# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2020

####################################################################### 
# 
# 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-Cl
_database_code_depnum_ccdc_archive 'CCDC 2022783'
loop_
_audit_author_name
_audit_author_address
'H. H. Li'
;Fuzhou University
China
;
_audit_update_record             
;
2020-08-12 deposited with the CCDC.	2020-10-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C48 H20 Cl2 O16 Pb4, 2(C3 H8 N)'
_chemical_formula_sum            'C54 H36 Cl2 N2 O16 Pb4'
_chemical_formula_weight         1868.55

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c
_space_group_name_Hall           -C2yc

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

_cell_length_a                   17.500(4)
_cell_length_b                   23.051(4)
_cell_length_c                   8.0270(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 116.673(4)
_cell_angle_gamma                90.00
_cell_volume                     2893.4(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    8750
_cell_measurement_theta_min      1.57
_cell_measurement_theta_max      24.97

_exptl_crystal_description       Block
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.145
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1728
_exptl_absorpt_coefficient_mu    11.762
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.25
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean None
_diffrn_standards_number         None
_diffrn_standards_interval_count 'not measured'
_diffrn_standards_interval_time  'not measured'
_diffrn_standards_decay_%        'not measured'
_diffrn_reflns_number            8750
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_sigmaI/netI    0.0224
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         1.57
_diffrn_reflns_theta_max         24.97
_reflns_number_total             2485
_reflns_number_gt                2352
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Nonius CAD4 software'
_computing_cell_refinement       'Nonius CAD4 software'
_computing_data_reduction        'XCAD (P.McArdle, 2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0261P)²+27.8324P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2485
_refine_ls_number_parameters     180
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0230
_refine_ls_R_factor_gt           0.0214
_refine_ls_wR_factor_ref         0.0570
_refine_ls_wR_factor_gt          0.0561
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_restrained_S_all      1.112
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.155226(11) 0.517174(8) 0.39966(2) 0.01368(8) Uani 1 1 d . . .
Cl1 Cl 0.0000 0.5000 0.0000 0.0699(11) Uani 1 2 d S . .
N1 N 0.0000 0.6945(11) -0.2500 0.139(8) Uani 1 2 d S . .
O1 O 0.2972(2) 0.54991(19) 0.6027(5) 0.0262(9) Uani 1 1 d . . .
O2 O 0.2247(2) 0.55597(16) 0.7689(5) 0.0186(8) Uani 1 1 d . . .
O3 O 0.1432(3) 0.62553(18) 0.3418(6) 0.0292(9) Uani 1 1 d . . .
O4 O 0.1941(3) 0.57257(16) 0.1832(5) 0.0220(8) Uani 1 1 d . . .
C1 C 0.2942(3) 0.5580(2) 0.7556(7) 0.0181(11) Uani 1 1 d . . .
C2 C 0.3774(3) 0.5692(3) 0.9258(7) 0.0216(12) Uani 1 1 d . . .
C3 C 0.3815(3) 0.5722(2) 1.1002(7) 0.0179(11) Uani 1 1 d . . .
H3 H 0.3313 0.5719 1.1134 0.021 Uiso 1 1 calc R . .
C4 C 0.4617(3) 0.5759(3) 1.2608(8) 0.0208(11) Uani 1 1 d . . .
C5 C 0.5318(4) 0.5761(4) 1.0571(8) 0.0393(18) Uani 1 1 d . . .
H5 H 0.5808 0.5785 1.0399 0.047 Uiso 1 1 calc R . .
C6 C 0.4528(4) 0.5726(4) 0.9057(8) 0.0403(19) Uani 1 1 d . . .
H6 H 0.4492 0.5724 0.7866 0.048 Uiso 1 1 calc R . .
C7 C 0.1776(3) 0.6213(2) 0.2337(7) 0.0191(11) Uani 1 1 d . . .
C8 C 0.2014(4) 0.6755(2) 0.1637(8) 0.0205(11) Uani 1 1 d . . .
C9 C 0.2041(4) 0.7295(3) 0.2536(8) 0.0250(12) Uani 1 1 d . . .
C10 C 0.2296(4) 0.7787(2) 0.1954(8) 0.0239(12) Uani 1 1 d . . .
H10 H 0.2319 0.8138 0.2547 0.029 Uiso 1 1 calc R . .
C11 C 0.2474(3) 0.7231(2) -0.0456(7) 0.0184(11) Uani 1 1 d . . .
C12 C 0.2221(3) 0.6725(2) 0.0172(7) 0.0188(11) Uani 1 1 d . . .
H12 H 0.2195 0.6371 -0.0407 0.023 Uiso 1 1 calc R . .
C13 C 0.0299(9) 0.6990(11) -0.395(3) 0.213(9) Uani 1 1 d U . .
H13A H 0.0829 0.6784 -0.3556 0.319 Uiso 1 1 calc R . .
H13B H 0.0385 0.7391 -0.4150 0.319 Uiso 1 1 calc R . .
H13C H -0.0122 0.6826 -0.5096 0.319 Uiso 1 1 calc R . .
C14 C 0.0000 0.6235(13) -0.2500 0.180(11) Uani 1 2 d SU . .
H14A H -0.0163 0.6033 -0.1708 0.216 Uiso 0.50 1 calc PR . .
H14B H 0.0163 0.6033 -0.3292 0.216 Uiso 0.50 1 calc PR . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pb1 0.01314(12) 0.01760(12) 0.01083(12) 0.00013(7) 0.00585(8) -0.00132(7)
Cl1 0.0169(11) 0.176(4) 0.0183(12) -0.0195(16) 0.0091(9) -0.0261(15)
N1 0.023(6) 0.23(2) 0.099(12) 0.000 -0.029(7) 0.000
O1 0.0192(19) 0.043(2) 0.0145(19) -0.0063(18) 0.0055(16) -0.0063(19)
O2 0.0165(18) 0.0199(19) 0.0183(19) -0.0033(16) 0.0067(15) -0.0023(15)
O3 0.037(2) 0.027(2) 0.032(2) 0.0074(19) 0.023(2) 0.0042(19)
O4 0.032(2) 0.018(2) 0.0188(19) -0.0009(15) 0.0138(17) -0.0059(16)
C1 0.020(3) 0.019(3) 0.012(2) -0.001(2) 0.005(2) -0.001(2)
C2 0.016(3) 0.034(3) 0.014(3) 0.000(2) 0.006(2) -0.003(2)
C3 0.013(2) 0.023(3) 0.015(3) 0.000(2) 0.004(2) 0.003(2)
C4 0.016(3) 0.031(3) 0.017(3) -0.001(2) 0.009(2) 0.000(2)
C5 0.017(3) 0.086(6) 0.015(3) 0.001(3) 0.008(2) -0.010(3)
C6 0.021(3) 0.087(6) 0.013(3) -0.002(3) 0.009(3) -0.011(3)
C7 0.020(3) 0.018(3) 0.015(3) 0.004(2) 0.004(2) -0.001(2)
C8 0.024(3) 0.017(3) 0.020(3) 0.002(2) 0.009(2) -0.003(2)
C9 0.034(3) 0.021(3) 0.024(3) 0.000(2) 0.018(3) -0.004(3)
C10 0.039(3) 0.017(3) 0.022(3) -0.003(2) 0.020(3) -0.002(2)
C11 0.019(3) 0.019(3) 0.017(3) 0.002(2) 0.008(2) 0.001(2)
C12 0.024(3) 0.013(2) 0.019(3) -0.001(2) 0.009(2) -0.003(2)
C13 0.050(7) 0.335(19) 0.176(15) 0.111(14) -0.019(9) -0.036(11)
C14 0.129(16) 0.156(18) 0.173(18) 0.000 -0.004(13) 0.000

_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 2.401(4) . ?
Pb1 O4 2.485(4) . ?
Pb1 O3 2.532(4) . ?
Pb1 O2 2.563(4) 6_565 ?
Pb1 C7 2.855(5) . ?
Pb1 Cl1 3.1628(5) . ?
N1 C13 1.48(2) 2_554 ?
N1 C13 1.48(2) . ?
N1 C14 1.64(3) . ?
O1 C1 1.266(6) . ?
O2 C1 1.269(6) . ?
O2 Pb1 2.563(4) 6_566 ?
O3 C7 1.263(7) . ?
O4 C7 1.270(7) . ?
C1 C2 1.506(7) . ?
C2 C3 1.371(8) . ?
C2 C6 1.401(8) . ?
C3 C4 1.419(7) . ?
C4 C5 1.414(8) 2_657 ?
C4 C4 1.427(10) 2_657 ?
C5 C6 1.374(9) . ?
C5 C4 1.414(8) 2_657 ?
C7 C8 1.504(7) . ?
C8 C12 1.379(8) . ?
C8 C9 1.428(8) . ?
C9 C10 1.374(8) . ?
C10 C11 1.430(7) 7_565 ?
C11 C12 1.416(7) . ?
C11 C11 1.424(11) 7_565 ?
C11 C10 1.430(7) 7_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 O4 77.79(13) . . ?
O1 Pb1 O3 77.89(15) . . ?
O4 Pb1 O3 52.50(13) . . ?
O1 Pb1 O2 87.04(13) . 6_565 ?
O4 Pb1 O2 73.90(12) . 6_565 ?
O3 Pb1 O2 126.14(12) . 6_565 ?
O1 Pb1 C7 74.68(15) . . ?
O4 Pb1 C7 26.36(14) . . ?
O3 Pb1 C7 26.25(14) . . ?
O2 Pb1 C7 99.91(14) 6_565 . ?
O1 Pb1 Cl1 152.11(9) . . ?
O4 Pb1 Cl1 74.63(9) . . ?
O3 Pb1 Cl1 88.54(10) . . ?
O2 Pb1 Cl1 81.45(8) 6_565 . ?
C7 Pb1 Cl1 82.36(11) . . ?
C13 N1 C13 172(3) 2_554 . ?
C13 N1 C14 94.0(15) 2_554 . ?
C13 N1 C14 94.0(15) . . ?
C1 O1 Pb1 102.9(3) . . ?
C1 O2 Pb1 135.0(3) . 6_566 ?
C7 O3 Pb1 91.3(3) . . ?
C7 O4 Pb1 93.3(3) . . ?
O1 C1 O2 122.4(5) . . ?
O1 C1 C2 117.4(5) . . ?
O2 C1 C2 120.3(4) . . ?
C3 C2 C6 119.6(5) . . ?
C3 C2 C1 121.4(5) . . ?
C6 C2 C1 118.9(5) . . ?
C2 C3 C4 120.5(5) . . ?
C5 C4 C3 121.8(5) 2_657 . ?
C5 C4 C4 118.7(6) 2_657 2_657 ?
C3 C4 C4 119.3(6) . 2_657 ?
C6 C5 C4 119.8(5) . 2_657 ?
C5 C6 C2 121.8(5) . . ?
O3 C7 O4 122.3(5) . . ?
O3 C7 C8 119.3(5) . . ?
O4 C7 C8 118.4(5) . . ?
O3 C7 Pb1 62.4(3) . . ?
O4 C7 Pb1 60.3(3) . . ?
C8 C7 Pb1 172.6(4) . . ?
C12 C8 C9 120.8(5) . . ?
C12 C8 C7 120.0(5) . . ?
C9 C8 C7 119.2(5) . . ?
C10 C9 C8 119.3(5) . . ?
C9 C10 C11 121.3(5) . 7_565 ?
C12 C11 C11 119.5(6) . 7_565 ?
C12 C11 C10 121.8(5) . 7_565 ?
C11 C11 C10 118.6(6) 7_565 7_565 ?
C8 C12 C11 120.4(5) . . ?

_diffrn_measured_fraction_theta_max 0.976
_diffrn_reflns_theta_full        24.97
_diffrn_measured_fraction_theta_full 0.976
_refine_diff_density_max         1.475
_refine_diff_density_min         -0.739
_refine_diff_density_rms         0.140
####################################################################### 
# 
# 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-Br
_database_code_depnum_ccdc_archive 'CCDC 2022784'
loop_
_audit_author_name
_audit_author_address
'H. H. Li'
;Fuzhou University
China
;
_audit_update_record             
;
2020-08-12 deposited with the CCDC.	2020-10-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H12 Br O8 Pb2, OH3'
_chemical_formula_sum            'C24 H15 Br O9 Pb2'
_chemical_formula_weight         941.68

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c
_space_group_name_Hall           -C2yc

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

_cell_length_a                   17.563(3)
_cell_length_b                   23.002(3)
_cell_length_c                   8.0489(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 116.980(2)
_cell_angle_gamma                90.00
_cell_volume                     2897.7(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    175(2)
_cell_measurement_reflns_used    7042
_cell_measurement_theta_min      1.77
_cell_measurement_theta_max      24.98

_exptl_crystal_description       Block
_exptl_crystal_colour            Brown
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.152
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1708
_exptl_absorpt_coefficient_mu    13.028
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.25
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      175(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean None
_diffrn_standards_number         None
_diffrn_standards_interval_count 'not measured'
_diffrn_standards_interval_time  'not measured'
_diffrn_standards_decay_%        'not measured'
_diffrn_reflns_number            7042
_diffrn_reflns_av_R_equivalents  0.0991
_diffrn_reflns_av_sigmaI/netI    0.0879
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         1.77
_diffrn_reflns_theta_max         24.98
_reflns_number_total             2343
_reflns_number_gt                2057
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Nonius CAD4 software'
_computing_cell_refinement       'Nonius CAD4 software'
_computing_data_reduction        'XCAD (P.McArdle, 2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1508P)²+91.2674P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2343
_refine_ls_number_parameters     165
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1000
_refine_ls_R_factor_gt           0.0938
_refine_ls_wR_factor_ref         0.2494
_refine_ls_wR_factor_gt          0.2446
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_restrained_S_all      1.079
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.34126(4) 0.48316(2) 0.59622(10) 0.0461(4) Uani 1 1 d . . .
Br1 Br 0.5000 0.5000 1.0000 0.157(3) Uani 1 2 d S . .
O1 O 0.2042(9) 0.4502(7) 0.404(2) 0.071(4) Uani 1 1 d . . .
O2 O 0.2747(11) 0.4437(7) 0.229(3) 0.069(4) Uani 1 1 d . . .
O3 O 0.3005(11) 0.4295(7) 0.820(2) 0.070(4) Uani 1 1 d . . .
O4 O 0.3537(12) 0.3737(7) 0.652(3) 0.076(4) Uani 1 1 d . . .
C1 C 0.2066(13) 0.4422(8) 0.244(3) 0.050(4) Uani 1 1 d . . .
C2 C 0.1189(16) 0.4312(9) 0.070(3) 0.063(5) Uani 1 1 d . . .
C3 C 0.1159(11) 0.4280(8) -0.109(3) 0.050(4) Uani 1 1 d . . .
H3 H 0.1666 0.4276 -0.1233 0.060 Uiso 1 1 calc R . .
C4 C 0.0407(15) 0.4255(10) -0.253(3) 0.067(5) Uani 1 1 d . . .
C5 C 0.0438(16) 0.4277(14) 0.072(6) 0.095(9) Uani 1 1 d . . .
H5 H 0.0488 0.4275 0.1949 0.114 Uiso 1 1 calc R . .
C6 C 0.0319(17) 0.4245(12) -0.449(3) 0.079(7) Uani 1 1 d . . .
H6 H 0.0792 0.4217 -0.4753 0.094 Uiso 1 1 calc R . .
C7 C 0.3170(18) 0.3786(9) 0.766(3) 0.068(6) Uani 1 1 d . . .
C8 C 0.2964(15) 0.3247(9) 0.833(4) 0.068(6) Uani 1 1 d . . .
C9 C 0.2771(14) 0.3274(8) 0.986(4) 0.066(6) Uani 1 1 d . . .
H9 H 0.2824 0.3628 1.0512 0.079 Uiso 1 1 calc R . .
C10 C 0.2503(16) 0.2767(9) 1.040(3) 0.068(6) Uani 1 1 d . . .
C11 C 0.268(2) 0.2221(11) 0.804(4) 0.084(8) Uani 1 1 d . . .
H11 H 0.2609 0.1869 0.7370 0.101 Uiso 1 1 calc R . .
C12 C 0.2937(15) 0.2696(9) 0.751(4) 0.067(5) Uani 1 1 d . . .
H12 H 0.3112 0.2666 0.6559 0.081 Uiso 1 1 calc R . .
O5 O 0.5000 0.296(9) 1.2500 1.1(3) Uani 1 2 d S . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pb1 0.0503(6) 0.0469(5) 0.0434(6) 0.0001(2) 0.0234(4) -0.0011(2)
Br1 0.079(3) 0.333(10) 0.064(3) -0.025(4) 0.038(3) -0.024(4)
O1 0.053(8) 0.087(10) 0.079(11) -0.003(8) 0.036(8) -0.002(7)
O2 0.067(10) 0.066(8) 0.076(10) 0.001(7) 0.035(8) -0.002(7)
O3 0.082(11) 0.068(9) 0.052(8) -0.003(7) 0.022(8) -0.021(8)
O4 0.101(12) 0.068(9) 0.081(10) 0.010(8) 0.059(9) 0.009(8)
C1 0.051(10) 0.058(9) 0.035(9) -0.004(7) 0.015(8) -0.002(8)
C2 0.087(15) 0.069(11) 0.039(10) 0.009(8) 0.034(10) 0.007(10)
C3 0.034(9) 0.064(10) 0.046(10) 0.001(8) 0.014(8) 0.006(7)
C4 0.071(13) 0.077(13) 0.064(13) 0.021(11) 0.040(12) 0.006(11)
C5 0.044(13) 0.11(2) 0.13(3) 0.010(19) 0.033(15) 0.016(13)
C6 0.069(15) 0.097(17) 0.040(11) -0.002(11) -0.001(11) 0.009(13)
C7 0.106(18) 0.050(10) 0.063(13) 0.005(9) 0.051(13) 0.006(10)
C8 0.073(14) 0.063(11) 0.084(16) -0.008(11) 0.049(13) -0.011(10)
C9 0.063(12) 0.044(9) 0.090(16) -0.012(10) 0.033(12) -0.007(8)
C10 0.083(14) 0.056(10) 0.068(14) 0.009(9) 0.036(12) -0.003(10)
C11 0.14(2) 0.064(12) 0.082(16) -0.011(11) 0.080(17) -0.002(14)
C12 0.074(14) 0.063(11) 0.078(15) -0.007(10) 0.044(12) -0.010(10)
O5 0.02(2) 1.1(4) 1.6(6) 0.000 -0.26(10) 0.000

_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 2.321(15) . ?
Pb1 O3 2.537(16) . ?
Pb1 O2 2.543(16) 6_566 ?
Pb1 O4 2.549(16) . ?
Pb1 Br1 3.2037(8) . ?
Pb1 Br1 3.2374(8) 2_656 ?
Br1 Pb1 3.2037(8) 5_667 ?
Br1 Pb1 3.2374(8) 2_656 ?
Br1 Pb1 3.2374(8) 6_566 ?
O1 C1 1.32(3) . ?
O2 C1 1.26(3) . ?
O2 Pb1 2.543(16) 6_565 ?
O3 C7 1.32(3) . ?
O4 C7 1.35(3) . ?
C1 C2 1.56(3) . ?
C2 C5 1.33(4) . ?
C2 C3 1.42(3) . ?
C3 C4 1.30(3) . ?
C3 H3 0.9500 . ?
C4 C4 1.45(5) 2_554 ?
C4 C6 1.51(4) . ?
C5 C6 1.25(4) 2_554 ?
C5 H5 0.9500 . ?
C6 C5 1.25(4) 2_554 ?
C6 H6 0.9500 . ?
C7 C8 1.46(3) . ?
C8 C12 1.42(3) . ?
C8 C9 1.43(4) . ?
C9 C10 1.39(3) . ?
C9 H9 0.9500 . ?
C10 C10 1.38(5) 7_557 ?
C10 C11 1.43(3) 7_557 ?
C11 C12 1.33(3) . ?
C11 C10 1.43(3) 7_557 ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?

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 O3 76.9(6) . . ?
O1 Pb1 O2 87.7(6) . 6_566 ?
O3 Pb1 O2 72.1(5) . 6_566 ?
O1 Pb1 O4 77.0(6) . . ?
O3 Pb1 O4 54.9(5) . . ?
O2 Pb1 O4 126.8(5) 6_566 . ?
O1 Pb1 Br1 151.4(4) . . ?
O3 Pb1 Br1 74.6(3) . . ?
O2 Pb1 Br1 81.3(4) 6_566 . ?
O4 Pb1 Br1 88.6(4) . . ?
O1 Pb1 Br1 128.7(4) . 2_656 ?
O3 Pb1 Br1 141.1(4) . 2_656 ?
O2 Pb1 Br1 129.1(4) 6_566 2_656 ?
O4 Pb1 Br1 98.4(4) . 2_656 ?
Br1 Pb1 Br1 77.33(2) . 2_656 ?
Pb1 Br1 Pb1 180.0 . 5_667 ?
Pb1 Br1 Pb1 100.97(2) . 2_656 ?
Pb1 Br1 Pb1 79.03(2) 5_667 2_656 ?
Pb1 Br1 Pb1 79.03(2) . 6_566 ?
Pb1 Br1 Pb1 100.97(2) 5_667 6_566 ?
Pb1 Br1 Pb1 180.0 2_656 6_566 ?
C1 O1 Pb1 102.3(12) . . ?
C1 O2 Pb1 134.4(13) . 6_565 ?
C7 O3 Pb1 91.5(13) . . ?
C7 O4 Pb1 90.5(12) . . ?
O2 C1 O1 123.0(18) . . ?
O2 C1 C2 120.8(17) . . ?
O1 C1 C2 116.1(17) . . ?
C5 C2 C3 115(3) . . ?
C5 C2 C1 125(2) . . ?
C3 C2 C1 119.0(19) . . ?
C4 C3 C2 117(2) . . ?
C4 C3 H3 121.3 . . ?
C2 C3 H3 121.3 . . ?
C3 C4 C4 126(3) . 2_554 ?
C3 C4 C6 121(2) . . ?
C4 C4 C6 113(3) 2_554 . ?
C6 C5 C2 134(4) 2_554 . ?
C6 C5 H5 112.9 2_554 . ?
C2 C5 H5 112.9 . . ?
C5 C6 C4 113(3) 2_554 . ?
C5 C6 H6 123.3 2_554 . ?
C4 C6 H6 123.3 . . ?
O3 C7 O4 122.6(19) . . ?
O3 C7 C8 120.2(19) . . ?
O4 C7 C8 117.1(18) . . ?
C12 C8 C9 118(2) . . ?
C12 C8 C7 123(2) . . ?
C9 C8 C7 118.6(19) . . ?
C10 C9 C8 118.6(19) . . ?
C10 C9 H9 120.7 . . ?
C8 C9 H9 120.7 . . ?
C10 C10 C9 122(3) 7_557 . ?
C10 C10 C11 118(2) 7_557 7_557 ?
C9 C10 C11 120(2) . 7_557 ?
C12 C11 C10 121(2) . 7_557 ?
C12 C11 H11 119.6 . . ?
C10 C11 H11 119.6 7_557 . ?
C11 C12 C8 122(2) . . ?
C11 C12 H12 118.9 . . ?
C8 C12 H12 118.9 . . ?

_diffrn_measured_fraction_theta_max 0.917
_diffrn_reflns_theta_full        24.98
_diffrn_measured_fraction_theta_full 0.917
_refine_diff_density_max         5.311
_refine_diff_density_min         -2.525
_refine_diff_density_rms         0.414
####################################################################### 
# 
# 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-I
_database_code_depnum_ccdc_archive 'CCDC 2022787'
loop_
_audit_author_name
_audit_author_address
'H. H. Li'
;Fuzhou University
China
;
_audit_update_record             
;
2020-08-12 deposited with the CCDC.	2020-10-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C48 H24 I2 O16 Pb4, 2(C3 H9 N)'
_chemical_formula_sum            'C54 H42 I2 N2 O16 Pb4'
_chemical_formula_weight         2057.50

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c
_space_group_name_Hall           -C2yc

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

_cell_length_a                   17.442(3)
_cell_length_b                   22.968(4)
_cell_length_c                   7.9938(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 116.630(2)
_cell_angle_gamma                90.00
_cell_volume                     2862.6(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    175(2)
_cell_measurement_reflns_used    4303
_cell_measurement_theta_min      1.77
_cell_measurement_theta_max      25.02

_exptl_crystal_description       Block
_exptl_crystal_colour            Red
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.387
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1884
_exptl_absorpt_coefficient_mu    12.874
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.25
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      175(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean None
_diffrn_standards_number         None
_diffrn_standards_interval_count 'not measured'
_diffrn_standards_interval_time  'not measured'
_diffrn_standards_decay_%        'not measured'
_diffrn_reflns_number            4303
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_sigmaI/netI    0.0633
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         1.77
_diffrn_reflns_theta_max         25.02
_reflns_number_total             2396
_reflns_number_gt                2230
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Nonius CAD4 software'
_computing_cell_refinement       'Nonius CAD4 software'
_computing_data_reduction        'XCAD (P.McArdle, 2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1715P)²+17.4833P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2396
_refine_ls_number_parameters     171
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0808
_refine_ls_R_factor_gt           0.0790
_refine_ls_wR_factor_ref         0.2221
_refine_ls_wR_factor_gt          0.2167
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_restrained_S_all      1.085
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.15524(3) 0.482859(17) 0.39955(5) 0.0449(4) Uani 1 1 d . . .
I1 I 0.0000 0.5000 0.0000 0.249(3) Uani 1 2 d S . .
O1 O 0.2970(6) 0.4509(4) 0.6020(11) 0.060(2) Uani 1 1 d . . .
O2 O 0.2244(6) 0.4448(4) 0.7703(12) 0.0500(19) Uani 1 1 d . . .
O3 O 0.1443(6) 0.3749(4) 0.3442(14) 0.0570(19) Uani 1 1 d . . .
O4 O 0.1929(6) 0.4274(4) 0.1814(13) 0.054(2) Uani 1 1 d . . .
N1 N 0.0000 0.3063(19) -0.2500 0.24(3) Uani 1 2 d S . .
C1 C 0.2975(8) 0.4416(5) 0.7589(17) 0.052(3) Uani 1 1 d . . .
C2 C 0.3781(8) 0.4311(5) 0.9256(18) 0.054(3) Uani 1 1 d . . .
C3 C 0.4508(10) 0.4272(10) 0.902(2) 0.076(4) Uani 1 1 d . . .
H3 H 0.4456 0.4260 0.7783 0.091 Uiso 1 1 calc R . .
C4 C 0.5328(10) 0.4247(9) 1.054(2) 0.070(4) Uani 1 1 d . . .
H4 H 0.5824 0.4228 1.0335 0.084 Uiso 1 1 calc R . .
C5 C 0.5406(8) 0.4252(6) 1.2435(17) 0.053(3) Uani 1 1 d . . .
C6 C 0.3836(9) 0.4278(5) 1.1019(16) 0.055(3) Uani 1 1 d . . .
H6 H 0.3322 0.4273 1.1155 0.066 Uiso 1 1 calc R . .
C7 C 0.1755(8) 0.3787(5) 0.2310(16) 0.050(3) Uani 1 1 d . . .
C8 C 0.2019(8) 0.3243(5) 0.1649(17) 0.050(2) Uani 1 1 d . . .
C9 C 0.2214(7) 0.3285(5) 0.0168(16) 0.050(2) Uani 1 1 d . . .
H9 H 0.2176 0.3647 -0.0439 0.060 Uiso 1 1 calc R . .
C10 C 0.2475(7) 0.2767(5) -0.0434(16) 0.049(2) Uani 1 1 d . . .
C11 C 0.2283(9) 0.2211(6) 0.1956(19) 0.058(3) Uani 1 1 d . . .
H11 H 0.2286 0.1851 0.2542 0.070 Uiso 1 1 calc R . .
C12 C 0.2051(9) 0.2708(5) 0.2538(17) 0.057(3) Uani 1 1 d . . .
H12 H 0.1910 0.2694 0.3556 0.068 Uiso 1 1 calc R . .
C13 C 0.029(4) 0.301(3) -0.429(10) 0.22(2) Uiso 1 1 d . . .
H13A H 0.0326 0.2595 -0.4560 0.329 Uiso 1 1 calc R . .
H13B H 0.0842 0.3195 -0.3920 0.329 Uiso 1 1 calc R . .
H13C H -0.0149 0.3198 -0.5410 0.329 Uiso 1 1 calc R . .
C14 C 0.0000 0.373(3) -0.2500 0.19(2) Uiso 1 2 d S . .
H14A H -0.0147 0.3871 -0.1524 0.288 Uiso 0.50 1 calc PR . .
H14B H -0.0424 0.3871 -0.3723 0.288 Uiso 0.50 1 calc PR . .
H14C H 0.0571 0.3871 -0.2253 0.288 Uiso 0.50 1 calc PR . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pb1 0.0495(5) 0.0492(5) 0.0401(5) -0.00010(12) 0.0237(3) 0.00129(13)
I1 0.206(5) 0.423(10) 0.155(4) 0.033(5) 0.114(4) 0.043(6)
O1 0.060(5) 0.080(6) 0.039(4) 0.001(4) 0.023(4) -0.002(4)
O2 0.051(5) 0.056(5) 0.047(4) 0.002(3) 0.025(4) -0.004(3)
O3 0.067(5) 0.054(5) 0.061(4) -0.002(4) 0.039(4) 0.002(4)
O4 0.062(5) 0.055(5) 0.048(4) -0.002(4) 0.028(4) 0.003(4)
N1 0.065(16) 0.18(3) 0.27(6) 0.000 -0.10(3) 0.000
C1 0.054(7) 0.062(6) 0.052(6) 0.004(5) 0.036(6) 0.004(5)
C2 0.059(7) 0.056(6) 0.053(6) 0.006(5) 0.029(6) 0.010(5)
C3 0.058(8) 0.136(14) 0.040(6) 0.003(8) 0.028(6) -0.004(9)
C4 0.057(9) 0.109(12) 0.054(8) 0.006(8) 0.034(7) 0.016(8)
C5 0.058(7) 0.064(7) 0.045(6) 0.005(5) 0.030(5) 0.009(5)
C6 0.077(8) 0.047(6) 0.045(6) -0.004(5) 0.030(6) -0.003(6)
C7 0.060(7) 0.045(6) 0.047(6) 0.000(5) 0.026(5) 0.002(5)
C8 0.057(7) 0.050(6) 0.051(6) -0.001(5) 0.031(6) 0.000(5)
C9 0.055(6) 0.050(6) 0.045(6) 0.002(4) 0.022(5) -0.002(5)
C10 0.044(6) 0.056(6) 0.046(5) -0.007(5) 0.020(5) -0.004(5)
C11 0.078(8) 0.047(6) 0.056(6) 0.006(5) 0.035(6) 0.000(5)
C12 0.075(8) 0.056(6) 0.049(6) 0.001(5) 0.036(6) -0.001(6)

_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 2.384(9) . ?
Pb1 O4 2.474(9) . ?
Pb1 O3 2.512(9) . ?
Pb1 O2 2.530(9) 6_565 ?
Pb1 C7 2.845(12) . ?
Pb1 I1 3.1520(6) . ?
Pb1 I1 3.1750(6) 2 ?
I1 Pb1 3.1520(6) 5_565 ?
I1 Pb1 3.1750(6) 2 ?
I1 Pb1 3.1750(6) 6_565 ?
O1 C1 1.269(15) . ?
O2 C1 1.320(15) . ?
O2 Pb1 2.530(9) 6_566 ?
O3 C7 1.250(16) . ?
O4 C7 1.269(16) . ?
N1 C14 1.53(9) . ?
N1 C13 1.72(6) . ?
N1 C13 1.72(6) 2_554 ?
C1 C2 1.460(18) . ?
C2 C3 1.37(2) . ?
C2 C6 1.371(18) . ?
C3 C4 1.40(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.46(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.347(18) 2_657 ?
C5 C5 1.47(3) 2_657 ?
C6 C5 1.347(18) 2_657 ?
C6 H6 0.9500 . ?
C7 C8 1.506(16) . ?
C8 C9 1.375(17) . ?
C8 C12 1.406(17) . ?
C9 C10 1.432(17) . ?
C9 H9 0.9500 . ?
C10 C10 1.39(2) 7 ?
C10 C11 1.457(18) 7 ?
C11 C12 1.360(19) . ?
C11 C10 1.457(18) 7 ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?

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 O4 78.3(3) . . ?
O1 Pb1 O3 77.8(3) . . ?
O4 Pb1 O3 52.4(3) . . ?
O1 Pb1 O2 86.6(3) . 6_565 ?
O4 Pb1 O2 74.0(3) . 6_565 ?
O3 Pb1 O2 126.1(3) . 6_565 ?
O1 Pb1 C7 75.6(3) . . ?
O4 Pb1 C7 26.4(3) . . ?
O3 Pb1 C7 26.0(3) . . ?
O2 Pb1 C7 100.1(3) 6_565 . ?
O1 Pb1 I1 152.2(2) . . ?
O4 Pb1 I1 74.3(2) . . ?
O3 Pb1 I1 89.0(2) . . ?
O2 Pb1 I1 81.6(2) 6_565 . ?
C7 Pb1 I1 81.8(2) . . ?
O1 Pb1 I1 127.5(2) . 2 ?
O4 Pb1 I1 140.2(2) . 2 ?
O3 Pb1 I1 99.28(19) . 2 ?
O2 Pb1 I1 129.69(19) 6_565 2 ?
C7 Pb1 I1 121.7(3) . 2 ?
I1 Pb1 I1 78.354(16) . 2 ?
Pb1 I1 Pb1 180.000(14) 5_565 . ?
Pb1 I1 Pb1 80.160(17) 5_565 2 ?
Pb1 I1 Pb1 99.840(17) . 2 ?
Pb1 I1 Pb1 99.840(17) 5_565 6_565 ?
Pb1 I1 Pb1 80.160(17) . 6_565 ?
Pb1 I1 Pb1 180.0 2 6_565 ?
C1 O1 Pb1 105.5(8) . . ?
C1 O2 Pb1 135.8(8) . 6_566 ?
C7 O3 Pb1 92.0(7) . . ?
C7 O4 Pb1 93.3(7) . . ?
C14 N1 C13 94(3) . . ?
C14 N1 C13 94(3) . 2_554 ?
C13 N1 C13 171(6) . 2_554 ?
O1 C1 O2 118.7(11) . . ?
O1 C1 C2 120.5(11) . . ?
O2 C1 C2 120.7(11) . . ?
C3 C2 C6 119.8(13) . . ?
C3 C2 C1 117.2(12) . . ?
C6 C2 C1 122.9(12) . . ?
C2 C3 C4 122.1(14) . . ?
C2 C3 H3 118.9 . . ?
C4 C3 H3 118.9 . . ?
C3 C4 C5 118.8(13) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 H4 120.6 . . ?
C6 C5 C4 123.3(12) 2_657 . ?
C6 C5 C5 121.2(14) 2_657 2_657 ?
C4 C5 C5 115.5(14) . 2_657 ?
C5 C6 C2 122.2(13) 2_657 . ?
C5 C6 H6 118.9 2_657 . ?
C2 C6 H6 118.9 . . ?
O3 C7 O4 122.0(11) . . ?
O3 C7 C8 119.7(11) . . ?
O4 C7 C8 117.9(10) . . ?
O3 C7 Pb1 61.9(6) . . ?
O4 C7 Pb1 60.2(6) . . ?
C8 C7 Pb1 170.4(8) . . ?
C9 C8 C12 121.8(11) . . ?
C9 C8 C7 118.4(11) . . ?
C12 C8 C7 119.8(10) . . ?
C8 C9 C10 118.0(11) . . ?
C8 C9 H9 121.0 . . ?
C10 C9 H9 121.0 . . ?
C10 C10 C9 121.5(13) 7 . ?
C10 C10 C11 118.0(13) 7 7 ?
C9 C10 C11 120.5(11) . 7 ?
C12 C11 C10 119.9(11) . 7 ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 7 . ?
C11 C12 C8 120.7(11) . . ?
C11 C12 H12 119.6 . . ?
C8 C12 H12 119.6 . . ?
N1 C13 H13A 109.5 . . ?
N1 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N1 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N1 C14 H14A 109.5 . . ?
N1 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N1 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.946
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.946
_refine_diff_density_max         3.977
_refine_diff_density_min         -3.355
_refine_diff_density_rms         0.481
