# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 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
_database_code_depnum_ccdc_archive 'CCDC 2032526'
loop_
_audit_author_name
_audit_author_address
'Xingyu Sun'
;Qufu Normal University
China
;
_audit_update_record             
;
2020-09-17 deposited with the CCDC.	2020-11-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        '[MeBAPIm]2Pb3Br12'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H50 Br12 N8 Pb3'
_chemical_formula_weight         1983.17

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/n  '

loop_
_symmetry_equiv_pos_as_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                   16.6739(15)
_cell_length_b                   8.1277(7)
_cell_length_c                   19.1970(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 115.7280(10)
_cell_angle_gamma                90.00
_cell_volume                     2343.7(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    6614
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      26.72

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.810
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1784
_exptl_absorpt_coefficient_mu    21.003
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19755
_diffrn_reflns_av_R_equivalents  0.0620
_diffrn_reflns_av_sigmaI/netI    0.0874
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.15
_diffrn_reflns_theta_max         27.55
_reflns_number_total             4235
_reflns_number_gt                2757
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0056P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4235
_refine_ls_number_parameters     196
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0316
_refine_ls_wR_factor_ref         0.0540
_refine_ls_wR_factor_gt          0.0506
_refine_ls_goodness_of_fit_ref   0.841
_refine_ls_restrained_S_all      0.841
_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 0.5000 0.0000 0.0000 0.02820(10) Uani 1 2 d S . .
Pb2 Pb 0.371288(19) -0.10889(3) 0.135281(17) 0.03377(8) Uani 1 1 d . . .
Br1 Br 0.57484(5) -0.10796(9) 0.16957(4) 0.03759(18) Uani 1 1 d . . .
Br2 Br 0.41113(6) 0.09476(10) 0.26616(5) 0.0470(2) Uani 1 1 d . . .
Br3 Br 0.36552(5) 0.20917(9) 0.02680(4) 0.04290(19) Uani 1 1 d . . .
Br4 Br 0.62979(5) 0.28066(9) 0.02589(4) 0.0439(2) Uani 1 1 d . . .
Br5 Br 0.40404(6) -0.39361(10) 0.23105(6) 0.0574(3) Uani 1 1 d . . .
Br6 Br 0.18810(6) -0.13769(12) 0.11018(6) 0.0652(3) Uani 1 1 d . . .
N1 N 0.4030(4) -0.2567(7) 0.5588(3) 0.0390(15) Uani 1 1 d . . .
N2 N 0.4689(4) -0.4778(8) 0.8784(3) 0.0482(17) Uani 1 1 d . . .
H2C H 0.5241 -0.4438 0.9081 0.072 Uiso 1 1 calc R . .
H2D H 0.4703 -0.5817 0.8643 0.072 Uiso 1 1 calc R . .
H2E H 0.4363 -0.4711 0.9047 0.072 Uiso 1 1 calc R . .
N3 N 0.3497(4) -0.3285(9) 0.6413(3) 0.0464(17) Uani 1 1 d . . .
C1 C 0.3652(5) -0.2063(10) 0.6029(4) 0.0394(18) Uani 1 1 d . . .
C2 C 0.4036(5) -0.1959(10) 0.4340(4) 0.0431(19) Uani 1 1 d . . .
H2A H 0.4067 -0.3135 0.4270 0.052 Uiso 1 1 calc R . .
H2B H 0.4382 -0.1416 0.4112 0.052 Uiso 1 1 calc R . .
C3 C 0.4291(5) -0.3727(9) 0.8086(4) 0.0397(19) Uani 1 1 d . . .
H3A H 0.4653 -0.3785 0.7806 0.048 Uiso 1 1 calc R . .
H3B H 0.4284 -0.2593 0.8241 0.048 Uiso 1 1 calc R . .
C4 C 0.4426(5) -0.1584(9) 0.5176(5) 0.048(2) Uani 1 1 d . . .
H4A H 0.5062 -0.1793 0.5400 0.057 Uiso 1 1 calc R . .
H4B H 0.4341 -0.0426 0.5246 0.057 Uiso 1 1 calc R . .
C5 C 0.3710(6) -0.4836(11) 0.6153(5) 0.059(2) Uani 1 1 d . . .
H5A H 0.3176 -0.5391 0.5792 0.071 Uiso 1 1 calc R . .
H5B H 0.4036 -0.5561 0.6586 0.071 Uiso 1 1 calc R . .
C6 C 0.2970(6) -0.3232(12) 0.6852(5) 0.071(3) Uani 1 1 d . . .
H6A H 0.2373 -0.3623 0.6528 0.085 Uiso 1 1 calc R . .
H6B H 0.2925 -0.2101 0.6993 0.085 Uiso 1 1 calc R . .
C7 C 0.3421(6) -0.0310(10) 0.6083(5) 0.063(3) Uani 1 1 d . . .
H7A H 0.3590 0.0353 0.5755 0.094 Uiso 1 1 calc R . .
H7B H 0.3733 0.0059 0.6608 0.094 Uiso 1 1 calc R . .
H7C H 0.2791 -0.0215 0.5921 0.094 Uiso 1 1 calc R . .
C8 C 0.3366(5) -0.4258(10) 0.7571(4) 0.049(2) Uani 1 1 d . . .
H8A H 0.2999 -0.4167 0.7847 0.059 Uiso 1 1 calc R . .
H8B H 0.3371 -0.5403 0.7430 0.059 Uiso 1 1 calc R . .
N4 N 0.2718(5) -0.1649(9) 0.3084(4) 0.070(2) Uani 1 1 d . . .
H4C H 0.2155 -0.1309 0.2865 0.105 Uiso 1 1 calc R . .
H4D H 0.2741 -0.2710 0.2980 0.105 Uiso 1 1 calc R . .
H4E H 0.3035 -0.1068 0.2899 0.105 Uiso 1 1 calc R . .
C9 C 0.4281(6) -0.4300(9) 0.5764(4) 0.052(2) Uani 1 1 d . . .
H9A H 0.4909 -0.4412 0.6108 0.062 Uiso 1 1 calc R . .
H9B H 0.4145 -0.4928 0.5297 0.062 Uiso 1 1 calc R . .
C10 C 0.3090(6) -0.1414(11) 0.3932(5) 0.058(3) Uani 1 1 d . . .
H10A H 0.2734 -0.2030 0.4129 0.070 Uiso 1 1 calc R . .
H10B H 0.3052 -0.0259 0.4041 0.070 Uiso 1 1 calc R . .


_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 Br3 3.0306(7) 3_655 ?
Pb1 Br3 3.0307(7) . ?
Pb1 Br4 3.0332(7) . ?
Pb1 Br4 3.0332(7) 3_655 ?
Pb1 Br1 3.0655(8) 3_655 ?
Pb1 Br1 3.0655(8) . ?
Pb2 Br2 2.8363(8) . ?
Pb2 Br5 2.8569(9) . ?
Pb2 Br6 2.8878(9) . ?
Pb2 Br1 3.1644(8) . ?
N1 C1 1.322(8) . ?
N1 C9 1.466(9) . ?
N1 C4 1.467(8) . ?
N2 C3 1.481(9) . ?
N3 C1 1.327(9) . ?
N3 C5 1.456(10) . ?
N3 C6 1.458(9) . ?
C1 C7 1.491(11) . ?
C2 C4 1.478(10) . ?
C2 C10 1.492(11) . ?
C3 C8 1.490(10) . ?
C5 C9 1.506(11) . ?
C6 C8 1.498(10) . ?
N4 C10 1.480(10) . ?

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
Br3 Pb1 Br3 180.0 3_655 . ?
Br3 Pb1 Br4 85.52(2) 3_655 . ?
Br3 Pb1 Br4 94.48(2) . . ?
Br3 Pb1 Br4 94.48(2) 3_655 3_655 ?
Br3 Pb1 Br4 85.52(2) . 3_655 ?
Br4 Pb1 Br4 180.0 . 3_655 ?
Br3 Pb1 Br1 88.31(2) 3_655 3_655 ?
Br3 Pb1 Br1 91.69(2) . 3_655 ?
Br4 Pb1 Br1 83.76(2) . 3_655 ?
Br4 Pb1 Br1 96.24(2) 3_655 3_655 ?
Br3 Pb1 Br1 91.70(2) 3_655 . ?
Br3 Pb1 Br1 88.30(2) . . ?
Br4 Pb1 Br1 96.24(2) . . ?
Br4 Pb1 Br1 83.76(2) 3_655 . ?
Br1 Pb1 Br1 180.0 3_655 . ?
Br2 Pb2 Br5 89.82(3) . . ?
Br2 Pb2 Br6 91.10(3) . . ?
Br5 Pb2 Br6 86.25(3) . . ?
Br2 Pb2 Br1 89.81(2) . . ?
Br5 Pb2 Br1 88.85(2) . . ?
Br6 Pb2 Br1 175.01(3) . . ?
Pb1 Br1 Pb2 82.78(2) . . ?
C1 N1 C9 108.5(6) . . ?
C1 N1 C4 128.9(6) . . ?
C9 N1 C4 119.8(6) . . ?
C1 N3 C5 108.8(6) . . ?
C1 N3 C6 127.6(7) . . ?
C5 N3 C6 121.5(7) . . ?
N1 C1 N3 112.7(7) . . ?
N1 C1 C7 123.4(7) . . ?
N3 C1 C7 123.9(7) . . ?
C4 C2 C10 112.1(6) . . ?
N2 C3 C8 111.2(6) . . ?
N1 C4 C2 112.5(6) . . ?
N3 C5 C9 102.7(6) . . ?
N3 C6 C8 112.4(7) . . ?
C3 C8 C6 111.4(7) . . ?
N1 C9 C5 102.4(6) . . ?
N4 C10 C2 112.5(7) . . ?

_diffrn_measured_fraction_theta_max 0.953
_diffrn_reflns_theta_full        27.55
_diffrn_measured_fraction_theta_full 0.782
_refine_diff_density_max         1.474
_refine_diff_density_min         -1.089
_refine_diff_density_rms         0.158
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2032527'
loop_
_audit_author_name
_audit_author_address
'Xingyu Sun'
;Qufu Normal University
China
;
_audit_update_record             
;
2020-09-17 deposited with the CCDC.	2020-11-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        '[PMDPTA]2Pb3Br12'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H60 Br12 N6 Pb3'
_chemical_formula_weight         1989.25

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'

_symmetry_cell_setting           Orthorhombic'
_symmetry_space_group_name_H-M   P2(1)2(1)2(1)

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

_cell_length_a                   9.9716(12)
_cell_length_b                   15.7329(19)
_cell_length_c                   31.996(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5019.6(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5612
_cell_measurement_theta_min      2.31
_cell_measurement_theta_max      18.12

_exptl_crystal_description       rod
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.632
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3600
_exptl_absorpt_coefficient_mu    19.612
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            28366
_diffrn_reflns_av_R_equivalents  0.0719
_diffrn_reflns_av_sigmaI/netI    0.0494
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.27
_diffrn_reflns_theta_max         27.541
_reflns_number_total             4172
_reflns_number_gt                3756
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0126P)²+13.9943P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.000075(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.016(11)
_refine_ls_number_reflns         4172
_refine_ls_number_parameters     374
_refine_ls_number_restraints     87
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0284
_refine_ls_wR_factor_ref         0.0607
_refine_ls_wR_factor_gt          0.0583
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.064
_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 0.27672(6) 0.31698(4) 0.38064(2) 0.0400(2) Uani 1 1 d . . .
Pb2 Pb 0.27139(6) 0.55978(4) 0.42484(2) 0.0434(2) Uani 1 1 d . . .
Pb3 Pb 0.31890(6) 0.08129(4) 0.33436(2) 0.0419(2) Uani 1 1 d . . .
Br1 Br 0.22758(19) 0.15484(12) 0.42517(6) 0.0645(6) Uani 1 1 d . . .
Br2 Br 0.42464(19) 0.06375(13) 0.25151(5) 0.0604(6) Uani 1 1 d . . .
Br3 Br 0.52415(17) 0.23204(12) 0.34513(6) 0.0553(5) Uani 1 1 d . . .
Br4 Br 0.03615(16) 0.40968(13) 0.41725(6) 0.0582(5) Uani 1 1 d . . .
Br5 Br 0.0949(2) 0.68078(13) 0.38542(6) 0.0698(6) Uani 1 1 d . . .
Br6 Br 0.34874(18) 0.48573(12) 0.33649(6) 0.0573(6) Uani 1 1 d . . .
Br7 Br 0.4991(2) -0.03699(13) 0.36944(6) 0.0722(6) Uani 1 1 d . . .
Br8 Br 0.43085(17) 0.39642(13) 0.45807(6) 0.0546(6) Uani 1 1 d . . .
Br9 Br 0.1784(2) 0.60563(15) 0.50806(6) 0.0790(7) Uani 1 1 d . . .
Br10 Br 0.12055(19) -0.05047(14) 0.31227(7) 0.0711(6) Uani 1 1 d . . .
Br11 Br 0.1195(2) 0.24528(16) 0.31026(8) 0.0992(9) Uani 1 1 d . . .
Br12 Br 0.4994(2) 0.66817(15) 0.42953(7) 0.0880(7) Uani 1 1 d . . .
N1 N 0.1951(16) 0.5965(11) 0.2598(5) 0.080(5) Uani 1 1 d U . .
H1C H 0.2487 0.5744 0.2801 0.096 Uiso 1 1 calc R . .
N2 N 0.2384(18) 0.3295(13) 0.5402(6) 0.116(5) Uani 1 1 d DU . .
H2C H 0.2816 0.3512 0.5175 0.139 Uiso 1 1 calc R . .
C1 C 0.251(3) 0.746(2) 0.2764(10) 0.182(11) Uiso 1 1 d DU . .
H1A H 0.1815 0.7362 0.2969 0.218 Uiso 1 1 calc R . .
H1B H 0.2316 0.7991 0.2623 0.218 Uiso 1 1 calc R . .
N3 N -0.1781(15) 0.4660(12) 0.3455(5) 0.078(5) Uani 1 1 d . . .
H3C H -0.1116 0.4529 0.3639 0.094 Uiso 1 1 calc R . .
C2 C 0.376(3) 0.754(2) 0.2974(8) 0.168(8) Uani 1 1 d DU . .
H2A H 0.3760 0.7061 0.3165 0.202 Uiso 1 1 calc R . .
H2B H 0.3633 0.8037 0.3149 0.202 Uiso 1 1 calc R . .
C3 C 0.052(2) 0.6050(15) 0.2777(6) 0.088(7) Uani 1 1 d . . .
H3A H 0.0505 0.6491 0.2989 0.106 Uiso 1 1 calc R . .
H3B H -0.0090 0.6220 0.2555 0.106 Uiso 1 1 calc R . .
C4 C -0.204(2) 0.3910(15) 0.3197(8) 0.123(9) Uani 1 1 d . . .
H4A H -0.1245 0.3769 0.3042 0.185 Uiso 1 1 calc R . .
H4B H -0.2758 0.4029 0.3006 0.185 Uiso 1 1 calc R . .
H4C H -0.2284 0.3441 0.3372 0.185 Uiso 1 1 calc R . .
C5 C 0.254(2) 0.2379(14) 0.5377(7) 0.123(7) Uani 1 1 d U . .
H5A H 0.3467 0.2234 0.5412 0.184 Uiso 1 1 calc R . .
H5B H 0.2234 0.2184 0.5109 0.184 Uiso 1 1 calc R . .
H5C H 0.2019 0.2115 0.5593 0.184 Uiso 1 1 calc R . .
N4 N 0.522(3) 0.7606(15) 0.2838(6) 0.127(7) Uani 1 1 d U . .
H4D H 0.5355 0.7159 0.2662 0.153 Uiso 1 1 calc R . .
C6 C -0.130(2) 0.5377(12) 0.3182(7) 0.075(7) Uani 1 1 d . . .
H6A H -0.1209 0.5885 0.3352 0.089 Uiso 1 1 calc R . .
H6B H -0.1970 0.5489 0.2970 0.089 Uiso 1 1 calc R . .
C7 C 0.0015(19) 0.5206(13) 0.2970(6) 0.071(6) Uani 1 1 d . . .
H7A H -0.0100 0.4781 0.2754 0.085 Uiso 1 1 calc R . .
H7B H 0.0663 0.4996 0.3171 0.085 Uiso 1 1 calc R . .
C8 C 0.808(3) 0.5319(14) 0.4929(8) 0.159(11) Uani 1 1 d U . .
H8A H 0.8311 0.5243 0.4640 0.238 Uiso 1 1 calc R . .
H8B H 0.7253 0.5032 0.4988 0.238 Uiso 1 1 calc R . .
H8C H 0.8780 0.5086 0.5102 0.238 Uiso 1 1 calc R . .
N5 N 0.794(3) 0.6182(12) 0.5014(7) 0.150(7) Uani 1 1 d DU . .
H5D H 0.7083 0.6227 0.4919 0.180 Uiso 1 1 calc R . .
C9 C 0.766(3) 0.6442(16) 0.5430(7) 0.149(8) Uani 1 1 d DU . .
H9A H 0.8471 0.6409 0.5595 0.179 Uiso 1 1 calc R . .
H9B H 0.7364 0.7030 0.5428 0.179 Uiso 1 1 calc R . .
C10 C 0.667(3) 0.5939(19) 0.5615(10) 0.158(9) Uani 1 1 d DU . .
H10A H 0.6777 0.5371 0.5503 0.190 Uiso 1 1 calc R . .
H10B H 0.6883 0.5906 0.5910 0.190 Uiso 1 1 calc R . .
C11 C 0.533(3) 0.6128(18) 0.5589(10) 0.157(10) Uani 1 1 d DU . .
H11A H 0.5027 0.5975 0.5311 0.188 Uiso 1 1 calc R . .
H11B H 0.5233 0.6739 0.5616 0.188 Uiso 1 1 calc R . .
C12 C 0.848(2) 0.6770(16) 0.4746(8) 0.139(10) Uani 1 1 d U . .
H12A H 0.8658 0.6506 0.4481 0.209 Uiso 1 1 calc R . .
H12B H 0.9303 0.6986 0.4861 0.209 Uiso 1 1 calc R . .
H12C H 0.7860 0.7230 0.4708 0.209 Uiso 1 1 calc R . .
C13 C 0.103(2) 0.3486(18) 0.5347(9) 0.159(9) Uani 1 1 d DU . .
H13A H 0.0723 0.3250 0.5087 0.239 Uiso 1 1 calc R . .
H13B H 0.0912 0.4092 0.5342 0.239 Uiso 1 1 calc R . .
H13C H 0.0520 0.3248 0.5573 0.239 Uiso 1 1 calc R . .
C14 C -0.3001(19) 0.4902(18) 0.3700(8) 0.158(13) Uani 1 1 d . . .
H14A H -0.2813 0.5400 0.3863 0.236 Uiso 1 1 calc R . .
H14B H -0.3246 0.4443 0.3882 0.236 Uiso 1 1 calc R . .
H14C H -0.3727 0.5018 0.3511 0.236 Uiso 1 1 calc R . .
C15 C 0.196(2) 0.5398(18) 0.2252(7) 0.145(12) Uani 1 1 d . . .
H15A H 0.2852 0.5347 0.2145 0.218 Uiso 1 1 calc R . .
H15B H 0.1378 0.5615 0.2037 0.218 Uiso 1 1 calc R . .
H15C H 0.1641 0.4850 0.2340 0.218 Uiso 1 1 calc R . .
N6 N 0.434(2) 0.5687(13) 0.5920(6) 0.131(8) Uani 1 1 d DU . .
H6C H 0.4935 0.5575 0.6129 0.157 Uiso 1 1 calc RD . .
C16 C 0.568(4) 0.8309(18) 0.2626(8) 0.167(12) Uani 1 1 d U . .
H16A H 0.5120 0.8408 0.2386 0.251 Uiso 1 1 calc R . .
H16B H 0.6584 0.8214 0.2537 0.251 Uiso 1 1 calc R . .
H16C H 0.5645 0.8796 0.2806 0.251 Uiso 1 1 calc R . .
C17 C 0.249(3) 0.6823(16) 0.2481(8) 0.131(10) Uani 1 1 d U . .
H17A H 0.3401 0.6741 0.2383 0.158 Uiso 1 1 calc R . .
H17B H 0.1972 0.7022 0.2243 0.158 Uiso 1 1 calc R . .
C18 C 0.422(3) 0.4760(18) 0.5720(9) 0.191(15) Uani 1 1 d DU . .
H18A H 0.5093 0.4490 0.5692 0.230 Uiso 1 1 calc RD . .
H18B H 0.3783 0.4774 0.5449 0.230 Uiso 1 1 calc R . .
C19 C 0.3491(18) 0.6238(14) 0.6130(6) 0.091(7) Uani 1 1 d DU . .
H19A H 0.3831 0.6807 0.6109 0.136 Uiso 1 1 calc R . .
H19B H 0.3442 0.6077 0.6419 0.136 Uiso 1 1 calc R . .
H19C H 0.2612 0.6212 0.6009 0.136 Uiso 1 1 calc R . .
C20 C 0.606(3) 0.7437(15) 0.3201(7) 0.134(10) Uani 1 1 d U . .
H21A H 0.5738 0.6943 0.3345 0.200 Uiso 1 1 calc R . .
H21B H 0.6042 0.7917 0.3386 0.200 Uiso 1 1 calc R . .
H21C H 0.6970 0.7339 0.3111 0.200 Uiso 1 1 calc R . .
C22 C 0.326(3) 0.3560(16) 0.5802(8) 0.137(6) Uiso 1 1 d DU . .
H22A H 0.3028 0.3141 0.6011 0.165 Uiso 1 1 calc R . .
H22B H 0.4177 0.3426 0.5720 0.165 Uiso 1 1 calc R . .
C23 C 0.339(3) 0.4343(18) 0.6037(9) 0.171(11) Uiso 1 1 d DU . .
H23A H 0.3858 0.4267 0.6300 0.205 Uiso 1 1 calc R . .
H23B H 0.2542 0.4627 0.6081 0.205 Uiso 1 1 calc R . .


_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 2.9627(19) . ?
Pb1 Br11 2.967(2) . ?
Pb1 Br3 3.0272(19) . ?
Pb1 Br4 3.0420(18) . ?
Pb1 Br6 3.092(2) . ?
Pb1 Br8 3.172(2) . ?
Pb2 Br12 2.846(2) . ?
Pb2 Br5 2.883(2) . ?
Pb2 Br9 2.910(2) . ?
Pb2 Br6 3.153(2) . ?
Pb2 Br8 3.204(2) . ?
Pb3 Br7 2.820(2) . ?
Pb3 Br2 2.8662(19) . ?
Pb3 Br10 2.951(2) . ?
Pb3 Br3 3.1516(19) . ?
N1 C15 1.42(2) . ?
N1 C17 1.50(3) . ?
N1 C3 1.55(2) . ?
N2 C13 1.395(16) . ?
N2 C5 1.45(2) . ?
N2 C22 1.61(3) . ?
C1 C17 1.35(3) . ?
C1 C2 1.416(19) . ?
N3 C4 1.46(2) . ?
N3 C6 1.51(2) . ?
N3 C14 1.50(2) . ?
C2 N4 1.52(3) . ?
C3 C7 1.55(3) . ?
N4 C16 1.38(3) . ?
N4 C20 1.46(3) . ?
C6 C7 1.50(2) . ?
C8 N5 1.39(3) . ?
N5 C12 1.37(3) . ?
N5 C9 1.420(17) . ?
C9 C10 1.40(3) . ?
C10 C11 1.369(18) . ?
C11 N6 1.61(3) . ?
N6 C18 1.60(2) . ?
N6 C19 1.385(16) . ?
C18 C23 1.464(19) . ?
C22 C23 1.449(18) . ?

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 Br11 87.14(7) . . ?
Br1 Pb1 Br3 86.28(5) . . ?
Br11 Pb1 Br3 88.73(6) . . ?
Br1 Pb1 Br4 95.58(6) . . ?
Br11 Pb1 Br4 93.32(6) . . ?
Br3 Pb1 Br4 177.29(6) . . ?
Br1 Pb1 Br6 175.93(6) . . ?
Br11 Pb1 Br6 95.88(7) . . ?
Br3 Pb1 Br6 91.05(5) . . ?
Br4 Pb1 Br6 86.98(5) . . ?
Br1 Pb1 Br8 92.51(5) . . ?
Br11 Pb1 Br8 177.08(7) . . ?
Br3 Pb1 Br8 94.14(5) . . ?
Br4 Pb1 Br8 83.83(5) . . ?
Br6 Pb1 Br8 84.61(5) . . ?
Br12 Pb2 Br5 96.62(7) . . ?
Br12 Pb2 Br9 93.32(7) . . ?
Br5 Pb2 Br9 92.41(6) . . ?
Br12 Pb2 Br6 94.20(6) . . ?
Br5 Pb2 Br6 90.06(5) . . ?
Br9 Pb2 Br6 171.76(6) . . ?
Br12 Pb2 Br8 93.82(6) . . ?
Br5 Pb2 Br8 167.91(6) . . ?
Br9 Pb2 Br8 93.05(6) . . ?
Br6 Pb2 Br8 83.09(5) . . ?
Br7 Pb3 Br2 94.03(6) . . ?
Br7 Pb3 Br10 93.37(6) . . ?
Br2 Pb3 Br10 87.56(6) . . ?
Br7 Pb3 Br3 92.25(6) . . ?
Br2 Pb3 Br3 86.26(5) . . ?
Br10 Pb3 Br3 171.92(6) . . ?
Pb1 Br3 Pb3 81.03(5) . . ?
Pb1 Br6 Pb2 81.42(5) . . ?
Pb1 Br8 Pb2 79.42(4) . . ?
C15 N1 C17 111.6(19) . . ?
C15 N1 C3 110.2(17) . . ?
C17 N1 C3 110.3(18) . . ?
C13 N2 C5 108(2) . . ?
C13 N2 C22 125(2) . . ?
C5 N2 C22 104.0(18) . . ?
C17 C1 C2 114(3) . . ?
C4 N3 C6 109.4(17) . . ?
C4 N3 C14 111.0(17) . . ?
C6 N3 C14 111.9(18) . . ?
C1 C2 N4 135(3) . . ?
C7 C3 N1 111.9(17) . . ?
C16 N4 C20 110(3) . . ?
C16 N4 C2 121(3) . . ?
C20 N4 C2 108(2) . . ?
N3 C6 C7 114.1(16) . . ?
C6 C7 C3 108.1(18) . . ?
C12 N5 C8 120(2) . . ?
C12 N5 C9 118(2) . . ?
C8 N5 C9 119(2) . . ?
C10 C9 N5 112(3) . . ?
C11 C10 C9 123(3) . . ?
C10 C11 N6 118(3) . . ?
C18 N6 C19 136(2) . . ?
C18 N6 C11 99.9(17) . . ?
C19 N6 C11 115(2) . . ?
C1 C17 N1 120(3) . . ?
N6 C18 C23 100(2) . . ?
C23 C22 N2 133(3) . . ?
C22 C23 C18 94(2) . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.541
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.883
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.110
