# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_U2023_03b_II_0m
_database_code_depnum_ccdc_archive 'CCDC 2269539'
loop_
_audit_author_name
_audit_author_address
'Gerasimenko Andrey V.'
;Institute of Chemistry, Far Eastern Branch of the Russian Academy of Sciences
Russia
;
_audit_update_record             
;
2023-06-13 deposited with the CCDC.	2023-11-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C5 H16  N2, Br4 Pb'
_chemical_formula_sum            'C5 H16 Br4 N2 Pb'
_chemical_formula_weight         631.03

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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. 
;

loop_
_space_group_symop_operation_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                   21.4488(11)
_cell_length_b                   8.1241(4)
_cell_length_c                   8.2662(4)
_cell_angle_alpha                90
_cell_angle_beta                 100.820(3)
_cell_angle_gamma                90
_cell_volume                     1414.80(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7744
_cell_measurement_theta_min      3.55
_cell_measurement_theta_max      26.01

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.963
_exptl_crystal_F_000             1128
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    23.185
_shelx_estimated_absorpt_T_min   0.072
_shelx_estimated_absorpt_T_max   0.129
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4114
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            23026
_diffrn_reflns_av_unetI/netI     0.0176
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         1.933
_diffrn_reflns_theta_max         26.086
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1409
_reflns_number_gt                1243
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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. 
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0203P)²+14.2427P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1409
_refine_ls_number_parameters     108
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0231
_refine_ls_wR_factor_ref         0.0560
_refine_ls_wR_factor_gt          0.0540
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_restrained_S_all      1.142
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.2500 0.2500 0.0000 0.02685(10) Uani 1 2 d S . P . .
Br1A Br 0.24982(10) 0.4412(4) 0.3082(3) 0.0373(5) Uani 0.5 1 d . . P A 2
Br2A Br 0.39295(10) 0.2774(3) 0.0535(2) 0.0374(4) Uani 0.5 1 d . . P A 2
Br1B Br 0.22411(9) 0.4422(4) 0.2914(3) 0.0359(5) Uani 0.5 1 d . . P A 3
Br2B Br 0.38572(9) 0.3237(3) 0.1032(2) 0.0353(4) Uani 0.5 1 d . . P A 3
N1 N 0.3728(7) 0.2798(17) 0.4971(17) 0.048(4) Uani 0.5 1 d . . P B -1
H1A H 0.3390 0.2239 0.5218 0.073 Uiso 0.5 1 calc R U P B -1
H1B H 0.3647 0.3077 0.3885 0.073 Uiso 0.5 1 calc R U P B -1
H1C H 0.3795 0.3727 0.5595 0.073 Uiso 0.5 1 calc R U P B -1
C1 C 0.4307(10) 0.173(3) 0.532(2) 0.051(6) Uani 0.5 1 d . . P B -1
H1D H 0.4607 0.2143 0.4643 0.062 Uiso 0.5 1 calc R U P B -1
H1E H 0.4178 0.0611 0.4925 0.062 Uiso 0.5 1 calc R U P B -1
C4 C 0.5362(9) 0.267(3) 0.9536(18) 0.070(6) Uani 0.5 1 d . . P B -1
H4A H 0.5406 0.3677 1.0218 0.084 Uiso 0.5 1 calc R U P B -1
H4B H 0.5143 0.1847 1.0116 0.084 Uiso 0.5 1 calc R U P B -1
C2 C 0.4673(8) 0.157(2) 0.7097(15) 0.066(6) Uani 0.5 1 d . . P B -1
H2D H 0.4395 0.1021 0.7760 0.079 Uiso 0.5 1 calc R U P B -1
H2E H 0.5043 0.0842 0.7091 0.079 Uiso 0.5 1 calc R U P B -1
C3 C 0.4901(11) 0.309(2) 0.791(2) 0.068(5) Uani 0.5 1 d . . P B -1
H3A H 0.4539 0.3744 0.8154 0.081 Uiso 0.5 1 calc R U P B -1
H3B H 0.5123 0.3756 0.7190 0.081 Uiso 0.5 1 calc R U P B -1
N2 N 0.6349(5) 0.3205(15) 0.8644(12) 0.037(2) Uani 0.5 1 d . . P B -1
H2A H 0.6212 0.3042 0.7546 0.056 Uiso 0.5 1 calc R U P B -1
H2B H 0.6776 0.3039 0.8900 0.056 Uiso 0.5 1 calc R U P B -1
H2C H 0.6259 0.4254 0.8910 0.056 Uiso 0.5 1 calc R U P B -1
C5 C 0.6023(14) 0.202(3) 0.959(3) 0.070(8) Uani 0.5 1 d . . P B -1
H5A H 0.6253 0.1947 1.0742 0.084 Uiso 0.5 1 calc R U P B -1
H5B H 0.6007 0.0916 0.9085 0.084 Uiso 0.5 1 calc R U P B -1


_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 Br2B 2.937(2) . ?
Pb1 Br2B 2.937(2) 7 ?
Pb1 Br1A 2.967(3) 6_565 ?
Pb1 Br1A 2.967(3) 4_545 ?
Pb1 Br1A 2.984(3) . ?
Pb1 Br1A 2.984(3) 7 ?
Pb1 Br1B 3.009(3) . ?
Pb1 Br1B 3.009(3) 7 ?
Pb1 Br2A 3.023(2) 7 ?
Pb1 Br2A 3.023(2) . ?
Pb1 Br1B 3.029(3) 4_545 ?
Pb1 Br1B 3.029(3) 6_565 ?
Br1A Pb1 2.967(3) 4 ?
Br1B Pb1 3.029(3) 4 ?
N1 C1 1.50(3) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 H1C 0.9100 . ?
C1 C2 1.53(2) . ?
C1 H1D 0.9900 . ?
C1 H1E 0.9900 . ?
C4 C5 1.50(3) . ?
C4 C3 1.55(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C2 C3 1.45(3) . ?
C2 H2D 0.9900 . ?
C2 H2E 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
N2 C5 1.49(3) . ?
N2 H2A 0.9100 . ?
N2 H2B 0.9100 . ?
N2 H2C 0.9100 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?

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
Br2B Pb1 Br2B 180.0 . 7 ?
Br1A Pb1 Br1A 180.00(6) 6_565 4_545 ?
Br1A Pb1 Br1A 90.92(2) 6_565 . ?
Br1A Pb1 Br1A 89.08(2) 4_545 . ?
Br1A Pb1 Br1A 89.08(2) 6_565 7 ?
Br1A Pb1 Br1A 90.92(2) 4_545 7 ?
Br1A Pb1 Br1A 180.0 . 7 ?
Br2B Pb1 Br1B 89.05(5) . . ?
Br2B Pb1 Br1B 90.96(5) 7 . ?
Br2B Pb1 Br1B 90.95(5) . 7 ?
Br2B Pb1 Br1B 89.05(5) 7 7 ?
Br1B Pb1 Br1B 180.0 . 7 ?
Br1A Pb1 Br2A 94.85(6) 6_565 7 ?
Br1A Pb1 Br2A 85.15(6) 4_545 7 ?
Br1A Pb1 Br2A 89.96(5) . 7 ?
Br1A Pb1 Br2A 90.04(5) 7 7 ?
Br1A Pb1 Br2A 85.15(6) 6_565 . ?
Br1A Pb1 Br2A 94.85(6) 4_545 . ?
Br1A Pb1 Br2A 90.04(5) . . ?
Br1A Pb1 Br2A 89.96(5) 7 . ?
Br2A Pb1 Br2A 180.000(13) 7 . ?
Br2B Pb1 Br1B 86.40(6) . 4_545 ?
Br2B Pb1 Br1B 93.60(6) 7 4_545 ?
Br1B Pb1 Br1B 90.82(3) . 4_545 ?
Br1B Pb1 Br1B 89.18(3) 7 4_545 ?
Br2B Pb1 Br1B 93.60(6) . 6_565 ?
Br2B Pb1 Br1B 86.40(6) 7 6_565 ?
Br1B Pb1 Br1B 89.18(3) . 6_565 ?
Br1B Pb1 Br1B 90.82(3) 7 6_565 ?
Br1B Pb1 Br1B 180.00(9) 4_545 6_565 ?
Pb1 Br1A Pb1 153.65(11) 4 . ?
Pb1 Br1B Pb1 147.42(10) . 4 ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
H1A N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
N1 C1 C2 119.5(17) . . ?
N1 C1 H1D 107.4 . . ?
C2 C1 H1D 107.4 . . ?
N1 C1 H1E 107.4 . . ?
C2 C1 H1E 107.4 . . ?
H1D C1 H1E 107.0 . . ?
C5 C4 C3 123.2(15) . . ?
C5 C4 H4A 106.5 . . ?
C3 C4 H4A 106.5 . . ?
C5 C4 H4B 106.5 . . ?
C3 C4 H4B 106.5 . . ?
H4A C4 H4B 106.5 . . ?
C3 C2 C1 116.1(17) . . ?
C3 C2 H2D 108.3 . . ?
C1 C2 H2D 108.3 . . ?
C3 C2 H2E 108.3 . . ?
C1 C2 H2E 108.3 . . ?
H2D C2 H2E 107.4 . . ?
C2 C3 C4 108.5(16) . . ?
C2 C3 H3A 110.0 . . ?
C4 C3 H3A 110.0 . . ?
C2 C3 H3B 110.0 . . ?
C4 C3 H3B 110.0 . . ?
H3A C3 H3B 108.4 . . ?
C5 N2 H2A 109.5 . . ?
C5 N2 H2B 109.5 . . ?
H2A N2 H2B 109.5 . . ?
C5 N2 H2C 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
N2 C5 C4 107.1(18) . . ?
N2 C5 H5A 110.3 . . ?
C4 C5 H5A 110.3 . . ?
N2 C5 H5B 110.3 . . ?
C4 C5 H5B 110.3 . . ?
H5A C5 H5B 108.6 . . ?

_refine_diff_density_max         1.894
_refine_diff_density_min         -1.047
_refine_diff_density_rms         0.135



####################################################################### 
# 
# 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_U2023_05b_2_0m
_database_code_depnum_ccdc_archive 'CCDC 2269541'
loop_
_audit_author_name
_audit_author_address
'Gerasimenko Andrey V.'
;Institute of Chemistry, Far Eastern Branch of the Russian Academy of Sciences
Russia
;
_audit_update_record             
;
2023-06-13 deposited with the CCDC.	2023-11-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C5 H16  N2, Cl4 Pb'
_chemical_formula_sum            'C5 H16 Cl4 N2 Pb'
_chemical_formula_weight         453.19

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_H-M_alt        'C 2 2 21'
_space_group_name_Hall           'C 2c 2'

_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. 
;

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

_cell_length_a                   7.4322(6)
_cell_length_b                   8.0456(6)
_cell_length_c                   22.5432(18)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1348.00(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4868
_cell_measurement_theta_min      3.62
_cell_measurement_theta_max      28.50

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.233
_exptl_crystal_F_000             840
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.037
_exptl_absorpt_coefficient_mu    13.270
_shelx_estimated_absorpt_T_min   0.225
_shelx_estimated_absorpt_T_max   0.639
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.2396
_exptl_absorpt_correction_T_max  0.6753
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6297
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_av_R_equivalents  0.0211
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.807
_diffrn_reflns_theta_max         28.514
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1718
_reflns_number_gt                1700
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.727
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    1.000

_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. 
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
; 
 Refined as a 2-component inversion twin. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0316P)²] 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_abs_structure_details 
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.466(13)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1718
_refine_ls_number_parameters     108
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0179
_refine_ls_R_factor_gt           0.0176
_refine_ls_wR_factor_ref         0.0439
_refine_ls_wR_factor_gt          0.0437
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.068
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.34181(2) 0.7500 0.01014(8) Uani 1 2 d S T P . .
Cl1A Cl 0.0288(4) 0.2821(3) 0.87446(11) 0.0173(7) Uani 0.5 1 d . . P A 2
Cl1B Cl 0.0355(4) 0.4111(3) 0.87387(12) 0.0181(8) Uani 0.5 1 d . . P A 3
Cl3 Cl 0.3222(4) 0.1553(3) 0.73664(11) 0.0167(5) Uani 0.5 1 d . . P A 2
Cl4 Cl -0.1777(3) 0.0302(3) 0.72796(12) 0.0188(5) Uani 0.5 1 d . . P A 2
N1 N 0.968(2) 0.1199(13) 0.1412(5) 0.019(4) Uani 0.5 1 d . . P B -1
H1A H 0.8464 0.1101 0.1376 0.029 Uiso 0.5 1 calc R U P B -1
H1B H 0.9954 0.1590 0.1780 0.029 Uiso 0.5 1 calc R U P B -1
H1C H 1.0200 0.0185 0.1359 0.029 Uiso 0.5 1 calc R U P B -1
N2 N 0.9640(18) -0.2027(15) -0.1354(4) 0.021(4) Uani 0.5 1 d . . P B -1
H2A H 0.8427 -0.1875 -0.1361 0.032 Uiso 0.5 1 calc R U P B -1
H2B H 0.9900 -0.3096 -0.1455 0.032 Uiso 0.5 1 calc R U P B -1
H2C H 1.0168 -0.1324 -0.1618 0.032 Uiso 0.5 1 calc R U P B -1
C1 C 1.0374(14) 0.2388(15) 0.0950(6) 0.016(3) Uani 0.5 1 d . . P B -1
H1D H 1.1704 0.2339 0.0943 0.020 Uiso 0.5 1 calc R U P B -1
H1E H 1.0019 0.3534 0.1059 0.020 Uiso 0.5 1 calc R U P B -1
C2 C 0.9652(14) 0.1990(14) 0.0332(5) 0.018(2) Uani 0.5 1 d . . P B -1
H2D H 0.8322 0.1950 0.0348 0.022 Uiso 0.5 1 calc R U P B -1
H2E H 0.9996 0.2897 0.0058 0.022 Uiso 0.5 1 calc R U P B -1
C3 C 1.0350(13) 0.0347(14) 0.0087(5) 0.019(2) Uani 0.5 1 d . . P B -1
H3A H 1.1681 0.0378 0.0076 0.023 Uiso 0.5 1 calc R U P B -1
H3B H 0.9987 -0.0564 0.0357 0.023 Uiso 0.5 1 calc R U P B -1
C4 C 0.9647(13) -0.0017(12) -0.0530(4) 0.017(2) Uani 0.5 1 d . . P B -1
H4A H 0.8315 -0.0028 -0.0524 0.020 Uiso 0.5 1 calc R U P B -1
H4B H 1.0039 0.0872 -0.0805 0.020 Uiso 0.5 1 calc R U P B -1
C5 C 1.0332(16) -0.1678(16) -0.0750(6) 0.020(3) Uani 0.5 1 d . . P B -1
H5A H 1.1664 -0.1668 -0.0757 0.024 Uiso 0.5 1 calc R U P B -1
H5B H 0.9939 -0.2568 -0.0476 0.024 Uiso 0.5 1 calc R U P B -1


_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 Cl3 2.842(3) 3_556 ?
Pb1 Cl3 2.842(2) . ?
Pb1 Cl1A 2.855(2) 3_556 ?
Pb1 Cl1A 2.855(2) . ?
Pb1 Cl1B 2.860(3) . ?
Pb1 Cl1B 2.860(3) 3_556 ?
Pb1 Cl3 2.863(2) 7_556 ?
Pb1 Cl3 2.863(2) 5_455 ?
Pb1 Cl4 2.877(3) . ?
Pb1 Cl4 2.877(3) 3_556 ?
Pb1 Cl4 2.878(2) 5 ?
Pb1 Cl4 2.878(2) 7_456 ?
Cl3 Cl4 1.674(4) 3_556 ?
Cl3 Pb1 2.863(2) 5_545 ?
Cl4 Cl3 1.674(4) 3_556 ?
Cl4 Pb1 2.878(2) 5_445 ?
N1 C1 1.506(14) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 H1C 0.9100 . ?
N2 C5 1.483(15) . ?
N2 H2A 0.9100 . ?
N2 H2B 0.9100 . ?
N2 H2C 0.9100 . ?
C1 C2 1.526(16) . ?
C1 H1D 0.9900 . ?
C1 H1E 0.9900 . ?
C2 C3 1.524(14) . ?
C2 H2D 0.9900 . ?
C2 H2E 0.9900 . ?
C3 C4 1.514(13) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.514(15) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?

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
Cl3 Pb1 Cl3 116.24(10) 3_556 . ?
Cl3 Pb1 Cl1A 87.26(8) 3_556 3_556 ?
Cl3 Pb1 Cl1A 82.54(8) . 3_556 ?
Cl3 Pb1 Cl1A 82.54(8) 3_556 . ?
Cl3 Pb1 Cl1A 87.26(8) . . ?
Cl1A Pb1 Cl1A 160.64(10) 3_556 . ?
Cl1B Pb1 Cl1B 157.51(11) . 3_556 ?
Cl3 Pb1 Cl3 147.45(10) 3_556 7_556 ?
Cl3 Pb1 Cl3 95.01(3) . 7_556 ?
Cl1A Pb1 Cl3 106.63(7) 3_556 7_556 ?
Cl1A Pb1 Cl3 90.58(7) . 7_556 ?
Cl3 Pb1 Cl3 95.02(3) 3_556 5_455 ?
Cl3 Pb1 Cl3 147.45(10) . 5_455 ?
Cl1A Pb1 Cl3 90.58(7) 3_556 5_455 ?
Cl1A Pb1 Cl3 106.63(7) . 5_455 ?
Cl3 Pb1 Cl3 56.51(11) 7_556 5_455 ?
Cl3 Pb1 Cl4 34.03(7) 3_556 . ?
Cl3 Pb1 Cl4 84.73(7) . . ?
Cl1A Pb1 Cl4 69.47(8) 3_556 . ?
Cl1A Pb1 Cl4 93.30(8) . . ?
Cl3 Pb1 Cl4 176.09(7) 7_556 . ?
Cl3 Pb1 Cl4 122.52(8) 5_455 . ?
Cl3 Pb1 Cl4 84.73(7) 3_556 3_556 ?
Cl3 Pb1 Cl4 34.04(7) . 3_556 ?
Cl1A Pb1 Cl4 93.30(7) 3_556 3_556 ?
Cl1A Pb1 Cl4 69.47(8) . 3_556 ?
Cl3 Pb1 Cl4 122.52(8) 7_556 3_556 ?
Cl3 Pb1 Cl4 176.09(7) 5_455 3_556 ?
Cl4 Pb1 Cl4 58.74(11) . 3_556 ?
Cl3 Pb1 Cl4 176.13(7) 3_556 5 ?
Cl3 Pb1 Cl4 63.80(8) . 5 ?
Cl1A Pb1 Cl4 88.93(8) 3_556 5 ?
Cl1A Pb1 Cl4 101.29(8) . 5 ?
Cl3 Pb1 Cl4 33.91(8) 7_556 5 ?
Cl3 Pb1 Cl4 84.39(8) 5_455 5 ?
Cl4 Pb1 Cl4 144.22(10) . 5 ?
Cl4 Pb1 Cl4 96.12(3) 3_556 5 ?
Cl3 Pb1 Cl4 63.80(8) 3_556 7_456 ?
Cl3 Pb1 Cl4 176.13(7) . 7_456 ?
Cl1A Pb1 Cl4 101.29(8) 3_556 7_456 ?
Cl1A Pb1 Cl4 88.93(8) . 7_456 ?
Cl3 Pb1 Cl4 84.39(7) 7_556 7_456 ?
Cl3 Pb1 Cl4 33.91(8) 5_455 7_456 ?
Cl4 Pb1 Cl4 96.12(3) . 7_456 ?
Cl4 Pb1 Cl4 144.22(10) 3_556 7_456 ?
Cl4 Pb1 Cl4 116.44(11) 5 7_456 ?
Cl4 Cl3 Pb1 74.13(13) 3_556 . ?
Cl4 Cl3 Pb1 73.53(13) 3_556 5_545 ?
Pb1 Cl3 Pb1 147.45(10) . 5_545 ?
Cl3 Cl4 Pb1 71.84(13) 3_556 . ?
Cl3 Cl4 Pb1 72.56(12) 3_556 5_445 ?
Pb1 Cl4 Pb1 144.22(10) . 5_445 ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
H1A N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C5 N2 H2A 109.5 . . ?
C5 N2 H2B 109.5 . . ?
H2A N2 H2B 109.5 . . ?
C5 N2 H2C 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
N1 C1 C2 112.2(10) . . ?
N1 C1 H1D 109.2 . . ?
C2 C1 H1D 109.2 . . ?
N1 C1 H1E 109.2 . . ?
C2 C1 H1E 109.2 . . ?
H1D C1 H1E 107.9 . . ?
C3 C2 C1 113.2(10) . . ?
C3 C2 H2D 108.9 . . ?
C1 C2 H2D 108.9 . . ?
C3 C2 H2E 108.9 . . ?
C1 C2 H2E 108.9 . . ?
H2D C2 H2E 107.8 . . ?
C4 C3 C2 112.6(9) . . ?
C4 C3 H3A 109.1 . . ?
C2 C3 H3A 109.1 . . ?
C4 C3 H3B 109.1 . . ?
C2 C3 H3B 109.1 . . ?
H3A C3 H3B 107.8 . . ?
C5 C4 C3 110.8(8) . . ?
C5 C4 H4A 109.5 . . ?
C3 C4 H4A 109.5 . . ?
C5 C4 H4B 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 108.1 . . ?
N2 C5 C4 110.6(10) . . ?
N2 C5 H5A 109.5 . . ?
C4 C5 H5A 109.5 . . ?
N2 C5 H5B 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 108.1 . . ?

_refine_diff_density_max         4.515
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.158



