# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2016

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

data_02_a
_database_code_depnum_ccdc_archive 'CCDC 1486414'
_audit_update_record             
;
2016-06-18 deposited with the CCDC.
2016-09-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 H7 Br3 N Pb'
_chemical_formula_weight         540.05

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)/c

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

_cell_length_a                   4.3566(7)
_cell_length_b                   21.531(3)
_cell_length_c                   11.0429(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.093(2)
_cell_angle_gamma                90.00
_cell_volume                     1035.7(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5984
_cell_measurement_theta_min      2.64
_cell_measurement_theta_max      27.53

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.463
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             948
_exptl_absorpt_coefficient_mu    27.805
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0255
_exptl_absorpt_correction_T_max  0.1250
_exptl_absorpt_process_details   'Bruker SADABS'

_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_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11594
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_sigmaI/netI    0.0318
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.89
_diffrn_reflns_theta_max         27.56
_reflns_number_total             2383
_reflns_number_gt                2090
_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, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0382P)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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2383
_refine_ls_number_parameters     101
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0273
_refine_ls_wR_factor_ref         0.0695
_refine_ls_wR_factor_gt          0.0669
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_restrained_S_all      1.099
_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 0.67980(4) 0.399085(9) 0.520678(18) 0.03185(9) Uani 1 1 d . . .
N1 N 0.8477(9) 0.3531(2) 0.9849(4) 0.0284(10) Uani 1 1 d . . .
C1 C 0.9757(16) 0.2900(3) 0.9740(6) 0.0449(15) Uani 1 1 d . . .
H1 H 0.8262 0.2633 0.9359 0.067 Uiso 1 1 calc R . .
H00C H 1.0272 0.2742 1.0532 0.067 Uiso 1 1 calc R . .
H00D H 1.1569 0.2913 0.9260 0.067 Uiso 1 1 calc R . .
Br1 Br 0.21649(13) 0.35404(3) 0.35269(5) 0.03735(15) Uani 1 1 d . . .
Br2 Br 0.49648(15) 0.30619(3) 0.68950(6) 0.04431(17) Uani 1 1 d . . .
C2 C 0.6718(13) 0.3677(3) 1.0799(5) 0.0344(12) Uani 1 1 d . . .
H2 H 0.6424 0.3385 1.1407 0.041 Uiso 1 1 calc R . .
C5 C 0.7613(11) 0.4528(2) 0.9012(4) 0.0268(10) Uani 1 1 d . . .
H5 H 0.7962 0.4812 0.8394 0.032 Uiso 1 1 calc R . .
C4 C 0.5761(11) 0.4692(2) 0.9971(4) 0.0235(10) Uani 1 1 d . . .
Br3 Br 0.24634(12) 0.48040(2) 0.64798(5) 0.03275(14) Uani 1 1 d . . .
C3 C 0.5365(13) 0.4245(3) 1.0882(5) 0.0331(12) Uani 1 1 d . . .
H3 H 0.4170 0.4338 1.1547 0.040 Uiso 1 1 calc R . .
C6 C 0.8927(13) 0.3952(2) 0.8969(5) 0.0309(12) Uani 1 1 d . . .
H6 H 1.0156 0.3849 0.8320 0.037 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 Br2 2.8585(7) . ?
Pb1 Br1 2.8832(7) . ?
Pb1 Br3 2.9511(6) . ?
Pb1 Br1 3.1645(7) 1_655 ?
Pb1 Br3 3.2140(7) 3_666 ?
N1 C6 1.345(7) . ?
N1 C2 1.348(7) . ?
N1 C1 1.476(7) . ?
C1 H1 0.9600 . ?
C1 H00C 0.9600 . ?
C1 H00D 0.9600 . ?
Br1 Pb1 3.1645(7) 1_455 ?
C2 C3 1.362(8) . ?
C2 H2 0.9300 . ?
C5 C6 1.368(7) . ?
C5 C4 1.389(7) . ?
C5 H5 0.9300 . ?
C4 C3 1.406(7) . ?
C4 C4 1.484(10) 3_667 ?
Br3 Pb1 3.2139(7) 3_666 ?
C3 H3 0.9300 . ?
C6 H6 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br2 Pb1 Br1 89.05(2) . . ?
Br2 Pb1 Br3 85.13(2) . . ?
Br1 Pb1 Br3 93.416(19) . . ?
Br2 Pb1 Br1 112.74(2) . 1_655 ?
Br1 Pb1 Br1 92.050(19) . 1_655 ?
Br3 Pb1 Br1 161.395(17) . 1_655 ?
Br2 Pb1 Br3 167.224(18) . 3_666 ?
Br1 Pb1 Br3 88.588(18) . 3_666 ?
Br3 Pb1 Br3 82.479(18) . 3_666 ?
Br1 Pb1 Br3 79.891(17) 1_655 3_666 ?
C6 N1 C2 119.9(4) . . ?
C6 N1 C1 120.1(5) . . ?
C2 N1 C1 119.9(5) . . ?
N1 C1 H1 109.5 . . ?
N1 C1 H00C 109.5 . . ?
H1 C1 H00C 109.5 . . ?
N1 C1 H00D 109.5 . . ?
H1 C1 H00D 109.5 . . ?
H00C C1 H00D 109.5 . . ?
Pb1 Br1 Pb1 92.049(19) . 1_455 ?
N1 C2 C3 121.0(5) . . ?
N1 C2 H2 119.5 . . ?
C3 C2 H2 119.5 . . ?
C6 C5 C4 120.4(5) . . ?
C6 C5 H5 119.8 . . ?
C4 C5 H5 119.8 . . ?
C5 C4 C3 116.9(5) . . ?
C5 C4 C4 121.8(5) . 3_667 ?
C3 C4 C4 121.3(5) . 3_667 ?
Pb1 Br3 Pb1 97.521(18) . 3_666 ?
C2 C3 C4 120.5(5) . . ?
C2 C3 H3 119.7 . . ?
C4 C3 H3 119.7 . . ?
N1 C6 C5 121.3(5) . . ?
N1 C6 H6 119.4 . . ?
C5 C6 H6 119.4 . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         1.403
_refine_diff_density_min         -2.031
_refine_diff_density_rms         0.224
####################################################################### 
# 
# 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_01_a
_database_code_depnum_ccdc_archive 'CCDC 1486415'
_audit_update_record             
;
2016-06-18 deposited with the CCDC.
2016-09-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H14 Br6 N2 Pb2'
_chemical_formula_weight         1080.09

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           Triclinic'
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.0898(6)
_cell_length_b                   12.4533(9)
_cell_length_c                   22.9102(16)
_cell_angle_alpha                82.1090(10)
_cell_angle_beta                 89.5550(10)
_cell_angle_gamma                76.3130(10)
_cell_volume                     2220.6(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    8668
_cell_measurement_theta_min      2.59
_cell_measurement_theta_max      27.58

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.231
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1896
_exptl_absorpt_coefficient_mu    25.937
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0274
_exptl_absorpt_correction_T_max  0.2962
_exptl_absorpt_process_details   'Bruker SADABS'

_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_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            25698
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_av_sigmaI/netI    0.0577
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.70
_diffrn_reflns_theta_max         27.10
_reflns_number_total             9710
_reflns_number_gt                7062
_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, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0274P)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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9710
_refine_ls_number_parameters     401
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0331
_refine_ls_wR_factor_ref         0.0749
_refine_ls_wR_factor_gt          0.0667
_refine_ls_goodness_of_fit_ref   0.955
_refine_ls_restrained_S_all      0.955
_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 1.04501(3) 0.31438(2) 0.516766(12) 0.03482(7) Uani 1 1 d . . .
C1 C 0.7901(12) 0.4158(7) 0.0475(4) 0.073(3) Uani 1 1 d . . .
H01D H 0.7283 0.3895 0.0190 0.110 Uiso 1 1 calc R . .
H01E H 0.9099 0.3931 0.0408 0.110 Uiso 1 1 calc R . .
H01F H 0.7557 0.4957 0.0435 0.110 Uiso 1 1 calc R . .
Br1 Br 1.11455(11) 0.14610(6) 0.44615(4) 0.0536(2) Uani 1 1 d . . .
Pb3 Pb -0.01652(3) 1.11889(2) 0.913003(12) 0.03733(8) Uani 1 1 d . . .
C3 C 0.7546(10) 0.2097(6) 0.1765(4) 0.054(2) Uani 1 1 d . . .
H3 H 0.7759 0.1324 0.1849 0.065 Uiso 1 1 calc R . .
Br3 Br 0.71784(9) 0.40034(6) 0.44427(3) 0.0496(2) Uani 1 1 d . . .
Pb2 Pb 0.56548(3) 0.38116(2) 0.583394(12) 0.03496(7) Uani 1 1 d . . .
C2 C 0.7829(11) 0.2575(6) 0.1215(4) 0.056(2) Uani 1 1 d . . .
H2 H 0.8235 0.2122 0.0930 0.068 Uiso 1 1 calc R . .
Br2 Br 1.35707(8) 0.20525(6) 0.59473(4) 0.04601(19) Uani 1 1 d . . .
Pb4 Pb 0.40785(3) 1.18893(2) 0.985843(13) 0.03954(8) Uani 1 1 d . . .
C4 C 0.6948(8) 0.2739(5) 0.2202(3) 0.0329(15) Uani 1 1 d . . .
Br4 Br 0.86308(9) 0.18749(6) 0.60302(4) 0.0482(2) Uani 1 1 d . . .
Br5 Br 0.80422(9) 0.53468(6) 0.57859(4) 0.0494(2) Uani 1 1 d . . .
C5 C 0.6598(9) 0.3895(6) 0.2030(4) 0.0471(19) Uani 1 1 d . . .
H5 H 0.6151 0.4370 0.2302 0.056 Uiso 1 1 calc R . .
Br9 Br 0.35073(10) 0.97637(7) 0.92232(4) 0.0579(2) Uani 1 1 d . . .
C9 C 0.7552(9) 0.0796(6) 0.3624(4) 0.048(2) Uani 1 1 d . . .
H9 H 0.8233 0.0106 0.3779 0.057 Uiso 1 1 calc R . .
Br8 Br -0.35108(10) 1.28546(7) 0.90629(4) 0.0633(2) Uani 1 1 d . . .
C8 C 0.7711(8) 0.1201(6) 0.3051(3) 0.0410(17) Uani 1 1 d . . .
H8 H 0.8476 0.0783 0.2815 0.049 Uiso 1 1 calc R . .
Br7 Br -0.01387(10) 1.08756(6) 0.79397(4) 0.0514(2) Uani 1 1 d . . .
C7 C 0.6731(8) 0.2240(5) 0.2817(3) 0.0321(15) Uani 1 1 d . . .
Br6 Br 0.53910(11) 0.40378(6) 0.70252(4) 0.0539(2) Uani 1 1 d . . .
C6 C 0.6896(10) 0.4339(6) 0.1475(4) 0.048(2) Uani 1 1 d . . .
H6 H 0.6652 0.5109 0.1372 0.058 Uiso 1 1 calc R . .
N00H N 0.6441(7) 0.1367(5) 0.3970(3) 0.0390(14) Uani 1 1 d . . .
Br10 Br 0.14193(10) 1.31382(6) 0.89489(4) 0.0585(2) Uani 1 1 d . . .
C10 C 0.5443(8) 0.2356(5) 0.3750(3) 0.0378(16) Uani 1 1 d . . .
H10 H 0.4647 0.2738 0.3991 0.045 Uiso 1 1 calc R . .
Br11 Br 0.12405(11) 1.10138(7) 1.05052(4) 0.0590(2) Uani 1 1 d . . .
C11 C 0.5570(8) 0.2816(5) 0.3182(3) 0.0411(18) Uani 1 1 d . . .
H11 H 0.4882 0.3512 0.3039 0.049 Uiso 1 1 calc R . .
Br12 Br 0.35154(11) 1.35101(6) 1.06253(4) 0.0538(2) Uani 1 1 d . . .
C12 C 0.6345(11) 0.0930(7) 0.4599(3) 0.061(2) Uani 1 1 d . . .
H00A H 0.6703 0.0130 0.4652 0.091 Uiso 1 1 calc R . .
H00B H 0.5194 0.1153 0.4724 0.091 Uiso 1 1 calc R . .
H00C H 0.7076 0.1224 0.4829 0.091 Uiso 1 1 calc R . .
C13 C 1.0638(10) 0.3494(6) 0.7208(4) 0.060(2) Uani 1 1 d . . .
H01A H 1.1078 0.3045 0.7573 0.090 Uiso 1 1 calc R . .
H01B H 1.1529 0.3453 0.6927 0.090 Uiso 1 1 calc R . .
H01C H 0.9731 0.3222 0.7059 0.090 Uiso 1 1 calc R . .
C19 C 0.7811(8) 0.8029(6) 0.7518(3) 0.0360(16) Uani 1 1 d . . .
C14 C 0.8938(9) 0.4897(6) 0.7753(3) 0.0426(18) Uani 1 1 d . . .
H14 H 0.8667 0.4317 0.8007 0.051 Uiso 1 1 calc R . .
C15 C 0.8267(8) 0.5979(6) 0.7839(3) 0.0413(17) Uani 1 1 d . . .
H15 H 0.7568 0.6130 0.8156 0.050 Uiso 1 1 calc R . .
C18 C 1.0368(9) 0.5491(6) 0.6936(3) 0.0410(17) Uani 1 1 d . . .
H18 H 1.1105 0.5320 0.6630 0.049 Uiso 1 1 calc R . .
C17 C 0.9691(8) 0.6580(6) 0.6999(3) 0.0377(16) Uani 1 1 d . . .
H17 H 0.9955 0.7145 0.6732 0.045 Uiso 1 1 calc R . .
C16 C 0.8625(8) 0.6850(5) 0.7454(3) 0.0341(16) Uani 1 1 d . . .
N1K N 0.9983(7) 0.4669(5) 0.7308(3) 0.0420(15) Uani 1 1 d . . .
C20 C 0.7348(10) 0.8348(6) 0.8055(3) 0.0482(19) Uani 1 1 d . . .
H20 H 0.7616 0.7831 0.8394 0.058 Uiso 1 1 calc R . .
C21 C 0.6495(10) 0.9422(6) 0.8098(3) 0.053(2) Uani 1 1 d . . .
H21 H 0.6211 0.9626 0.8468 0.063 Uiso 1 1 calc R . .
C22 C 0.6568(9) 0.9916(6) 0.7095(3) 0.0465(19) Uani 1 1 d . . .
H22 H 0.6337 1.0463 0.6767 0.056 Uiso 1 1 calc R . .
C23 C 0.7417(9) 0.8856(6) 0.7032(3) 0.0432(18) Uani 1 1 d . . .
H23 H 0.7738 0.8683 0.6659 0.052 Uiso 1 1 calc R . .
C24 C 0.5102(11) 1.1315(6) 0.7692(4) 0.072(3) Uani 1 1 d . . .
H01G H 0.4409 1.1291 0.8033 0.107 Uiso 1 1 calc R . .
H01H H 0.4388 1.1624 0.7348 0.107 Uiso 1 1 calc R . .
H01I H 0.5882 1.1773 0.7736 0.107 Uiso 1 1 calc R . .
N1J N 0.7535(8) 0.3678(5) 0.1078(3) 0.0448(15) Uani 1 1 d . . .
N1I N 0.6066(7) 1.0173(5) 0.7627(3) 0.0424(15) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br1 2.7720(8) . ?
Pb1 Br4 2.9608(8) . ?
Pb1 Br3 3.0248(7) . ?
Pb1 Br2 3.0316(7) . ?
Pb1 Br5 3.1160(8) 2_766 ?
C1 N1J 1.484(9) . ?
C1 H01D 0.9600 . ?
C1 H01E 0.9600 . ?
C1 H01F 0.9600 . ?
Pb3 Br7 2.8066(9) . ?
Pb3 Br10 2.9826(8) . ?
Pb3 Br8 2.9856(8) . ?
Pb3 Br9 3.0712(8) . ?
Pb3 Br11 3.0771(8) 2_577 ?
C3 C2 1.360(10) . ?
C3 C4 1.378(9) . ?
C3 H3 0.9300 . ?
Br3 Pb2 3.1076(7) 2_666 ?
Pb2 Br6 2.7833(9) . ?
Pb2 Br4 2.9642(7) . ?
Pb2 Br5 3.0139(7) . ?
Pb2 Br2 3.0486(7) 1_455 ?
Pb2 Br3 3.1075(8) 2_666 ?
C2 N1J 1.331(9) . ?
C2 H2 0.9300 . ?
Br2 Pb2 3.0486(7) 1_655 ?
Pb4 Br12 2.8098(8) . ?
Pb4 Br10 2.9976(8) . ?
Pb4 Br8 3.0038(9) 1_655 ?
Pb4 Br11 3.0567(8) . ?
Pb4 Br9 3.0742(8) 2_677 ?
C4 C5 1.401(9) . ?
C4 C7 1.486(9) . ?
Br5 Pb1 3.1160(8) 2_766 ?
C5 C6 1.359(10) . ?
C5 H5 0.9300 . ?
Br9 Pb4 3.0743(8) 2_677 ?
C9 N00H 1.335(9) . ?
C9 C8 1.357(10) . ?
C9 H9 0.9300 . ?
Br8 Pb4 3.0039(9) 1_455 ?
C8 C7 1.386(8) . ?
C8 H8 0.9300 . ?
C7 C11 1.390(9) . ?
C6 N1J 1.330(9) . ?
C6 H6 0.9300 . ?
N00H C10 1.337(8) . ?
N00H C12 1.478(9) . ?
C10 C11 1.361(9) . ?
C10 H10 0.9300 . ?
Br11 Pb3 3.0771(8) 2_577 ?
C11 H11 0.9300 . ?
C12 H00A 0.9600 . ?
C12 H00B 0.9600 . ?
C12 H00C 0.9600 . ?
C13 N1K 1.483(8) . ?
C13 H01A 0.9600 . ?
C13 H01B 0.9600 . ?
C13 H01C 0.9600 . ?
C19 C20 1.368(9) . ?
C19 C23 1.391(9) . ?
C19 C16 1.488(9) . ?
C14 N1K 1.338(9) . ?
C14 C15 1.368(9) . ?
C14 H14 0.9300 . ?
C15 C16 1.386(9) . ?
C15 H15 0.9300 . ?
C18 N1K 1.334(8) . ?
C18 C17 1.365(9) . ?
C18 H18 0.9300 . ?
C17 C16 1.373(9) . ?
C17 H17 0.9300 . ?
C20 C21 1.368(10) . ?
C20 H20 0.9300 . ?
C21 N1I 1.317(9) . ?
C21 H21 0.9300 . ?
C22 N1I 1.337(9) . ?
C22 C23 1.362(9) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 N1I 1.478(9) . ?
C24 H01G 0.9600 . ?
C24 H01H 0.9600 . ?
C24 H01I 0.9600 . ?

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 Br4 92.68(3) . . ?
Br1 Pb1 Br3 85.38(2) . . ?
Br4 Pb1 Br3 88.93(2) . . ?
Br1 Pb1 Br2 91.98(2) . . ?
Br4 Pb1 Br2 85.19(2) . . ?
Br3 Pb1 Br2 173.43(2) . . ?
Br1 Pb1 Br5 89.25(2) . 2_766 ?
Br4 Pb1 Br5 173.45(2) . 2_766 ?
Br3 Pb1 Br5 84.99(2) . 2_766 ?
Br2 Pb1 Br5 101.01(2) . 2_766 ?
N1J C1 H01D 109.5 . . ?
N1J C1 H01E 109.5 . . ?
H01D C1 H01E 109.5 . . ?
N1J C1 H01F 109.5 . . ?
H01D C1 H01F 109.5 . . ?
H01E C1 H01F 109.5 . . ?
Br7 Pb3 Br10 95.54(3) . . ?
Br7 Pb3 Br8 96.16(3) . . ?
Br10 Pb3 Br8 86.51(2) . . ?
Br7 Pb3 Br9 86.80(2) . . ?
Br10 Pb3 Br9 85.34(2) . . ?
Br8 Pb3 Br9 171.56(3) . . ?
Br7 Pb3 Br11 91.06(2) . 2_577 ?
Br10 Pb3 Br11 168.92(2) . 2_577 ?
Br8 Pb3 Br11 101.65(3) . 2_577 ?
Br9 Pb3 Br11 86.16(3) . 2_577 ?
C2 C3 C4 121.2(7) . . ?
C2 C3 H3 119.4 . . ?
C4 C3 H3 119.4 . . ?
Pb1 Br3 Pb2 138.83(3) . 2_666 ?
Br6 Pb2 Br4 93.61(2) . . ?
Br6 Pb2 Br5 85.82(2) . . ?
Br4 Pb2 Br5 89.13(2) . . ?
Br6 Pb2 Br2 92.68(2) . 1_455 ?
Br4 Pb2 Br2 84.71(2) . 1_455 ?
Br5 Pb2 Br2 173.56(2) . 1_455 ?
Br6 Pb2 Br3 88.79(2) . 2_666 ?
Br4 Pb2 Br3 173.37(2) . 2_666 ?
Br5 Pb2 Br3 84.87(2) . 2_666 ?
Br2 Pb2 Br3 101.37(2) 1_455 2_666 ?
N1J C2 C3 121.3(7) . . ?
N1J C2 H2 119.4 . . ?
C3 C2 H2 119.4 . . ?
Pb1 Br2 Pb2 103.68(2) . 1_655 ?
Br12 Pb4 Br10 96.55(3) . . ?
Br12 Pb4 Br8 97.10(3) . 1_655 ?
Br10 Pb4 Br8 84.62(2) . 1_655 ?
Br12 Pb4 Br11 86.12(2) . . ?
Br10 Pb4 Br11 86.83(3) . . ?
Br8 Pb4 Br11 171.16(3) 1_655 . ?
Br12 Pb4 Br9 90.58(2) . 2_677 ?
Br10 Pb4 Br9 169.12(2) . 2_677 ?
Br8 Pb4 Br9 102.69(3) 1_655 2_677 ?
Br11 Pb4 Br9 85.46(3) . 2_677 ?
C3 C4 C5 115.5(7) . . ?
C3 C4 C7 122.4(6) . . ?
C5 C4 C7 122.1(6) . . ?
Pb1 Br4 Pb2 87.54(2) . . ?
Pb2 Br5 Pb1 137.87(3) . 2_766 ?
C6 C5 C4 121.4(7) . . ?
C6 C5 H5 119.3 . . ?
C4 C5 H5 119.3 . . ?
Pb3 Br9 Pb4 138.91(3) . 2_677 ?
N00H C9 C8 121.5(7) . . ?
N00H C9 H9 119.2 . . ?
C8 C9 H9 119.2 . . ?
Pb3 Br8 Pb4 108.36(3) . 1_455 ?
C9 C8 C7 119.9(7) . . ?
C9 C8 H8 120.1 . . ?
C7 C8 H8 120.1 . . ?
C8 C7 C11 117.7(6) . . ?
C8 C7 C4 121.2(6) . . ?
C11 C7 C4 121.0(6) . . ?
N1J C6 C5 120.5(7) . . ?
N1J C6 H6 119.8 . . ?
C5 C6 H6 119.8 . . ?
C9 N00H C10 119.9(6) . . ?
C9 N00H C12 120.4(6) . . ?
C10 N00H C12 119.6(6) . . ?
Pb3 Br10 Pb4 87.93(2) . . ?
N00H C10 C11 121.3(6) . . ?
N00H C10 H10 119.4 . . ?
C11 C10 H10 119.4 . . ?
Pb4 Br11 Pb3 140.26(3) . 2_577 ?
C10 C11 C7 119.7(6) . . ?
C10 C11 H11 120.1 . . ?
C7 C11 H11 120.1 . . ?
N00H C12 H00A 109.5 . . ?
N00H C12 H00B 109.5 . . ?
H00A C12 H00B 109.5 . . ?
N00H C12 H00C 109.5 . . ?
H00A C12 H00C 109.5 . . ?
H00B C12 H00C 109.5 . . ?
N1K C13 H01A 109.5 . . ?
N1K C13 H01B 109.5 . . ?
H01A C13 H01B 109.5 . . ?
N1K C13 H01C 109.5 . . ?
H01A C13 H01C 109.5 . . ?
H01B C13 H01C 109.5 . . ?
C20 C19 C23 116.5(7) . . ?
C20 C19 C16 121.7(6) . . ?
C23 C19 C16 121.8(6) . . ?
N1K C14 C15 120.4(7) . . ?
N1K C14 H14 119.8 . . ?
C15 C14 H14 119.8 . . ?
C14 C15 C16 120.2(7) . . ?
C14 C15 H15 119.9 . . ?
C16 C15 H15 119.9 . . ?
N1K C18 C17 120.6(7) . . ?
N1K C18 H18 119.7 . . ?
C17 C18 H18 119.7 . . ?
C18 C17 C16 120.6(6) . . ?
C18 C17 H17 119.7 . . ?
C16 C17 H17 119.7 . . ?
C17 C16 C15 117.5(6) . . ?
C17 C16 C19 121.7(6) . . ?
C15 C16 C19 120.7(6) . . ?
C18 N1K C14 120.6(6) . . ?
C18 N1K C13 119.8(6) . . ?
C14 N1K C13 119.5(6) . . ?
C19 C20 C21 120.6(7) . . ?
C19 C20 H20 119.7 . . ?
C21 C20 H20 119.7 . . ?
N1I C21 C20 121.5(7) . . ?
N1I C21 H21 119.3 . . ?
C20 C21 H21 119.3 . . ?
N1I C22 C23 120.3(7) . . ?
N1I C22 H22 119.9 . . ?
C23 C22 H22 119.9 . . ?
C22 C23 C19 120.9(7) . . ?
C22 C23 H23 119.5 . . ?
C19 C23 H23 119.5 . . ?
N1I C24 H01G 109.5 . . ?
N1I C24 H01H 109.5 . . ?
H01G C24 H01H 109.5 . . ?
N1I C24 H01I 109.5 . . ?
H01G C24 H01I 109.5 . . ?
H01H C24 H01I 109.5 . . ?
C6 N1J C2 120.0(7) . . ?
C6 N1J C1 120.7(6) . . ?
C2 N1J C1 119.2(7) . . ?
C21 N1I C22 120.0(6) . . ?
C21 N1I C24 119.8(7) . . ?
C22 N1I C24 120.2(7) . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        27.10
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         1.385
_refine_diff_density_min         -1.959
_refine_diff_density_rms         0.243
####################################################################### 
# 
# 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_02_a
_database_code_depnum_ccdc_archive 'CCDC 1486416'
_audit_update_record             
;
2016-06-18 deposited with the CCDC.
2016-09-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H28 Br18 N4 Pb7'
_chemical_formula_weight         3261.21

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           Triclinic'
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.7421(6)
_cell_length_b                   12.9277(8)
_cell_length_c                   13.2958(8)
_cell_angle_alpha                116.0700(10)
_cell_angle_beta                 110.7090(10)
_cell_angle_gamma                90.9180(10)
_cell_volume                     1377.36(15)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5452
_cell_measurement_theta_min      2.28
_cell_measurement_theta_max      27.30

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.932
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1404
_exptl_absorpt_coefficient_mu    34.390
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0604
_exptl_absorpt_correction_T_max  0.5463
_exptl_absorpt_process_details   'Bruker SADABS'

_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_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15048
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_av_sigmaI/netI    0.0782
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.79
_diffrn_reflns_theta_max         26.37
_reflns_number_total             5612
_reflns_number_gt                4642
_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 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0066P)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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5612
_refine_ls_number_parameters     243
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0365
_refine_ls_wR_factor_ref         0.0925
_refine_ls_wR_factor_gt          0.0874
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_restrained_S_all      1.009
_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 1.0000 1.0000 0.03267(13) Uani 1 2 d S . .
C1 C 0.5629(12) 0.3576(9) 0.3030(10) 0.050(3) Uani 1 1 d . . .
H1A H 0.6400 0.3405 0.2724 0.074 Uiso 1 1 calc R . .
H1B H 0.5018 0.2853 0.2797 0.074 Uiso 1 1 calc R . .
H1C H 0.6079 0.4030 0.3905 0.074 Uiso 1 1 calc R . .
Br1 Br 0.19323(12) 0.87972(9) 0.79920(9) 0.0448(3) Uani 1 1 d . . .
Pb2 Pb 0.59227(3) 0.88588(3) 0.58425(3) 0.02744(10) Uani 1 1 d . . .
C2 C 0.5252(11) 0.4836(8) 0.2081(8) 0.037(2) Uani 1 1 d . . .
H2 H 0.6216 0.4807 0.2106 0.044 Uiso 1 1 calc R . .
Br2 Br 0.67174(12) 0.94968(10) 0.84030(9) 0.0462(3) Uani 1 1 d . . .
Pb3 Pb 0.76344(4) 0.94046(3) 0.32303(3) 0.03482(11) Uani 1 1 d . . .
C3 C 0.4398(10) 0.5489(8) 0.1592(8) 0.033(2) Uani 1 1 d . . .
H3 H 0.4796 0.5893 0.1294 0.040 Uiso 1 1 calc R . .
Br3 Br 0.27455(10) 0.78464(9) 0.50503(10) 0.0435(3) Uani 1 1 d . . .
Pb4 Pb 0.98851(4) 0.69541(3) 0.52401(3) 0.03664(11) Uani 1 1 d . . .
C4 C 0.2960(9) 0.5537(8) 0.1548(8) 0.031(2) Uani 1 1 d . . .
Br4 Br 0.89617(10) 0.97623(9) 0.59577(9) 0.0400(2) Uani 1 1 d . . .
C12 C -0.0374(12) 0.8478(10) -0.0146(11) 0.057(3) Uani 1 1 d . . .
H12A H -0.1344 0.8415 -0.0123 0.086 Uiso 1 1 calc R . .
H12B H -0.0489 0.8255 -0.0967 0.086 Uiso 1 1 calc R . .
H12C H 0.0173 0.9275 0.0386 0.086 Uiso 1 1 calc R . .
Br5 Br 0.47969(9) 0.86632(7) 0.33008(8) 0.0293(2) Uani 1 1 d . . .
C5 C 0.2459(11) 0.4938(9) 0.2020(9) 0.042(2) Uani 1 1 d . . .
H5 H 0.1503 0.4964 0.2016 0.051 Uiso 1 1 calc R . .
Br6 Br 0.68743(10) 0.65969(8) 0.52682(9) 0.0382(2) Uani 1 1 d . . .
C6 C 0.3282(11) 0.4314(9) 0.2491(9) 0.044(3) Uani 1 1 d . . .
H6 H 0.2894 0.3921 0.2804 0.053 Uiso 1 1 calc R . .
Br7 Br 0.59130(11) 0.79511(8) 0.04647(9) 0.0401(2) Uani 1 1 d . . .
C7 C 0.2067(9) 0.6260(8) 0.1081(8) 0.031(2) Uani 1 1 d . . .
Br8 Br 0.82620(10) 0.70979(8) 0.28509(9) 0.0352(2) Uani 1 1 d . . .
C8 C 0.2305(11) 0.6510(9) 0.0246(9) 0.039(2) Uani 1 1 d . . .
H8 H 0.3012 0.6194 -0.0057 0.047 Uiso 1 1 calc R . .
N13 N 0.4690(8) 0.4252(7) 0.2513(7) 0.0376(19) Uani 1 1 d . . .
Br9 Br 0.96025(11) 0.45560(8) 0.33573(9) 0.0417(2) Uani 1 1 d . . .
C9 C 0.1494(11) 0.7230(9) -0.0149(9) 0.043(3) Uani 1 1 d . . .
H9 H 0.1672 0.7399 -0.0708 0.051 Uiso 1 1 calc R . .
N14 N 0.0464(8) 0.7683(7) 0.0265(7) 0.039(2) Uani 1 1 d . . .
C11 C 0.0981(10) 0.6734(9) 0.1484(9) 0.043(3) Uani 1 1 d . . .
H11 H 0.0786 0.6575 0.2044 0.052 Uiso 1 1 calc R . .
C10 C 0.0198(11) 0.7427(9) 0.1073(9) 0.045(3) Uani 1 1 d . . .
H10 H -0.0533 0.7732 0.1350 0.054 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 3.0061(10) . ?
Pb1 Br1 3.0061(10) 2_677 ?
Pb1 Br2 3.0107(10) . ?
Pb1 Br2 3.0107(10) 2_677 ?
Pb1 Br7 3.0519(10) 1_556 ?
Pb1 Br7 3.0520(10) 2_676 ?
C1 N13 1.478(12) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
Br1 Pb4 3.1728(10) 1_455 ?
Pb2 Br2 2.9185(10) . ?
Pb2 Br6 2.9356(10) . ?
Pb2 Br3 2.9591(10) . ?
Pb2 Br5 3.0505(10) . ?
Pb2 Br5 3.0791(9) 2_676 ?
Pb2 Br4 3.0926(10) . ?
C2 N13 1.338(12) . ?
C2 C3 1.396(13) . ?
C2 H2 0.9300 . ?
Pb3 Br8 2.9113(10) . ?
Pb3 Br5 2.9574(9) . ?
Pb3 Br7 3.0543(10) . ?
Pb3 Br4 3.1070(9) 2_776 ?
Pb3 Br4 3.1978(11) . ?
C3 C4 1.384(11) . ?
C3 H3 0.9300 . ?
Br3 Pb4 3.1319(10) 1_455 ?
Pb4 Br9 2.9356(10) . ?
Pb4 Br6 2.9779(10) . ?
Pb4 Br8 3.0986(11) . ?
Pb4 Br3 3.1320(10) 1_655 ?
Pb4 Br1 3.1728(10) 1_655 ?
Pb4 Br9 3.1798(11) 2_766 ?
C4 C5 1.366(13) . ?
C4 C7 1.474(13) . ?
Br4 Pb3 3.1070(9) 2_776 ?
C12 N14 1.493(13) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
Br5 Pb2 3.0791(9) 2_676 ?
C5 C6 1.339(14) . ?
C5 H5 0.9300 . ?
C6 N13 1.366(12) . ?
C6 H6 0.9300 . ?
Br7 Pb1 3.0520(10) 1_554 ?
C7 C8 1.373(12) . ?
C7 C11 1.384(11) . ?
C8 C9 1.388(13) . ?
C8 H8 0.9300 . ?
Br9 Pb4 3.1798(11) 2_766 ?
C9 N14 1.333(11) . ?
C9 H9 0.9300 . ?
N14 C10 1.354(12) . ?
C11 C10 1.358(14) . ?
C11 H11 0.9300 . ?
C10 H10 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br1 Pb1 Br1 179.999(1) . 2_677 ?
Br1 Pb1 Br2 97.54(3) . . ?
Br1 Pb1 Br2 82.46(3) 2_677 . ?
Br1 Pb1 Br2 82.46(3) . 2_677 ?
Br1 Pb1 Br2 97.54(3) 2_677 2_677 ?
Br2 Pb1 Br2 180.0 . 2_677 ?
Br1 Pb1 Br7 99.32(3) . 1_556 ?
Br1 Pb1 Br7 80.68(3) 2_677 1_556 ?
Br2 Pb1 Br7 90.08(3) . 1_556 ?
Br2 Pb1 Br7 89.92(3) 2_677 1_556 ?
Br1 Pb1 Br7 80.68(3) . 2_676 ?
Br1 Pb1 Br7 99.33(3) 2_677 2_676 ?
Br2 Pb1 Br7 89.92(3) . 2_676 ?
Br2 Pb1 Br7 90.08(3) 2_677 2_676 ?
Br7 Pb1 Br7 180.00(4) 1_556 2_676 ?
N13 C1 H1A 109.5 . . ?
N13 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N13 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Pb1 Br1 Pb4 149.58(4) . 1_455 ?
Br2 Pb2 Br6 93.51(3) . . ?
Br2 Pb2 Br3 94.31(3) . . ?
Br6 Pb2 Br3 94.27(3) . . ?
Br2 Pb2 Br5 167.63(3) . . ?
Br6 Pb2 Br5 98.74(3) . . ?
Br3 Pb2 Br5 83.12(3) . . ?
Br2 Pb2 Br5 81.85(3) . 2_676 ?
Br6 Pb2 Br5 174.11(3) . 2_676 ?
Br3 Pb2 Br5 89.71(3) . 2_676 ?
Br5 Pb2 Br5 86.02(2) . 2_676 ?
Br2 Pb2 Br4 100.77(3) . . ?
Br6 Pb2 Br4 85.76(3) . . ?
Br3 Pb2 Br4 164.89(3) . . ?
Br5 Pb2 Br4 81.95(3) . . ?
Br5 Pb2 Br4 91.52(3) 2_676 . ?
N13 C2 C3 120.3(9) . . ?
N13 C2 H2 119.8 . . ?
C3 C2 H2 119.8 . . ?
Pb2 Br2 Pb1 134.64(4) . . ?
Br8 Pb3 Br5 87.37(3) . . ?
Br8 Pb3 Br7 79.43(3) . . ?
Br5 Pb3 Br7 83.82(3) . . ?
Br8 Pb3 Br4 87.27(3) . 2_776 ?
Br5 Pb3 Br4 160.16(3) . 2_776 ?
Br7 Pb3 Br4 113.88(3) . 2_776 ?
Br8 Pb3 Br4 77.97(3) . . ?
Br5 Pb3 Br4 81.65(2) . . ?
Br7 Pb3 Br4 153.57(3) . . ?
Br4 Pb3 Br4 78.55(3) 2_776 . ?
C4 C3 C2 120.3(9) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
Pb2 Br3 Pb4 158.17(4) . 1_455 ?
Br9 Pb4 Br6 96.91(3) . . ?
Br9 Pb4 Br8 77.94(3) . . ?
Br6 Pb4 Br8 86.84(3) . . ?
Br9 Pb4 Br3 91.25(3) . 1_655 ?
Br6 Pb4 Br3 165.02(3) . 1_655 ?
Br8 Pb4 Br3 82.60(3) . 1_655 ?
Br9 Pb4 Br1 141.19(3) . 1_655 ?
Br6 Pb4 Br1 103.55(3) . 1_655 ?
Br8 Pb4 Br1 135.12(3) . 1_655 ?
Br3 Pb4 Br1 77.08(3) 1_655 1_655 ?
Br9 Pb4 Br9 75.87(3) . 2_766 ?
Br6 Pb4 Br9 79.30(3) . 2_766 ?
Br8 Pb4 Br9 148.50(3) . 2_766 ?
Br3 Pb4 Br9 115.00(3) 1_655 2_766 ?
Br1 Pb4 Br9 76.03(3) 1_655 2_766 ?
C5 C4 C3 116.6(9) . . ?
C5 C4 C7 122.3(8) . . ?
C3 C4 C7 121.0(8) . . ?
Pb2 Br4 Pb3 163.05(4) . 2_776 ?
Pb2 Br4 Pb3 95.11(3) . . ?
Pb3 Br4 Pb3 101.45(3) 2_776 . ?
N14 C12 H12A 109.5 . . ?
N14 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N14 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Pb3 Br5 Pb2 101.19(3) . . ?
Pb3 Br5 Pb2 93.72(3) . 2_676 ?
Pb2 Br5 Pb2 93.98(2) . 2_676 ?
C6 C5 C4 122.9(9) . . ?
C6 C5 H5 118.5 . . ?
C4 C5 H5 118.5 . . ?
Pb2 Br6 Pb4 106.20(3) . . ?
C5 C6 N13 120.3(9) . . ?
C5 C6 H6 119.9 . . ?
N13 C6 H6 119.9 . . ?
Pb1 Br7 Pb3 96.64(3) 1_554 . ?
C8 C7 C11 117.5(9) . . ?
C8 C7 C4 121.1(8) . . ?
C11 C7 C4 121.5(8) . . ?
Pb3 Br8 Pb4 114.31(3) . . ?
C7 C8 C9 120.4(9) . . ?
C7 C8 H8 119.8 . . ?
C9 C8 H8 119.8 . . ?
C2 N13 C6 119.5(9) . . ?
C2 N13 C1 118.8(8) . . ?
C6 N13 C1 121.6(8) . . ?
Pb4 Br9 Pb4 104.13(3) . 2_766 ?
N14 C9 C8 120.8(9) . . ?
N14 C9 H9 119.6 . . ?
C8 C9 H9 119.6 . . ?
C9 N14 C10 119.5(9) . . ?
C9 N14 C12 120.2(9) . . ?
C10 N14 C12 120.3(9) . . ?
C10 C11 C7 120.8(10) . . ?
C10 C11 H11 119.6 . . ?
C7 C11 H11 119.6 . . ?
N14 C10 C11 121.0(9) . . ?
N14 C10 H10 119.5 . . ?
C11 C10 H10 119.5 . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         2.191
_refine_diff_density_min         -1.644
_refine_diff_density_rms         0.285
####################################################################### 
# 
# 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_02_a
_database_code_depnum_ccdc_archive 'CCDC 1486417'
_audit_update_record             
;
2016-06-18 deposited with the CCDC.
2016-09-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H28 Br10 N4 Pb3'
_chemical_formula_weight         1793.17

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   C2/m

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

_cell_length_a                   18.748(3)
_cell_length_b                   9.5035(16)
_cell_length_c                   12.453(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.850(2)
_cell_angle_gamma                90.00
_cell_volume                     2073.5(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1493
_cell_measurement_theta_min      2.32
_cell_measurement_theta_max      24.53

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.872
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1592
_exptl_absorpt_coefficient_mu    21.805
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0818
_exptl_absorpt_correction_T_max  0.3187
_exptl_absorpt_process_details   'Bruker SADABS'

_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_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5952
_diffrn_reflns_av_R_equivalents  0.0699
_diffrn_reflns_av_sigmaI/netI    0.0900
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.32
_diffrn_reflns_theta_max         26.37
_reflns_number_total             2243
_reflns_number_gt                1713
_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, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0485P)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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2243
_refine_ls_number_parameters     111
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0490
_refine_ls_wR_factor_ref         0.1258
_refine_ls_wR_factor_gt          0.1153
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_restrained_S_all      0.996
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.7622(8) 0.5000 0.0308(11) 0.053(4) Uani 1 2 d S . .
H1A H 0.7607 0.5951 0.0040 0.079 Uiso 0.50 1 calc PR . .
H1B H 0.7129 0.4575 -0.0044 0.079 Uiso 0.50 1 calc PR . .
H1C H 0.7994 0.4474 0.0108 0.079 Uiso 0.50 1 calc PR . .
Pb1 Pb 0.54176(3) 0.5000 0.69566(4) 0.0358(2) Uani 1 2 d S . .
Br1 Br 0.69934(8) 0.5000 0.72047(13) 0.0446(4) Uani 1 2 d S . .
C8 C 0.9163(11) 0.5000 0.8802(12) 0.065(5) Uani 1 2 d S . .
H8A H 0.9115 0.5932 0.9066 0.097 Uiso 0.50 1 calc PR . .
H8B H 0.9687 0.4705 0.9123 0.097 Uiso 0.50 1 calc PR . .
H8C H 0.8850 0.4363 0.9039 0.097 Uiso 0.50 1 calc PR . .
C7 C 0.8789(7) 0.3811(12) 0.6967(9) 0.052(3) Uani 1 1 d . . .
H7 H 0.8856 0.2970 0.7373 0.062 Uiso 1 1 calc R . .
C6 C 0.8567(6) 0.3766(11) 0.5810(9) 0.046(3) Uani 1 1 d . . .
H6 H 0.8494 0.2902 0.5435 0.055 Uiso 1 1 calc R . .
N1 N 0.7831(6) 0.5000 0.1571(9) 0.036(3) Uani 1 2 d S . .
Br2 Br 0.5000 0.29150(16) 0.5000 0.0512(4) Uani 1 2 d S . .
C2 C 0.7924(6) 0.3773(11) 0.2146(9) 0.046(3) Uani 1 1 d . . .
H2 H 0.7852 0.2928 0.1744 0.055 Uiso 1 1 calc R . .
Pb2 Pb 0.5000 0.5000 1.0000 0.0416(2) Uani 1 4 d S . .
N2 N 0.8914(6) 0.5000 0.7535(9) 0.037(3) Uani 1 2 d S . .
Br3 Br 0.57649(7) 0.71818(12) 0.89773(10) 0.0536(3) Uani 1 1 d . . .
C3 C 0.8118(6) 0.3756(11) 0.3296(9) 0.045(3) Uani 1 1 d . . .
H3 H 0.8174 0.2900 0.3679 0.054 Uiso 1 1 calc R . .
Br4 Br 0.61282(9) 0.5000 1.24508(19) 0.0718(6) Uani 1 2 d S . .
C4 C 0.8237(7) 0.5000 0.3911(10) 0.029(3) Uani 1 2 d S . .
C5 C 0.8448(7) 0.5000 0.5179(11) 0.032(3) Uani 1 2 d S . .


_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
C1 N1 1.479(16) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
Pb1 Br1 2.8591(15) . ?
Pb1 Br2 3.0197(12) . ?
Pb1 Br2 3.0197(12) 5_666 ?
Pb1 Br3 3.1446(12) 6_565 ?
Pb1 Br3 3.1447(12) . ?
Pb1 Br4 3.2352(19) 5_667 ?
C8 N2 1.477(17) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C7 N2 1.310(12) . ?
C7 C6 1.350(14) . ?
C7 H7 0.9300 . ?
C6 C5 1.385(12) . ?
C6 H6 0.9300 . ?
N1 C2 1.347(11) 6_565 ?
N1 C2 1.347(11) . ?
Br2 Pb1 3.0197(11) 5_666 ?
C2 C3 1.346(14) . ?
C2 H2 0.9300 . ?
Pb2 Br4 3.032(2) . ?
Pb2 Br4 3.032(2) 5_667 ?
Pb2 Br3 3.0460(11) 5_667 ?
Pb2 Br3 3.0460(11) . ?
Pb2 Br3 3.0460(11) 6_565 ?
Pb2 Br3 3.0461(11) 2_657 ?
N2 C7 1.310(12) 6_565 ?
C3 C4 1.384(11) . ?
C3 H3 0.9300 . ?
Br4 Pb1 3.2352(19) 5_667 ?
C4 C3 1.384(11) 6_565 ?
C4 C5 1.484(17) . ?
C5 C6 1.385(12) 6_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
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Br1 Pb1 Br2 92.77(3) . . ?
Br1 Pb1 Br2 92.77(3) . 5_666 ?
Br2 Pb1 Br2 82.02(5) . 5_666 ?
Br1 Pb1 Br3 90.10(3) . 6_565 ?
Br2 Pb1 Br3 97.67(4) . 6_565 ?
Br2 Pb1 Br3 177.12(3) 5_666 6_565 ?
Br1 Pb1 Br3 90.11(3) . . ?
Br2 Pb1 Br3 177.12(3) . . ?
Br2 Pb1 Br3 97.67(4) 5_666 . ?
Br3 Pb1 Br3 82.50(5) 6_565 . ?
Br1 Pb1 Br4 161.90(5) . 5_667 ?
Br2 Pb1 Br4 100.84(3) . 5_667 ?
Br2 Pb1 Br4 100.84(3) 5_666 5_667 ?
Br3 Pb1 Br4 76.39(4) 6_565 5_667 ?
Br3 Pb1 Br4 76.39(4) . 5_667 ?
N2 C8 H8A 109.5 . . ?
N2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C7 C6 122.1(11) . . ?
N2 C7 H7 119.0 . . ?
C6 C7 H7 119.0 . . ?
C7 C6 C5 120.3(11) . . ?
C7 C6 H6 119.8 . . ?
C5 C6 H6 119.8 . . ?
C2 N1 C2 119.9(12) 6_565 . ?
C2 N1 C1 120.0(6) 6_565 . ?
C2 N1 C1 120.0(6) . . ?
Pb1 Br2 Pb1 97.98(5) . 5_666 ?
N1 C2 C3 120.7(11) . . ?
N1 C2 H2 119.6 . . ?
C3 C2 H2 119.6 . . ?
Br4 Pb2 Br4 180.0 . 5_667 ?
Br4 Pb2 Br3 80.95(4) . 5_667 ?
Br4 Pb2 Br3 99.05(4) 5_667 5_667 ?
Br4 Pb2 Br3 99.05(4) . . ?
Br4 Pb2 Br3 80.95(4) 5_667 . ?
Br3 Pb2 Br3 180.00(4) 5_667 . ?
Br4 Pb2 Br3 99.05(4) . 6_565 ?
Br4 Pb2 Br3 80.95(4) 5_667 6_565 ?
Br3 Pb2 Br3 94.20(4) 5_667 6_565 ?
Br3 Pb2 Br3 85.80(4) . 6_565 ?
Br4 Pb2 Br3 80.95(4) . 2_657 ?
Br4 Pb2 Br3 99.05(4) 5_667 2_657 ?
Br3 Pb2 Br3 85.80(4) 5_667 2_657 ?
Br3 Pb2 Br3 94.20(4) . 2_657 ?
Br3 Pb2 Br3 180.0 6_565 2_657 ?
C7 N2 C7 119.4(13) 6_565 . ?
C7 N2 C8 120.3(6) 6_565 . ?
C7 N2 C8 120.3(6) . . ?
Pb2 Br3 Pb1 83.77(3) . . ?
C2 C3 C4 120.6(10) . . ?
C2 C3 H3 119.7 . . ?
C4 C3 H3 119.7 . . ?
Pb2 Br4 Pb1 82.47(4) . 5_667 ?
C3 C4 C3 117.4(12) 6_565 . ?
C3 C4 C5 121.2(6) 6_565 . ?
C3 C4 C5 121.2(6) . . ?
C6 C5 C6 115.8(12) . 6_565 ?
C6 C5 C4 122.1(6) . . ?
C6 C5 C4 122.1(6) 6_565 . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         2.415
_refine_diff_density_min         -2.821
_refine_diff_density_rms         0.288
