H41 126.1 . . ?
N5 C42 H42 126.3 . . ?
C43 C42 N5 107.4(9) . . ?
C43 C42 H42 126.3 . . ?
N9 C43 H43 126.6 . . ?
C42 C43 N9 106.9(8) . . ?
C42 C43 H43 126.6 . . ?
N9 C44 N9 111.6(10) . 8 ?
N9 C44 H44A 109.3 . . ?
N9 C44 H44A 109.3 8 . ?
N9 C44 H44B 109.3 . . ?
N9 C44 H44B 109.3 8 . ?
H44A C44 H44B 108.0 . . ?
O2 N13 O3 117(4) . . ?
O2 N13 O5 105(3) . . ?
O3 N13 O5 138(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pb1 O1A C34 O1B -3.8(14) . . . . ?
Pb1 O1A C34 C35 176.3(7) . . . . ?
Pb2 O4A C22 O4B 130.9(12) . . . . ?
Pb2 O4A C22 C19 -53.5(19) . . . . ?
Pb2 O6A C23 O6B 130.0(14) . . . . ?
Pb2 O6A C23 C24 -47(2) . . . . ?
Pb2 O12 N10 O13 180.000(0) . . . . ?
Pb2 O12 N10 O14 0.000(1) . . . . ?
Pb3 O4A C22 O4B -1.0(12) . . . . ?
Pb3 O4A C22 C19 174.6(8) . . . . ?
Pb3 O4B C22 O4A 0.9(11) . . . . ?
Pb3 O4B C22 C19 -174.6(9) . . . . ?
Pb3 O9 N8 O10 0.000(2) . . . . ?
Pb3 O9 N8 O11 180.000(6) . . . . ?
Pb4 O6A C23 O6B 2.7(9) . . . . ?
Pb4 O6A C23 C24 -174.5(8) . . . . ?
Pb4 O6B C23 O6A -3.1(11) . . . . ?
Pb4 O6B C23 C24 174.2(7) . . . . ?
Pb4 O7 C11 O8 1.7(11) . . . . ?
Pb4 O7 C11 C7 -179.3(8) . . . . ?
Pb4 O8 C11 O7 -1.9(12) . . . . ?
Pb4 O8 C11 C7 179.1(7) . . . . ?
O1A C34 C35 C36 -14.0(14) . . . . ?
O1A C34 C35 C40 167.6(10) . . . . ?
O1B C34 C35 C36 166.1(10) . . . . ?
O1B C34 C35 C40 -12.3(16) . . . . ?
O6A C23 C24 C25 179.0(9) . . . . ?
O6A C23 C24 C29 -4.7(15) . . . . ?
O6B C23 C24 C25 1.7(14) . . . . ?
O6B C23 C24 C29 178.0(9) . . . . ?
N2 C3 C4 N1 -0.2(11) . . . . ?
N3 C14 C15 N4 -0.8(14) . . . . ?
N4 C16 C17 C18 -177.1(8) . . . . ?
N4 C16 C21 C20 178.7(9) . . . . ?
N5 C38 C39 C40 178.2(8) . . . . ?
N5 C42 C43 N9 -0.9(12) . . . . ?
N6 C27 C28 C29 -179.5(9) . . . . ?
N6 C30 C31 N7 -1.0(18) . . . . ?
C1 N1 C2 N2 -172.6(8) . . . . ?
C1 N1 C4 C3 171.6(8) . . . . ?
C2 N1 C1 N1 83.3(14) . . . 8 ?
C2 N1 C4 C3 1.6(11) . . . . ?
C2 N2 C3 C4 -1.3(11) . . . . ?
C2 N2 C10 C5 5.5(15) . . . . ?
C2 N2 C10 C9 -173.3(9) . . . . ?
C3 N2 C2 N1 2.3(11) . . . . ?
C3 N2 C10 C5 180.0(11) . . . . ?
C3 N2 C10 C9 1.1(15) . . . . ?
C4 N1 C1 N1 -85.3(13) . . . 8 ?
C4 N1 C2 N2 -2.4(11) . . . . ?
C5 C6 C7 C8 -0.6(18) . . . . ?
C5 C6 C7 C11 -178.4(11) . . . . ?
C6 C5 C10 N2 178.5(10) . . . . ?
C6 C5 C10 C9 -2.6(19) . . . . ?
C6 C7 C8 C9 -0.1(16) . . . . ?
C6 C7 C11 O7 177.1(10) . . . . ?
C6 C7 C11 O8 -3.9(15) . . . . ?
C7 C8 C9 C10 -0.6(17) . . . . ?
C8 C7 C11 O7 -0.8(15) . . . . ?
C8 C7 C11 O8 178.3(10) . . . . ?
C8 C9 C10 N2 -179.1(9) . . . . ?
C8 C9 C10 C5 2.0(17) . . . . ?
C10 N2 C2 N1 177.6(8) . . . . ?
C10 N2 C3 C4 -176.4(8) . . . . ?
C10 C5 C6 C7 2(2) . . . . ?
C11 C7 C8 C9 177.8(9) . . . . ?
C12 N3 C13 N4 -176.5(9) . . . . ?
C12 N3 C14 C15 177.5(10) . . . . ?
C13 N3 C12 N3 -96.6(12) . . . 8 ?
C13 N3 C14 C15 -0.2(13) . . . . ?
C13 N4 C15 C14 1.5(13) . . . . ?
C13 N4 C16 C17 -138.9(10) . . . . ?
C13 N4 C16 C21 38.6(15) . . . . ?
C14 N3 C12 N3 86.1(14) . . . 8 ?
C14 N3 C13 N4 1.2(12) . . . . ?
C15 N4 C13 N3 -1.6(11) . . . . ?
C15 N4 C16 C17 38.6(14) . . . . ?
C15 N4 C16 C21 -143.9(10) . . . . ?
C16 N4 C13 N3 176.2(9) . . . . ?
C16 N4 C15 C14 -176.5(10) . . . . ?
C16 C17 C18 C19 -3.7(14) . . . . ?
C17 C16 C21 C20 -3.9(15) . . . . ?
C17 C18 C19 C20 0.3(15) . . . . ?
C17 C18 C19 C22 173.5(9) . . . . ?
C18 C19 C20 C21 1.5(15) . . . . ?
C18 C19 C22 O4A -10.5(15) . . . . ?
C18 C19 C22 O4B 165.0(10) . . . . ?
C19 C20 C21 C16 0.3(15) . . . . ?
C20 C19 C22 O4A 162.8(10) . . . . ?
C20 C19 C22 O4B -21.7(16) . . . . ?
C21 C16 C17 C18 5.5(14) . . . . ?
C22 C19 C20 C21 -171.9(9) . . . . ?
C23 C24 C25 C26 -178.8(9) . . . . ?
C23 C24 C29 C28 177.6(9) . . . . ?
C24 C25 C26 C27 -0.6(15) . . . . ?
C25 C24 C29 C28 -6.0(15) . . . . ?
C25 C26 C27 N6 178.2(9) . . . . ?
C25 C26 C27 C28 -2.3(16) . . . . ?
C26 C27 C28 C29 1.1(16) . . . . ?
C27 N6 C30 C31 179.1(12) . . . . ?
C27 N6 C32 N7 179.9(9) . . . . ?
C27 C28 C29 C24 3.2(16) . . . . ?
C29 C24 C25 C26 4.7(15) . . . . ?
C30 N6 C27 C26 145.9(13) . . . . ?
C30 N6 C27 C28 -33.6(18) . . . . ?
C30 N6 C32 N7 -3.7(13) . . . . ?
C31 N7 C32 N6 3.1(13) . . . . ?
C31 N7 C33 N7 -99.1(15) . . . 8 ?
C32 N6 C27 C26 -38.5(15) . . . . ?
C32 N6 C27 C28 142.1(11) . . . . ?
C32 N6 C30 C31 2.9(17) . . . . ?
C32 N7 C31 C30 -1.2(16) . . . . ?
C32 N7 C33 N7 83.7(16) . . . 8 ?
C33 N7 C31 C30 -178.8(13) . . . . ?
C33 N7 C32 N6 -179.2(10) . . . . ?
C34 C35 C36 C37 179.7(9) . . . . ?
C34 C35 C40 C39 179.4(9) . . . . ?
C35 C36 C37 C38 1.1(14) . . . . ?
C36 C35 C40 C39 1.0(15) . . . . ?
C36 C37 C38 N5 -179.0(8) . . . . ?
C36 C37 C38 C39 0.4(15) . . . . ?
C37 C38 C39 C40 -1.2(15) . . . . ?
C38 N5 C41 N9 -176.3(8) . . . . ?
C38 N5 C42 C43 176.6(9) . . . . ?
C38 C39 C40 C35 0.5(15) . . . . ?
C40 C35 C36 C37 -1.8(15) . . . . ?
C41 N5 C38 C37 136.3(10) . . . . ?
C41 N5 C38 C39 -43.1(13) . . . . ?
C41 N5 C42 C43 0.7(12) . . . . ?
C41 N9 C43 C42 0.8(12) . . . . ?
C41 N9 C44 N9 95.7(12) . . . 8 ?
C42 N5 C38 C37 -39.1(14) . . . . ?
C42 N5 C38 C39 141.5(10) . . . . ?
C42 N5 C41 N9 -0.2(11) . . . . ?
C43 N9 C41 N5 -0.4(11) . . . . ?
C43 N9 C44 N9 -88.9(13) . . . 8 ?
C44 N9 C41 N5 175.8(8) . . . . ?
C44 N9 C43 C42 -175.2(9) . . . . ?

_shelx_SHELXL_version_number     2014/8
_olex2_submission_special_instructions 'No special instructions were received'
_vrf_PLAT601_I                   
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of .        442 Ang3  
RESPONSE: Approximately 15% of the unit cell volume comprises 10 different 
sets of disordered solvents which could not be modelled as discrete 
atomic sites. We employed SQUEEZE procedure using PLATON program to 
calculate the contribution to the diffraction from the solvent region and 
thereby produced a set of solvent-free diffraction intensities. SQUEEZE 
estimated the total count of 625 electrons per unit cell.
;
####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1423049'
_audit_update_record             
;
2016-03-29 deposited with the CCDC.
2016-04-04 downloaded from the CCDC.
;
_audit_creation_date             2016-03-25
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2016.02.24 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C22 H20 N8 O17 Pb2, C22 H24 N6 O13 Pb2'
_chemical_formula_sum            'C44 H44 N14 O30 Pb4'
_chemical_formula_weight         2077.69
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -4.0753 8.5060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.0229(6)
_cell_length_b                   24.1691(7)
_cell_length_c                   19.4086(7)
_cell_angle_alpha                90
_cell_angle_beta                 109.221(4)
_cell_angle_gamma                90
_cell_volume                     6211.3(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    11561
_cell_measurement_temperature    293
_cell_measurement_theta_max      70.69
_cell_measurement_theta_min      3.81
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    21.556
_exptl_absorpt_correction_T_max  0.1186
_exptl_absorpt_correction_T_min  0.020
_exptl_absorpt_correction_type   Sphere
_exptl_absorpt_process_details   
;
C.W.Dwiggins Jr, Acta Cryst.(1975)
A31,146-148
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.222
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             3896
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_exptl_crystal_size_rad          0.0130
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0956
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11561
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.690
_diffrn_reflns_theta_min         3.806
_diffrn_ambient_temperature      293
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  
;
Goniometer Xcalibur, detector: Ruby
Oxford Diffraction (2007). Oxford Diffraction Ltd.,
Xcalibur CCD system
;
_diffrn_measurement_method       w\scan
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7772
_reflns_number_total             11561
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55
;
_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_refine_diff_density_max         2.689
_refine_diff_density_min         -1.517
_refine_diff_density_rms         0.234
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.951
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     842
_refine_ls_number_reflns         11561
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_gt           0.0712
_refine_ls_restrained_S_all      0.954
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1007P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1785
_refine_ls_wR_factor_ref         0.1985
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained planarity
 O18, O19, O20, N10
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
Uanis(O26) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O18) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(O3) \\sim Ueq, Uanis(O25) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Fixed Sof: Pb4(0.5) Pb5(0.5)
5.a Rotating group:
 O30(H30A,H30B), O3(H3A,H3B), O28(H28A,H28B), O29(H29A,H29B)
5.b Secondary CH2 refined with riding coordinates:
 C34(H34A,H34B), C35(H35A,H35B), C11A(H11B,H11A), C12(H12A,H12B)
5.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C26(H26), C27(H27), C29(H29), C30(H30), C32(H32), C33(H33),
 C36(H36), C37(H37), C38(H38), C40(H40), C41(H41), C43(H43), C44(H44), C3(H3),
 C4(H4), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C13(H13), C14(H14), C15(H15),
  C17(H17), C18(H18), C20(H20), C21(H21)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb3 Pb 0.48198(4) 0.10656(2) -0.08687(3) 0.05723(17) Uani 1 1 d . . . . .
O7 O 0.3130(12) 0.1121(5) -0.0654(9) 0.099(4) Uani 1 1 d . . . . .
O8 O 0.3129(11) 0.1896(5) -0.1109(6) 0.075(4) Uani 1 1 d . . . . .
O9 O 0.2102(10) 0.1763(6) -0.0580(8) 0.097(4) Uani 1 1 d . . . . .
O10 O 0.5218(9) 0.1776(4) 0.0282(6) 0.070(3) Uani 1 1 d . . . . .
O11 O 0.5144(9) 0.0881(4) 0.0422(7) 0.075(3) Uani 1 1 d . . . . .
O12 O 0.6253(13) 0.0302(7) -0.0442(10) 0.122(6) Uani 1 1 d . . . . .
O13 O 0.6971(11) -0.0169(5) -0.1152(10) 0.111(5) Uani 1 1 d . . . . .
O14 O 0.5590(10) 0.0298(5) -0.1674(9) 0.094(4) Uani 1 1 d . . . . .
O15 O 0.9216(9) 0.4860(4) 1.1579(8) 0.081(3) Uani 1 1 d . . . . .
O16 O 0.8361(13) 0.4092(4) 1.1364(8) 0.102(5) Uani 1 1 d . . . . .
O17 O 0.7616(9) 0.4876(5) 1.1461(7) 0.086(4) Uani 1 1 d . . . . .
O18 O 0.4628(18) 0.1780(4) -0.2298(7) 0.147(7) Uani 1 1 d . U . . .
O19 O 0.3377(13) 0.1091(5) -0.2211(7) 0.102(5) Uani 1 1 d . . . . .
O20 O 0.2653(8) 0.1808(4) -0.2880(6) 0.066(2) Uani 1 1 d . . . . .
O21 O 1.0202(12) 0.4205(5) 1.0625(7) 0.094(4) Uani 1 1 d . . . . .
O22 O 1.0054(10) 0.3313(5) 1.0848(6) 0.083(3) Uani 1 1 d . . . . .
O30 O 0.3915(11) 0.0164(5) -0.0848(8) 0.093(4) Uani 1 1 d . . . . .
H30A H 0.3263 0.0162 -0.1165 0.139 Uiso 1 1 d GR . . . .
H30B H 0.3873 0.0081 -0.0396 0.139 Uiso 1 1 d GR . . . .
N6 N 0.8403(12) 0.4608(6) 1.1448(8) 0.075(3) Uani 1 1 d . . . . .
N7 N 0.2860(10) 0.1649(6) -0.0859(11) 0.087(5) Uani 1 1 d . . . . .
N9 N 0.6282(16) 0.0129(6) -0.1093(13) 0.106(6) Uani 1 1 d . . . . .
N10 N 0.3416(12) 0.1553(5) -0.2489(8) 0.080(4) Uani 1 1 d . . . . .
N12 N 0.7150(8) 0.1887(5) 0.4864(6) 0.056(2) Uani 1 1 d . . . . .
N13 N 0.8367(9) 0.2907(4) 0.6324(7) 0.057(3) Uani 1 1 d . . . . .
N14 N 0.8692(9) 0.3300(4) 0.7376(7) 0.056(3) Uani 1 1 d . . . . .
N31 N 0.6808(8) 0.1553(4) 0.3790(6) 0.054(2) Uani 1 1 d . . . . .
C11 C 0.7228(11) 0.1136(5) 0.4241(9) 0.065(4) Uani 1 1 d . . . . .
H11 H 0.7339 0.0778 0.4108 0.078 Uiso 1 1 calc R . . . .
C23 C 1.0056(15) 0.3703(6) 1.0427(9) 0.076(4) Uani 1 1 d . . . . .
C24 C 0.5309(10) 0.1356(5) 0.0672(7) 0.051(3) Uani 1 1 d . . . . .
C25 C 0.5682(10) 0.1423(5) 0.1483(7) 0.054(3) Uani 1 1 d . . . . .
C26 C 0.5753(9) 0.0965(5) 0.1937(8) 0.053(3) Uani 1 1 d . . . . .
H26 H 0.5557 0.0620 0.1727 0.063 Uiso 1 1 calc R . . . .
C27 C 0.6098(12) 0.1009(5) 0.2676(8) 0.061(3) Uani 1 1 d . . . . .
H27 H 0.6101 0.0701 0.2964 0.073 Uiso 1 1 calc R . . . .
C28 C 0.6447(10) 0.1514(5) 0.2999(8) 0.057(3) Uani 1 1 d . . . . .
C29 C 0.6386(11) 0.1981(5) 0.2570(8) 0.057(3) Uani 1 1 d . . . . .
H29 H 0.6608 0.2323 0.2782 0.068 Uiso 1 1 calc R . . . .
C30 C 0.5982(10) 0.1926(5) 0.1813(8) 0.054(3) Uani 1 1 d . . . . .
H30 H 0.5915 0.2239 0.1523 0.064 Uiso 1 1 calc R . . . .
C32 C 0.6758(10) 0.2016(5) 0.4158(8) 0.057(3) Uani 1 1 d . . . . .
H32 H 0.6503 0.2357 0.3961 0.068 Uiso 1 1 calc R . . . .
C33 C 0.7462(11) 0.1339(6) 0.4934(8) 0.061(3) Uani 1 1 d . . . . .
H33 H 0.7770 0.1148 0.5367 0.073 Uiso 1 1 calc R . . . .
C34 C 0.7255(11) 0.2275(6) 0.5467(9) 0.062(4) Uani 1 1 d . . . . .
H34A H 0.7038 0.2096 0.5838 0.075 Uiso 1 1 calc R . . . .
H34B H 0.6825 0.2594 0.5287 0.075 Uiso 1 1 calc R . . . .
C35 C 0.8355(12) 0.2463(6) 0.5802(9) 0.069(4) Uani 1 1 d . . . . .
H35A H 0.8777 0.2157 0.6049 0.083 Uiso 1 1 calc R . . . .
H35B H 0.8607 0.2600 0.5425 0.083 Uiso 1 1 calc R . . . .
C36 C 0.8011(10) 0.3426(6) 0.6173(8) 0.061(3) Uani 1 1 d . . . . .
H36 H 0.7699 0.3577 0.5712 0.073 Uiso 1 1 calc R . . . .
C37 C 0.8195(12) 0.3686(6) 0.6820(9) 0.067(4) Uani 1 1 d . . . . .
H37 H 0.8028 0.4050 0.6889 0.080 Uiso 1 1 calc R . . . .
C38 C 0.8759(11) 0.2833(6) 0.7037(8) 0.062(3) Uani 1 1 d . . . . .
H38 H 0.9039 0.2505 0.7265 0.075 Uiso 1 1 calc R . . . .
C39 C 0.9014(11) 0.3406(5) 0.8137(8) 0.055(3) Uani 1 1 d . . . . .
C40 C 0.9061(11) 0.2970(6) 0.8618(8) 0.060(3) Uani 1 1 d . . . . .
H40 H 0.8846 0.2619 0.8437 0.073 Uiso 1 1 calc R . . . .
C41 C 0.9418(11) 0.3056(5) 0.9343(8) 0.058(3) Uani 1 1 d . . . . .
H41 H 0.9468 0.2763 0.9662 0.070 Uiso 1 1 calc R . . . .
C42 C 0.9717(12) 0.3594(5) 0.9621(8) 0.062(3) Uani 1 1 d . . . . .
C43 C 0.9675(12) 0.4023(6) 0.9138(9) 0.063(4) Uani 1 1 d . . . . .
H43 H 0.9874 0.4378 0.9312 0.076 Uiso 1 1 calc R . . . .
C44 C 0.9338(9) 0.3920(5) 0.8398(8) 0.052(3) Uani 1 1 d . . . . .
H44 H 0.9331 0.4204 0.8073 0.063 Uiso 1 1 calc R . . . .
Pb4 Pb 1.0490(4) 0.40336(18) 1.1894(3) 0.0522(6) Uani 0.5 1 d . . P A -2
Pb5 Pb 1.0729(5) 0.4027(2) 1.1977(4) 0.0804(18) Uani 0.5 1 d . . P A -1
Pb1 Pb 0.62767(4) 0.40779(2) 1.18077(3) 0.05580(17) Uani 1 1 d . . . . .
Pb2 Pb -0.05141(6) 0.11469(3) -0.09674(4) 0.0766(2) Uani 1 1 d . . . . .
O1 O 0.5616(8) 0.4362(4) 1.0461(5) 0.061(2) Uani 1 1 d . . . . .
O2 O 0.5437(8) 0.3488(4) 1.0724(6) 0.065(2) Uani 1 1 d . . . . .
O3 O 0.4547(12) 0.4488(8) 1.1606(9) 0.125(5) Uani 1 1 d . U . . .
H3A H 0.4383 0.4875 1.1813 0.188 Uiso 1 1 d GR . . . .
H3B H 0.3839 0.4306 1.1295 0.188 Uiso 1 1 d GR . . . .
O4 O 0.5485(9) 0.3197(4) 1.2218(7) 0.076(3) Uani 1 1 d . . . . .
O5 O 0.5704(10) 0.3835(4) 1.3041(6) 0.078(3) Uani 1 1 d . . . . .
O6 O 0.5230(8) 0.2997(4) 1.3229(6) 0.072(3) Uani 1 1 d . . . . .
O23 O -0.2459(15) 0.1064(5) -0.0986(14) 0.144(8) Uani 1 1 d . . . . .
O24 O -0.2080(9) 0.1913(5) -0.0984(9) 0.094(4) Uani 1 1 d . . . . .
O25 O -0.3431(10) 0.1667(5) -0.0813(10) 0.109(5) Uani 1 1 d . U . . .
O26 O -0.0386(12) 0.1037(6) 0.0281(8) 0.105(4) Uani 1 1 d . U . . .
O27 O 0.0250(9) 0.1833(4) 0.0160(6) 0.072(3) Uani 1 1 d . . . . .
O28 O 0.1175(12) 0.0815(6) -0.0345(8) 0.103(4) Uani 1 1 d . . . . .
H28A H 0.1279 0.0454 -0.0466 0.155 Uiso 1 1 d GR . . . .
H28B H 0.1350 0.0818 0.0162 0.155 Uiso 1 1 d GR . . . .
O29 O -0.0897(14) 0.0137(6) -0.0856(11) 0.127(6) Uani 1 1 d . . . . .
H29A H -0.0383 -0.0031 -0.0524 0.190 Uiso 1 1 d GR . . . .
H29B H -0.1007 -0.0040 -0.1279 0.190 Uiso 1 1 d GR . . . .
N1 N 0.3520(8) 0.3414(4) 0.7237(6) 0.048(2) Uani 1 1 d . . . . .
N2 N 0.3201(9) 0.2988(4) 0.6219(6) 0.054(2) Uani 1 1 d . . . . .
N3 N 0.2040(8) 0.1938(4) 0.4751(6) 0.052(2) Uani 1 1 d . . . . .
N4 N 0.1716(8) 0.1629(4) 0.3663(6) 0.053(2) Uani 1 1 d . . . . .
N5 N -0.2635(9) 0.1537(5) -0.0937(8) 0.066(3) Uani 1 1 d . . . . .
N8 N 0.5486(10) 0.3347(5) 1.2830(8) 0.071(3) Uani 1 1 d . . . . .
C1 C 0.5279(11) 0.3901(5) 1.0266(8) 0.056(3) Uani 1 1 d . . . . .
C2 C 0.4778(10) 0.3771(5) 0.9475(8) 0.054(3) Uani 1 1 d . . . . .
C3 C 0.4530(9) 0.3224(5) 0.9246(7) 0.048(3) Uani 1 1 d . . . . .
H3 H 0.4668 0.2941 0.9589 0.058 Uiso 1 1 calc R . . . .
C4 C 0.4073(10) 0.3102(5) 0.8502(7) 0.051(3) Uani 1 1 d . . . . .
H4 H 0.3896 0.2741 0.8346 0.061 Uiso 1 1 calc R . . . .
C5 C 0.3890(10) 0.3542(5) 0.8000(7) 0.051(3) Uani 1 1 d . . . . .
C6 C 0.4085(10) 0.4068(5) 0.8233(8) 0.052(3) Uani 1 1 d . . . . .
H6 H 0.3936 0.4355 0.7895 0.063 Uiso 1 1 calc R . . . .
C7 C 0.4507(10) 0.4185(5) 0.8970(7) 0.053(3) Uani 1 1 d . . . . .
H7 H 0.4606 0.4552 0.9123 0.063 Uiso 1 1 calc R . . . .
C8 C 0.3587(10) 0.2940(5) 0.6909(7) 0.051(3) Uani 1 1 d . . . . .
H8 H 0.3875 0.2617 0.7150 0.061 Uiso 1 1 calc R . . . .
C9 C 0.3045(10) 0.3792(5) 0.6690(7) 0.054(3) Uani 1 1 d . . . . .
H9 H 0.2895 0.4159 0.6754 0.064 Uiso 1 1 calc R . . . .
C10 C 0.2844(11) 0.3520(6) 0.6048(8) 0.062(3) Uani 1 1 d . . . . .
H10 H 0.2527 0.3663 0.5584 0.075 Uiso 1 1 calc R . . . .
C11A C 0.3167(10) 0.2555(5) 0.5663(8) 0.057(3) Uani 1 1 d . . . . .
H11B H 0.3644 0.2262 0.5883 0.069 Uiso 1 1 calc R . . . .
H11A H 0.3352 0.2714 0.5266 0.069 Uiso 1 1 calc R . . . .
C12 C 0.2095(11) 0.2318(5) 0.5371(7) 0.058(3) Uani 1 1 d . . . . .
H12A H 0.1940 0.2117 0.5754 0.070 Uiso 1 1 calc R . . . .
H12B H 0.1609 0.2616 0.5205 0.070 Uiso 1 1 calc R . . . .
C13 C 0.2360(12) 0.1404(6) 0.4821(9) 0.066(3) Uani 1 1 d . . . . .
H13 H 0.2669 0.1214 0.5253 0.079 Uiso 1 1 calc R . . . .
C14 C 0.2133(10) 0.1204(5) 0.4122(8) 0.057(3) Uani 1 1 d . . . . .
H14 H 0.2244 0.0846 0.3988 0.068 Uiso 1 1 calc R . . . .
C15 C 0.1632(9) 0.2081(5) 0.4045(7) 0.051(3) Uani 1 1 d . . . . .
H15 H 0.1350 0.2420 0.3860 0.061 Uiso 1 1 calc R . . . .
C16 C 0.1314(10) 0.1605(6) 0.2866(9) 0.060(3) Uani 1 1 d . . . . .
C17 C 0.0961(11) 0.1096(6) 0.2572(9) 0.062(3) Uani 1 1 d . . . . .
H17 H 0.0975 0.0788 0.2863 0.074 Uiso 1 1 calc R . . . .
C18 C 0.0584(12) 0.1068(6) 0.1817(9) 0.066(4) Uani 1 1 d . . . . .
H18 H 0.0360 0.0727 0.1602 0.079 Uiso 1 1 calc R . . . .
C19 C 0.0520(11) 0.1520(7) 0.1361(8) 0.064(4) Uani 1 1 d . . . . .
C20 C 0.0927(10) 0.2029(6) 0.1704(7) 0.054(3) Uani 1 1 d . . . . .
H20 H 0.0930 0.2336 0.1416 0.065 Uiso 1 1 calc R . . . .
C21 C 0.1317(9) 0.2075(5) 0.2454(8) 0.054(3) Uani 1 1 d . . . . .
H21 H 0.1573 0.2410 0.2676 0.065 Uiso 1 1 calc R . . . .
C22 C 0.0097(11) 0.1469(7) 0.0540(9) 0.066(4) 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
Pb3 O7 2.541(14) . ?
Pb3 O10 2.726(10) . ?
Pb3 O11 2.436(12) . ?
Pb3 O12 2.651(14) . ?
Pb3 O19 2.723(15) . ?
Pb3 O30 2.529(12) . ?
O7 N7 1.353(19) . ?
O8 N7 0.92(2) . ?
O9 N7 1.37(2) . ?
O10 C24 1.248(16) . ?
O11 C24 1.239(16) . ?
O12 N9 1.34(2) . ?
O13 N9 1.24(2) . ?
O14 N9 1.29(2) . ?
O15 N6 1.243(17) . ?
O15 Pb4 2.614(12) . ?
O16 N6 1.256(17) . ?
O17 N6 1.287(18) . ?
O18 N10 1.71(3) . ?
O19 N10 1.248(16) . ?
O20 N10 1.251(17) . ?
O21 C23 1.269(19) . ?
O21 Pb4 2.397(14) . ?
O21 Pb5 2.519(15) . ?
O22 C23 1.249(19) . ?
O22 Pb4 2.591(12) . ?
O22 Pb5 2.706(14) . ?
O30 H30A 0.9195 . ?
O30 H30B 0.9209 . ?
N12 C32 1.334(18) . ?
N12 C33 1.389(18) . ?
N12 C34 1.467(18) . ?
N13 C35 1.471(17) . ?
N13 C36 1.347(18) . ?
N13 C38 1.322(19) . ?
N14 C37 1.425(19) . ?
N14 C38 1.325(18) . ?
N14 C39 1.419(18) . ?
N31 C11 1.338(17) . ?
N31 C28 1.453(18) . ?
N31 C32 1.340(17) . ?
C11 H11 0.9300 . ?
C11 C33 1.37(2) . ?
C23 C42 1.50(2) . ?
C23 Pb4 2.824(18) . ?
C24 C25 1.495(17) . ?
C25 C26 1.397(18) . ?
C25 C30 1.373(17) . ?
C26 H26 0.9300 . ?
C26 C27 1.36(2) . ?
C27 H27 0.9300 . ?
C27 C28 1.387(19) . ?
C28 C29 1.389(18) . ?
C29 H29 0.9300 . ?
C29 C30 1.396(19) . ?
C30 H30 0.9300 . ?
C32 H32 0.9300 . ?
C33 H33 0.9300 . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C34 C35 1.53(2) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 H36 0.9300 . ?
C36 C37 1.35(2) . ?
C37 H37 0.9300 . ?
C38 H38 0.9300 . ?
C39 C40 1.394(18) . ?
C39 C44 1.361(18) . ?
C40 H40 0.9300 . ?
C40 C41 1.35(2) . ?
C41 H41 0.9300 . ?
C41 C42 1.416(19) . ?
C42 C43 1.387(19) . ?
C43 H43 0.9300 . ?
C43 C44 1.38(2) . ?
C44 H44 0.9300 . ?
Pb1 O1 2.564(10) . ?
Pb1 O2 2.491(10) . ?
Pb1 O3 2.528(14) . ?
Pb1 O4 2.643(10) . ?
Pb2 O23 2.723(17) . ?
Pb2 O26 2.383(14) . ?
Pb2 O27 2.672(11) . ?
Pb2 O28 2.414(15) . ?
Pb2 O29 2.523(15) . ?
O1 C1 1.222(16) . ?
O2 C1 1.306(16) . ?
O3 H3A 1.0725 . ?
O3 H3B 1.0722 . ?
O4 N8 1.242(17) . ?
O5 N8 1.253(16) . ?
O6 N8 1.276(15) . ?
O23 N5 1.180(16) . ?
O24 N5 1.221(16) . ?
O25 N5 1.257(16) . ?
O26 C22 1.26(2) . ?
O27 C22 1.21(2) . ?
O28 H28A 0.9294 . ?
O28 H28B 0.9315 . ?
O29 H29A 0.8923 . ?
O29 H29B 0.8925 . ?
N1 C5 1.431(17) . ?
N1 C8 1.330(14) . ?
N1 C9 1.392(17) . ?
N2 C8 1.274(17) . ?
N2 C10 1.379(16) . ?
N2 C11A 1.493(16) . ?
N3 C12 1.496(15) . ?
N3 C13 1.357(18) . ?
N3 C15 1.344(17) . ?
N4 C14 1.360(17) . ?
N4 C15 1.346(15) . ?
N4 C16 1.463(19) . ?
C1 C2 1.50(2) . ?
C2 C3 1.401(17) . ?
C2 C7 1.364(19) . ?
C3 H3 0.9300 . ?
C3 C4 1.405(18) . ?
C4 H4 0.9300 . ?
C4 C5 1.408(16) . ?
C5 C6 1.347(17) . ?
C6 H6 0.9300 . ?
C6 C7 1.387(18) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C9 C10 1.354(19) . ?
C10 H10 0.9300 . ?
C11A H11B 0.9700 . ?
C11A H11A 0.9700 . ?
C11A C12 1.53(2) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 H13 0.9300 . ?
C13 C14 1.38(2) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.380(19) . ?
C16 C21 1.39(2) . ?
C17 H17 0.9300 . ?
C17 C18 1.39(2) . ?
C18 H18 0.9300 . ?
C18 C19 1.39(2) . ?
C19 C20 1.424(19) . ?
C19 C22 1.51(2) . ?
C20 H20 0.9300 . ?
C20 C21 1.382(19) . ?
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
O7 Pb3 O10 77.5(4) . . ?
O7 Pb3 O12 129.6(4) . . ?
O7 Pb3 O19 73.5(5) . . ?
O11 Pb3 O7 73.1(4) . . ?
O11 Pb3 O10 49.8(3) . . ?
O11 Pb3 O12 71.7(5) . . ?
O11 Pb3 O19 144.8(4) . . ?
O11 Pb3 O30 75.6(4) . . ?
O12 Pb3 O10 104.6(5) . . ?
O12 Pb3 O19 124.3(5) . . ?
O19 Pb3 O10 131.1(4) . . ?
O30 Pb3 O7 62.8(4) . . ?
O30 Pb3 O10 119.9(4) . . ?
O30 Pb3 O12 74.2(5) . . ?
O30 Pb3 O19 79.4(4) . . ?
N7 O7 Pb3 100.8(11) . . ?
C24 O10 Pb3 86.4(7) . . ?
C24 O11 Pb3 100.4(8) . . ?
N9 O12 Pb3 100.2(13) . . ?
N6 O15 Pb4 100.6(9) . . ?
N10 O19 Pb3 108.0(11) . . ?
C23 O21 Pb4 95.8(10) . . ?
C23 O21 Pb5 96.6(10) . . ?
C23 O22 Pb4 87.3(10) . . ?
C23 O22 Pb5 88.4(10) . . ?
Pb3 O30 H30A 112.8 . . ?
Pb3 O30 H30B 113.1 . . ?
H30A O30 H30B 106.0 . . ?
O15 N6 O16 120.9(16) . . ?
O15 N6 O17 119.0(13) . . ?
O16 N6 O17 119.9(15) . . ?
O7 N7 O9 104.6(17) . . ?
O8 N7 O7 129.8(18) . . ?
O8 N7 O9 125.5(15) . . ?
O13 N9 O12 122(2) . . ?
O13 N9 O14 119(2) . . ?
O14 N9 O12 118.4(18) . . ?
O19 N10 O18 112.0(14) . . ?
O19 N10 O20 123.5(16) . . ?
O20 N10 O18 124.4(10) . . ?
C32 N12 C33 109.5(12) . . ?
C32 N12 C34 124.7(12) . . ?
C33 N12 C34 125.8(12) . . ?
C36 N13 C35 127.6(13) . . ?
C38 N13 C35 122.0(13) . . ?
C38 N13 C36 110.5(12) . . ?
C38 N14 C37 106.1(12) . . ?
C38 N14 C39 128.4(12) . . ?
C39 N14 C37 125.4(11) . . ?
C11 N31 C28 124.5(12) . . ?
C11 N31 C32 111.7(13) . . ?
C32 N31 C28 123.8(11) . . ?
N31 C11 H11 126.8 . . ?
N31 C11 C33 106.5(12) . . ?
C33 C11 H11 126.8 . . ?
O21 C23 C42 116.6(14) . . ?
O21 C23 Pb4 57.6(9) . . ?
O22 C23 O21 124.0(16) . . ?
O22 C23 C42 118.7(14) . . ?
O22 C23 Pb4 66.4(9) . . ?
C42 C23 Pb4 171.8(11) . . ?
O10 C24 C25 118.8(11) . . ?
O11 C24 O10 123.3(13) . . ?
O11 C24 C25 117.9(12) . . ?
C26 C25 C24 120.4(11) . . ?
C30 C25 C24 122.3(12) . . ?
C30 C25 C26 117.3(12) . . ?
C25 C26 H26 118.9 . . ?
C27 C26 C25 122.1(11) . . ?
C27 C26 H26 118.9 . . ?
C26 C27 H27 120.1 . . ?
C26 C27 C28 119.7(12) . . ?
C28 C27 H27 120.1 . . ?
C27 C28 N31 118.9(12) . . ?
C27 C28 C29 120.1(14) . . ?
C29 C28 N31 120.9(12) . . ?
C28 C29 H29 120.8 . . ?
C28 C29 C30 118.5(13) . . ?
C30 C29 H29 120.8 . . ?
C25 C30 C29 122.1(12) . . ?
C25 C30 H30 118.9 . . ?
C29 C30 H30 118.9 . . ?
N12 C32 N31 106.1(11) . . ?
N12 C32 H32 127.0 . . ?
N31 C32 H32 127.0 . . ?
N12 C33 H33 126.9 . . ?
C11 C33 N12 106.2(12) . . ?
C11 C33 H33 126.9 . . ?
N12 C34 H34A 109.5 . . ?
N12 C34 H34B 109.5 . . ?
N12 C34 C35 110.6(10) . . ?
H34A C34 H34B 108.1 . . ?
C35 C34 H34A 109.5 . . ?
C35 C34 H34B 109.5 . . ?
N13 C35 C34 106.9(11) . . ?
N13 C35 H35A 110.3 . . ?
N13 C35 H35B 110.3 . . ?
C34 C35 H35A 110.3 . . ?
C34 C35 H35B 110.3 . . ?
H35A C35 H35B 108.6 . . ?
N13 C36 H36 126.6 . . ?
N13 C36 C37 106.8(14) . . ?
C37 C36 H36 126.6 . . ?
N14 C37 H37 126.4 . . ?
C36 C37 N14 107.2(13) . . ?
C36 C37 H37 126.4 . . ?
N13 C38 N14 109.4(12) . . ?
N13 C38 H38 125.3 . . ?
N14 C38 H38 125.3 . . ?
C40 C39 N14 119.2(12) . . ?
C44 C39 N14 120.3(12) . . ?
C44 C39 C40 120.3(14) . . ?
C39 C40 H40 120.0 . . ?
C41 C40 C39 120.1(13) . . ?
C41 C40 H40 120.0 . . ?
C40 C41 H41 119.9 . . ?
C40 C41 C42 120.1(13) . . ?
C42 C41 H41 119.9 . . ?
C41 C42 C23 120.7(13) . . ?
C43 C42 C23 120.0(13) . . ?
C43 C42 C41 119.3(14) . . ?
C42 C43 H43 120.3 . . ?
C44 C43 C42 119.4(13) . . ?
C44 C43 H43 120.3 . . ?
C39 C44 C43 120.7(13) . . ?
C39 C44 H44 119.7 . . ?
C43 C44 H44 119.7 . . ?
O15 Pb4 C23 94.4(5) . . ?
O21 Pb4 O15 75.9(4) . . ?
O21 Pb4 O22 52.8(4) . . ?
O21 Pb4 C23 26.6(4) . . ?
O22 Pb4 O15 111.3(5) . . ?
O22 Pb4 C23 26.2(4) . . ?
O21 Pb5 O22 50.2(4) . . ?
O1 Pb1 O4 118.5(4) . . ?
O2 Pb1 O1 51.8(3) . . ?
O2 Pb1 O3 86.0(5) . . ?
O2 Pb1 O4 70.4(4) . . ?
O3 Pb1 O1 74.4(4) . . ?
O3 Pb1 O4 83.5(5) . . ?
O26 Pb2 O23 75.3(7) . . ?
O26 Pb2 O27 50.3(4) . . ?
O26 Pb2 O28 73.8(5) . . ?
O26 Pb2 O29 75.7(6) . . ?
O27 Pb2 O23 100.8(5) . . ?
O28 Pb2 O23 142.7(5) . . ?
O28 Pb2 O27 74.5(4) . . ?
O28 Pb2 O29 80.7(5) . . ?
O29 Pb2 O23 71.9(5) . . ?
O29 Pb2 O27 124.7(5) . . ?
C1 O1 Pb1 92.5(8) . . ?
C1 O2 Pb1 93.7(8) . . ?
Pb1 O3 H3A 126.7 . . ?
Pb1 O3 H3B 126.2 . . ?
H3A O3 H3B 107.1 . . ?
N8 O4 Pb1 100.6(8) . . ?
N5 O23 Pb2 99.3(11) . . ?
C22 O26 Pb2 99.5(11) . . ?
C22 O27 Pb2 86.8(9) . . ?
Pb2 O28 H28A 113.3 . . ?
Pb2 O28 H28B 113.7 . . ?
H28A O28 H28B 105.3 . . ?
Pb2 O29 H29A 111.0 . . ?
Pb2 O29 H29B 111.2 . . ?
H29A O29 H29B 107.4 . . ?
C8 N1 C5 128.5(11) . . ?
C8 N1 C9 106.9(11) . . ?
C9 N1 C5 124.5(10) . . ?
C8 N2 C10 109.5(11) . . ?
C8 N2 C11A 126.6(10) . . ?
C10 N2 C11A 123.9(12) . . ?
C13 N3 C12 125.1(12) . . ?
C15 N3 C12 123.7(10) . . ?
C15 N3 C13 111.2(11) . . ?
C14 N4 C16 126.5(11) . . ?
C15 N4 C14 110.4(12) . . ?
C15 N4 C16 122.9(12) . . ?
O23 N5 O24 124.1(14) . . ?
O23 N5 O25 118.7(13) . . ?
O24 N5 O25 117.2(12) . . ?
O4 N8 O5 120.7(12) . . ?
O4 N8 O6 118.4(12) . . ?
O5 N8 O6 120.9(14) . . ?
O1 C1 O2 121.7(14) . . ?
O1 C1 C2 120.8(12) . . ?
O2 C1 C2 117.1(11) . . ?
C3 C2 C1 120.4(12) . . ?
C7 C2 C1 120.6(11) . . ?
C7 C2 C3 118.9(13) . . ?
C2 C3 H3 119.8 . . ?
C2 C3 C4 120.4(12) . . ?
C4 C3 H3 119.8 . . ?
C3 C4 H4 121.0 . . ?
C3 C4 C5 118.0(11) . . ?
C5 C4 H4 121.0 . . ?
C4 C5 N1 118.3(11) . . ?
C6 C5 N1 121.0(11) . . ?
C6 C5 C4 120.7(13) . . ?
C5 C6 H6 119.7 . . ?
C5 C6 C7 120.7(12) . . ?
C7 C6 H6 119.7 . . ?
C2 C7 C6 120.9(11) . . ?
C2 C7 H7 119.5 . . ?
C6 C7 H7 119.5 . . ?
N1 C8 H8 124.7 . . ?
N2 C8 N1 110.6(11) . . ?
N2 C8 H8 124.7 . . ?
N1 C9 H9 126.7 . . ?
C10 C9 N1 106.6(11) . . ?
C10 C9 H9 126.7 . . ?
N2 C10 H10 126.8 . . ?
C9 C10 N2 106.3(12) . . ?
C9 C10 H10 126.8 . . ?
N2 C11A H11B 109.9 . . ?
N2 C11A H11A 109.9 . . ?
N2 C11A C12 108.9(10) . . ?
H11B C11A H11A 108.3 . . ?
C12 C11A H11B 109.9 . . ?
C12 C11A H11A 109.9 . . ?
N3 C12 C11A 108.1(11) . . ?
N3 C12 H12A 110.1 . . ?
N3 C12 H12B 110.1 . . ?
C11A C12 H12A 110.1 . . ?
C11A C12 H12B 110.1 . . ?
H12A C12 H12B 108.4 . . ?
N3 C13 H13 127.0 . . ?
N3 C13 C14 105.9(13) . . ?
C14 C13 H13 127.0 . . ?
N4 C14 C13 106.8(12) . . ?
N4 C14 H14 126.6 . . ?
C13 C14 H14 126.6 . . ?
N3 C15 N4 105.6(11) . . ?
N3 C15 H15 127.2 . . ?
N4 C15 H15 127.2 . . ?
C17 C16 N4 115.7(13) . . ?
C17 C16 C21 124.1(15) . . ?
C21 C16 N4 120.1(12) . . ?
C16 C17 H17 121.9 . . ?
C16 C17 C18 116.1(14) . . ?
C18 C17 H17 121.9 . . ?
C17 C18 H18 118.1 . . ?
C17 C18 C19 123.8(14) . . ?
C19 C18 H18 118.1 . . ?
C18 C19 C20 116.8(14) . . ?
C18 C19 C22 121.9(14) . . ?
C20 C19 C22 121.3(14) . . ?
C19 C20 H20 119.3 . . ?
C21 C20 C19 121.4(13) . . ?
C21 C20 H20 119.3 . . ?
C16 C21 H21 121.2 . . ?
C20 C21 C16 117.6(12) . . ?
C20 C21 H21 121.2 . . ?
O26 C22 C19 117.5(16) . . ?
O27 C22 O26 122.7(16) . . ?
O27 C22 C19 119.8(14) . . ?

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
Pb3 O7 N7 O8 13(3) . . . . ?
Pb3 O7 N7 O9 -164.2(10) . . . . ?
Pb3 O10 C24 O11 -4.4(14) . . . . ?
Pb3 O10 C24 C25 172.5(11) . . . . ?
Pb3 O11 C24 O10 4.9(16) . . . . ?
Pb3 O11 C24 C25 -172.0(10) . . . . ?
Pb3 O12 N9 O13 167.9(13) . . . . ?
Pb3 O12 N9 O14 -9.4(18) . . . . ?
Pb3 O19 N10 O18 38.5(12) . . . . ?
Pb3 O19 N10 O20 -143.7(11) . . . . ?
O10 C24 C25 C26 177.3(12) . . . . ?
O10 C24 C25 C30 -4(2) . . . . ?
O11 C24 C25 C26 -5.7(19) . . . . ?
O11 C24 C25 C30 173.3(13) . . . . ?
O21 C23 C42 C41 -172.4(15) . . . . ?
O21 C23 C42 C43 6(2) . . . . ?
O22 C23 C42 C41 -1(3) . . . . ?
O22 C23 C42 C43 177.6(15) . . . . ?
N12 C34 C35 N13 172.0(12) . . . . ?
N13 C36 C37 N14 0.5(16) . . . . ?
N14 C39 C40 C41 176.4(12) . . . . ?
N14 C39 C44 C43 -178.4(12) . . . . ?
N31 C11 C33 N12 0.6(16) . . . . ?
N31 C28 C29 C30 -176.6(12) . . . . ?
C11 N31 C28 C27 29(2) . . . . ?
C11 N31 C28 C29 -155.0(13) . . . . ?
C11 N31 C32 N12 -0.6(15) . . . . ?
C23 C42 C43 C44 -178.4(14) . . . . ?
C24 C25 C26 C27 179.3(13) . . . . ?
C24 C25 C30 C29 -176.2(12) . . . . ?
C25 C26 C27 C28 -4(2) . . . . ?
C26 C25 C30 C29 3(2) . . . . ?
C26 C27 C28 N31 179.6(12) . . . . ?
C26 C27 C28 C29 4(2) . . . . ?
C27 C28 C29 C30 -1(2) . . . . ?
C28 N31 C11 C33 180.0(12) . . . . ?
C28 N31 C32 N12 179.4(11) . . . . ?
C28 C29 C30 C25 -2(2) . . . . ?
C30 C25 C26 C27 0(2) . . . . ?
C32 N12 C33 C11 -1.0(16) . . . . ?
C32 N12 C34 C35 -103.8(15) . . . . ?
C32 N31 C11 C33 0.0(16) . . . . ?
C32 N31 C28 C27 -150.7(13) . . . . ?
C32 N31 C28 C29 25.0(19) . . . . ?
C33 N12 C32 N31 1.0(15) . . . . ?
C33 N12 C34 C35 74.4(16) . . . . ?
C34 N12 C32 N31 179.4(11) . . . . ?
C34 N12 C33 C11 -179.4(12) . . . . ?
C35 N13 C36 C37 -179.4(13) . . . . ?
C35 N13 C38 N14 178.6(12) . . . . ?
C36 N13 C35 C34 -71.4(17) . . . . ?
C36 N13 C38 N14 -1.1(17) . . . . ?
C37 N14 C38 N13 1.3(16) . . . . ?
C37 N14 C39 C40 151.3(13) . . . . ?
C37 N14 C39 C44 -33(2) . . . . ?
C38 N13 C35 C34 108.9(16) . . . . ?
C38 N13 C36 C37 0.3(16) . . . . ?
C38 N14 C37 C36 -1.1(16) . . . . ?
C38 N14 C39 C40 -27(2) . . . . ?
C38 N14 C39 C44 148.7(14) . . . . ?
C39 N14 C37 C36 -179.7(12) . . . . ?
C39 N14 C38 N13 179.9(12) . . . . ?
C39 C40 C41 C42 2(2) . . . . ?
C40 C39 C44 C43 -3(2) . . . . ?
C40 C41 C42 C23 176.3(14) . . . . ?
C40 C41 C42 C43 -3(2) . . . . ?
C41 C42 C43 C44 0(2) . . . . ?
C42 C43 C44 C39 2(2) . . . . ?
C44 C39 C40 C41 1(2) . . . . ?
Pb4 O15 N6 O16 -12.7(17) . . . . ?
Pb4 O15 N6 O17 161.4(12) . . . . ?
Pb4 O21 C23 O22 3(2) . . . . ?
Pb4 O21 C23 C42 173.2(14) . . . . ?
Pb4 O22 C23 O21 -2.4(19) . . . . ?
Pb4 O22 C23 C42 -172.8(15) . . . . ?
Pb5 O21 C23 O22 10(2) . . . . ?
Pb5 O21 C23 C42 -179.8(13) . . . . ?
Pb5 O22 C23 O21 -9(2) . . . . ?
Pb5 O22 C23 C42 -179.3(15) . . . . ?
Pb1 O1 C1 O2 -5.9(14) . . . . ?
Pb1 O1 C1 C2 -178.2(11) . . . . ?
Pb1 O2 C1 O1 6.1(14) . . . . ?
Pb1 O2 C1 C2 178.7(10) . . . . ?
Pb1 O4 N8 O5 8.3(17) . . . . ?
Pb1 O4 N8 O6 -173.8(11) . . . . ?
Pb2 O23 N5 O24 9(2) . . . . ?
Pb2 O23 N5 O25 -169.1(15) . . . . ?
Pb2 O26 C22 O27 9.4(19) . . . . ?
Pb2 O26 C22 C19 -168.9(10) . . . . ?
Pb2 O27 C22 O26 -8.2(16) . . . . ?
Pb2 O27 C22 C19 170.0(12) . . . . ?
O1 C1 C2 C3 170.4(12) . . . . ?
O1 C1 C2 C7 -13(2) . . . . ?
O2 C1 C2 C3 -2.2(19) . . . . ?
O2 C1 C2 C7 174.2(12) . . . . ?
N1 C5 C6 C7 -175.6(12) . . . . ?
N1 C9 C10 N2 -0.2(16) . . . . ?
N2 C11A C12 N3 172.9(10) . . . . ?
N3 C13 C14 N4 1.8(15) . . . . ?
N4 C16 C17 C18 -179.7(12) . . . . ?
N4 C16 C21 C20 -179.9(11) . . . . ?
C1 C2 C3 C4 -179.1(12) . . . . ?
C1 C2 C7 C6 177.0(12) . . . . ?
C2 C3 C4 C5 0.9(18) . . . . ?
C3 C2 C7 C6 -6.5(19) . . . . ?
C3 C4 C5 N1 173.8(11) . . . . ?
C3 C4 C5 C6 -4.4(19) . . . . ?
C4 C5 C6 C7 2(2) . . . . ?
C5 N1 C8 N2 -177.6(11) . . . . ?
C5 N1 C9 C10 177.8(12) . . . . ?
C5 C6 C7 C2 3(2) . . . . ?
C7 C2 C3 C4 4.4(19) . . . . ?
C8 N1 C5 C4 -21.7(19) . . . . ?
C8 N1 C5 C6 156.5(13) . . . . ?
C8 N1 C9 C10 0.1(15) . . . . ?
C8 N2 C10 C9 0.2(16) . . . . ?
C8 N2 C11A C12 104.3(15) . . . . ?
C9 N1 C5 C4 161.2(12) . . . . ?
C9 N1 C5 C6 -20.6(19) . . . . ?
C9 N1 C8 N2 -0.1(15) . . . . ?
C10 N2 C8 N1 -0.1(16) . . . . ?
C10 N2 C11A C12 -78.5(16) . . . . ?
C11A N2 C8 N1 177.5(11) . . . . ?
C11A N2 C10 C9 -177.5(12) . . . . ?
C12 N3 C13 C14 177.6(12) . . . . ?
C12 N3 C15 N4 -179.3(11) . . . . ?
C13 N3 C12 C11A 81.6(15) . . . . ?
C13 N3 C15 N4 -1.2(14) . . . . ?
C14 N4 C15 N3 2.4(14) . . . . ?
C14 N4 C16 C17 27.2(18) . . . . ?
C14 N4 C16 C21 -152.0(13) . . . . ?
C15 N3 C12 C11A -100.6(14) . . . . ?
C15 N3 C13 C14 -0.4(16) . . . . ?
C15 N4 C14 C13 -2.7(15) . . . . ?
C15 N4 C16 C17 -146.6(13) . . . . ?
C15 N4 C16 C21 34.3(18) . . . . ?
C16 N4 C14 C13 -177.1(12) . . . . ?
C16 N4 C15 N3 177.0(10) . . . . ?
C16 C17 C18 C19 -2(2) . . . . ?
C17 C16 C21 C20 1(2) . . . . ?
C17 C18 C19 C20 4(2) . . . . ?
C17 C18 C19 C22 -179.7(13) . . . . ?
C18 C19 C20 C21 -3.3(19) . . . . ?
C18 C19 C22 O26 14(2) . . . . ?
C18 C19 C22 O27 -164.0(14) . . . . ?
C19 C20 C21 C16 1.0(19) . . . . ?
C20 C19 C22 O26 -169.3(15) . . . . ?
C20 C19 C22 O27 12(2) . . . . ?
C21 C16 C17 C18 -1(2) . . . . ?
C22 C19 C20 C21 -179.8(12) . . . . ?

_shelx_SHELXL_version_number     2014/8
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1423050'
_audit_update_record             
;
2016-03-29 deposited with the CCDC.
2016-04-04 downloaded from the CCDC.
;
_audit_creation_date             2015-08-30
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2015.08.17 svn.r3210 for OlexSys, GUI svn.r5083)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C17 H11 Cl N2 O4 Pb'
_chemical_formula_sum            'C17 H11 Cl N2 O4 Pb'
_chemical_formula_weight         549.92
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -4.0753 8.5060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   7.3476(4)
_cell_length_b                   17.9122(8)
_cell_length_c                   12.0710(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1588.68(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4054
_cell_measurement_temperature    150
_cell_measurement_theta_max      70.800
_cell_measurement_theta_min      4.417
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    22.443
_exptl_absorpt_correction_T_max  0.0970
_exptl_absorpt_correction_T_min  0.0190
_exptl_absorpt_correction_type   Sphere
_exptl_absorpt_process_details   
;
C.W.Dwiggins Jr. Acta Cryst.(1975), A31,146-148.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.299
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_crystal_size_rad          0.15
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3715
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.800
_diffrn_reflns_theta_min         4.417
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  
;
Goniometer Xcalibur, detector: Ruby
Oxford Diffraction (2007). Oxford Diffraction Ltd.,
Xcalibur CCD system
;
_diffrn_measurement_method       'w\ scan'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1270
_reflns_number_total             1553
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55
;
_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2011 (Burla et al., 2007)'
_refine_diff_density_max         2.329
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.235
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         1553
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0514
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0967P)²+0.2688P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1356
_refine_ls_wR_factor_ref         0.1469
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C9(H9), C7(H7), C8(H8)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.49149(6) -0.2500 0.17188(4) 0.0610(3) Uani 1 2 d S T P . .
Cl1 Cl 0.4670(5) -0.2500 -0.0438(3) 0.0773(8) Uani 1 2 d S T P . .
O1 O 0.7141(10) -0.1527(3) 0.1406(6) 0.0787(17) Uani 1 1 d . . . . .
O2 O 0.7311(14) -0.1374(4) 0.3217(5) 0.088(2) Uani 1 1 d . . . . .
N1 N 0.9361(11) 0.1894(3) 0.1444(6) 0.0627(14) Uani 1 1 d . . . . .
C1 C 0.7435(11) -0.1134(5) 0.2256(8) 0.0677(19) Uani 1 1 d . . . . .
C2 C 0.7935(11) -0.0332(4) 0.2056(7) 0.0657(17) Uani 1 1 d . . . . .
C3 C 0.8412(13) 0.0131(4) 0.2929(7) 0.0703(19) Uani 1 1 d . . . . .
H3 H 0.8410 -0.0058 0.3646 0.084 Uiso 1 1 calc R . . . .
C4 C 0.8891(12) 0.0873(4) 0.2755(7) 0.0686(19) Uani 1 1 d . . . . .
H4 H 0.9221 0.1181 0.3343 0.082 Uiso 1 1 calc R . . . .
C5 C 0.8860(12) 0.1138(4) 0.1679(6) 0.0651(19) Uani 1 1 d . . . . .
C6 C 0.8392(13) 0.0687(4) 0.0789(7) 0.073(2) Uani 1 1 d . . . . .
H6 H 0.8378 0.0875 0.0071 0.087 Uiso 1 1 calc R . . . .
C9 C 1.0349(14) 0.2117(5) 0.0568(9) 0.076(2) Uani 1 1 d . . . . .
H9 H 1.0926 0.1809 0.0057 0.092 Uiso 1 1 calc R . . . .
C7 C 0.7948(13) -0.0049(4) 0.1000(7) 0.073(2) Uani 1 1 d . . . . .
H7 H 0.7651 -0.0360 0.0411 0.088 Uiso 1 1 calc R . . . .
C8 C 0.8739(14) 0.2500 0.1977(9) 0.061(2) Uani 1 2 d S T P . .
H8 H 0.8006 0.2500 0.2605 0.073 Uiso 1 2 calc RS T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Cl1 2.610(3) . ?
Pb1 O1 2.420(6) 8 ?
Pb1 O1 2.420(6) . ?
O1 C1 1.263(11) . ?
O2 C1 1.240(10) . ?
N1 C5 1.433(10) . ?
N1 C9 1.343(12) . ?
N1 C8 1.343(9) . ?
C1 C2 1.503(12) . ?
C2 C3 1.387(11) . ?
C2 C7 1.372(11) . ?
C3 H3 0.9300 . ?
C3 C4 1.390(11) . ?
C4 H4 0.9300 . ?
C4 C5 1.384(11) . ?
C5 C6 1.386(11) . ?
C6 H6 0.9300 . ?
C6 C7 1.382(11) . ?
C9 C9 1.372(18) 8_565 ?
C9 H9 0.9300 . ?
C7 H7 0.9300 . ?
C8 N1 1.343(9) 8_565 ?
C8 H8 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
O1 Pb1 Cl1 83.73(16) 8 . ?
O1 Pb1 Cl1 83.73(16) . . ?
O1 Pb1 O1 92.1(3) 8 . ?
C1 O1 Pb1 112.9(6) . . ?
C9 N1 C5 125.2(7) . . ?
C8 N1 C5 125.6(7) . . ?
C8 N1 C9 108.7(7) . . ?
O1 C1 C2 116.3(8) . . ?
O2 C1 O1 123.7(9) . . ?
O2 C1 C2 120.0(9) . . ?
C3 C2 C1 120.8(7) . . ?
C7 C2 C1 120.3(8) . . ?
C7 C2 C3 118.8(7) . . ?
C2 C3 H3 119.3 . . ?
C2 C3 C4 121.5(8) . . ?
C4 C3 H3 119.3 . . ?
C3 C4 H4 121.2 . . ?
C5 C4 C3 117.7(7) . . ?
C5 C4 H4 121.2 . . ?
C4 C5 N1 120.4(7) . . ?
C4 C5 C6 122.2(7) . . ?
C6 C5 N1 117.4(7) . . ?
C5 C6 H6 120.9 . . ?
C7 C6 C5 118.1(8) . . ?
C7 C6 H6 120.9 . . ?
N1 C9 C9 107.3(5) . 8_565 ?
N1 C9 H9 126.4 . . ?
C9 C9 H9 126.4 8_565 . ?
C2 C7 C6 121.7(8) . . ?
C2 C7 H7 119.1 . . ?
C6 C7 H7 119.1 . . ?
N1 C8 N1 107.9(10) 8_565 . ?
N1 C8 H8 126.0 8_565 . ?
N1 C8 H8 126.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pb1 O1 C1 O2 30.3(12) . . . . ?
Pb1 O1 C1 C2 -148.8(6) . . . . ?
O1 C1 C2 C3 -175.3(8) . . . . ?
O1 C1 C2 C7 3.9(12) . . . . ?
O2 C1 C2 C3 5.5(14) . . . . ?
O2 C1 C2 C7 -175.3(10) . . . . ?
N1 C5 C6 C7 178.4(8) . . . . ?
C1 C2 C3 C4 179.5(8) . . . . ?
C1 C2 C7 C6 179.6(9) . . . . ?
C2 C3 C4 C5 0.6(13) . . . . ?
C3 C2 C7 C6 -1.2(14) . . . . ?
C3 C4 C5 N1 -179.2(8) . . . . ?
C3 C4 C5 C6 -0.8(14) . . . . ?
C4 C5 C6 C7 -0.1(14) . . . . ?
C5 N1 C9 C9 173.0(7) . . . 8_565 ?
C5 N1 C8 N1 -173.3(5) . . . 8_565 ?
C5 C6 C7 C2 1.0(14) . . . . ?
C9 N1 C5 C4 140.1(10) . . . . ?
C9 N1 C5 C6 -38.5(13) . . . . ?
C9 N1 C8 N1 -0.9(14) . . . 8_565 ?
C7 C2 C3 C4 0.3(13) . . . . ?
C8 N1 C5 C4 -48.8(14) . . . . ?
C8 N1 C5 C6 132.7(10) . . . . ?
C8 N1 C9 C9 0.6(8) . . . 8_565 ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 1423051'
_audit_update_record             
;
2016-03-29 deposited with the CCDC.
2016-04-04 downloaded from the CCDC.
;
_audit_creation_date             2016-03-26
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2016.02.24 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C17 H11 N3 O7 Pb'
_chemical_formula_sum            'C17 H11 N3 O7 Pb'
_chemical_formula_weight         576.48
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -4.0753 8.5060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_H-M_alt        'C m c 21'
_space_group_name_Hall           'C 2c -2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   17.2038(9)
_cell_length_b                   11.4575(6)
_cell_length_c                   8.4614(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1667.85(15)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1206
_cell_measurement_temperature    150
_cell_measurement_theta_max      70.923
_cell_measurement_theta_min      5.142
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    20.142
_exptl_absorpt_correction_T_max  0.1146
_exptl_absorpt_correction_T_min  0.0296
_exptl_absorpt_correction_type   Sphere
_exptl_absorpt_process_details   
;
C.W.Dwiggins Jr (Acta Cryst.(1975)A31,146-148 
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.296
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.07
_exptl_crystal_size_rad          0.1430
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0211
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            2042
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        68.700
_diffrn_reflns_theta_max         70.923
_diffrn_reflns_theta_min         5.142
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  
;
Goniometer Xcalibur, detector: Ruby
Oxford Diffraction (2007). Oxford Diffraction Ltd.,
Xcalibur CCD system
;
_diffrn_measurement_method       'w\ scan'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_source                   'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.864
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.977
_reflns_number_gt                1203
_reflns_number_total             1206
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55
;
_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2011 (Burla et al., 2007)'
_refine_diff_density_max         1.665
_refine_diff_density_min         -1.269
_refine_diff_density_rms         0.213
_refine_ls_abs_structure_details 
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_coef       0.00070(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/8 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         1206
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0430
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0889P)²+12.0491P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1149
_refine_ls_wR_factor_ref         0.1149
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 1.02(4) -0.02(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained planarity
 O4_$1, O3, N2, O4
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(N2) \\sim Ueq, Uanis(O4) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.001
5. Others
 Fixed U12: Pb1(0) O3(0) N2(0) C9(0)
 Fixed U13: Pb1(0) O3(0) C9(0)
 Fixed X: Pb1(0) O3(0) N2(0) C9(-0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C9(H9)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.0000 0.00990(5) 0.9995(14) 0.0390(4) Uani 1 2 d S T P . .
O1 O -0.1106(5) 0.1516(9) 1.0839(18) 0.050(2) Uani 1 1 d . . . . .
O2 O -0.0923(8) -0.0093(11) 1.222(2) 0.045(4) Uani 1 1 d . . . . .
O3 O 0.0000 -0.3710(14) 0.989(4) 0.092(7) Uani 1 2 d S T P . .
O4 O 0.0627(15) -0.2082(19) 0.9485(17) 0.137(7) Uani 1 1 d . U . . .
N1 N -0.4381(7) 0.1243(14) 1.445(2) 0.043(3) Uani 1 1 d . . . . .
N2 N 0.0000 -0.262(3) 0.9621(7) 0.090(8) Uani 1 2 d S TU P . .
C1 C -0.1337(8) 0.0818(13) 1.183(2) 0.043(3) Uani 1 1 d . . . . .
C2 C -0.2116(8) 0.0960(15) 1.2618(19) 0.037(3) Uani 1 1 d . . . . .
C3 C -0.2393(11) 0.0117(12) 1.366(3) 0.049(4) Uani 1 1 d . . . . .
H3 H -0.2085 -0.0513 1.3954 0.058 Uiso 1 1 calc R . . . .
C4 C -0.3140(10) 0.0238(13) 1.426(3) 0.044(3) Uani 1 1 d . . . . .
H4 H -0.3335 -0.0314 1.4962 0.053 Uiso 1 1 calc R . . . .
C5 C -0.3589(8) 0.1164(11) 1.383(2) 0.040(3) Uani 1 1 d . . . . .
C6 C -0.3318(8) 0.2029(14) 1.2810(19) 0.042(3) Uani 1 1 d . . . . .
H6 H -0.3627 0.2670 1.2564 0.051 Uiso 1 1 calc R . . . .
C7 C -0.2589(7) 0.1922(15) 1.218(2) 0.048(3) Uani 1 1 d . . . . .
H7 H -0.2405 0.2477 1.1474 0.057 Uiso 1 1 calc R . . . .
C8 C -0.4617(10) 0.1158(16) 1.601(2) 0.042(3) Uani 1 1 d . . . . .
H8 H -0.4295 0.1111 1.6895 0.050 Uiso 1 1 calc R . . . .
C9 C -0.5000 0.1283(19) 1.350(3) 0.042(5) Uani 1 2 d S T P . .
H9 H -0.5000 0.1329 1.2405 0.050 Uiso 1 2 calc RS T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 O1 2.601(10) . ?
Pb1 O1 2.601(10) 3 ?
Pb1 O2 2.470(15) . ?
Pb1 O2 2.470(15) 3 ?
Pb1 O4 2.76(2) 3 ?
Pb1 O4 2.76(2) . ?
O1 C1 1.225(18) . ?
O2 C1 1.30(2) . ?
O3 N2 1.27(3) . ?
O4 N2 1.25(3) . ?
N1 C5 1.464(18) . ?
N1 C8 1.39(2) . ?
N1 C9 1.332(19) . ?
N2 O4 1.25(3) 3 ?
C1 C2 1.507(18) . ?
C2 C3 1.39(3) . ?
C2 C7 1.42(2) . ?
C3 H3 0.9300 . ?
C3 C4 1.39(3) . ?
C4 H4 0.9300 . ?
C4 C5 1.36(2) . ?
C5 C6 1.39(2) . ?
C6 H6 0.9300 . ?
C6 C7 1.366(19) . ?
C7 H7 0.9300 . ?
C8 C8 1.32(4) 3_455 ?
C8 H8 0.9300 . ?
C9 N1 1.332(19) 3_455 ?
C9 H9 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
O1 Pb1 O1 94.0(5) 3 . ?
O1 Pb1 O4 153.6(6) . . ?
O1 Pb1 O4 108.8(5) 3 . ?
O1 Pb1 O4 108.8(5) . 3 ?
O1 Pb1 O4 153.6(6) 3 3 ?
O2 Pb1 O1 108.5(4) . 3 ?
O2 Pb1 O1 51.4(4) 3 3 ?
O2 Pb1 O1 108.5(4) 3 . ?
O2 Pb1 O1 51.4(4) . . ?
O2 Pb1 O2 80.0(6) . 3 ?
O2 Pb1 O4 106.9(6) 3 3 ?
O2 Pb1 O4 77.7(5) 3 . ?
O2 Pb1 O4 77.7(5) . 3 ?
O2 Pb1 O4 106.9(6) . . ?
O4 Pb1 O4 46.1(11) 3 . ?
C1 O1 Pb1 91.0(9) . . ?
C1 O2 Pb1 95.1(10) . . ?
N2 O4 Pb1 95.5(18) . . ?
C8 N1 C5 127.6(13) . . ?
C9 N1 C5 122.0(13) . . ?
C9 N1 C8 110.0(14) . . ?
O4 N2 O3 120.2(16) 3 . ?
O4 N2 O3 120.2(16) . . ?
O4 N2 O4 120(3) . 3 ?
O1 C1 O2 121.2(14) . . ?
O1 C1 C2 121.3(14) . . ?
O2 C1 C2 117.5(14) . . ?
C3 C2 C1 120.7(15) . . ?
C3 C2 C7 120.4(14) . . ?
C7 C2 C1 118.7(13) . . ?
C2 C3 H3 120.7 . . ?
C4 C3 C2 118.6(15) . . ?
C4 C3 H3 120.7 . . ?
C3 C4 H4 119.9 . . ?
C5 C4 C3 120.2(16) . . ?
C5 C4 H4 119.9 . . ?
C4 C5 N1 118.6(14) . . ?
C4 C5 C6 122.1(14) . . ?
C6 C5 N1 119.3(13) . . ?
C5 C6 H6 120.6 . . ?
C7 C6 C5 118.8(14) . . ?
C7 C6 H6 120.6 . . ?
C2 C7 H7 120.1 . . ?
C6 C7 C2 119.7(15) . . ?
C6 C7 H7 120.1 . . ?
N1 C8 H8 126.5 . . ?
C8 C8 N1 107.0(9) 3_455 . ?
C8 C8 H8 126.5 3_455 . ?
N1 C9 N1 106(2) 3_455 . ?
N1 C9 H9 126.9 3_455 . ?
N1 C9 H9 126.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pb1 O1 C1 O2 11.6(15) . . . . ?
Pb1 O1 C1 C2 -166.9(12) . . . . ?
Pb1 O2 C1 O1 -12.2(15) . . . . ?
Pb1 O2 C1 C2 166.2(11) . . . . ?
Pb1 O4 N2 O3 -161.6(15) . . . . ?
Pb1 O4 N2 O4 18.7(15) . . . 3 ?
O1 C1 C2 C3 175.6(16) . . . . ?
O1 C1 C2 C7 0(2) . . . . ?
O2 C1 C2 C3 -3(2) . . . . ?
O2 C1 C2 C7 -178.0(14) . . . . ?
N1 C5 C6 C7 -177.2(14) . . . . ?
C1 C2 C3 C4 -174.8(15) . . . . ?
C1 C2 C7 C6 176.0(14) . . . . ?
C2 C3 C4 C5 0(3) . . . . ?
C3 C2 C7 C6 1(2) . . . . ?
C3 C4 C5 N1 178.3(16) . . . . ?
C3 C4 C5 C6 -2(3) . . . . ?
C4 C5 C6 C7 3(2) . . . . ?
C5 N1 C8 C8 -173.6(15) . . . 3_455 ?
C5 N1 C9 N1 174.4(10) . . . 3_455 ?
C5 C6 C7 C2 -2(2) . . . . ?
C7 C2 C3 C4 0(3) . . . . ?
C8 N1 C5 C4 51(3) . . . . ?
C8 N1 C5 C6 -129(2) . . . . ?
C8 N1 C9 N1 1(3) . . . 3_455 ?
C9 N1 C5 C4 -121(2) . . . . ?
C9 N1 C5 C6 58(2) . . . . ?
C9 N1 C8 C8 -0.6(19) . . . 3_455 ?

_shelx_SHELXL_version_number     2014/8
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 1.02(4)
2 -0.02(4)

