# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1917733'
loop_
_audit_author_name
_audit_author_address
'Yuan-Yuan Guo'
;University of St Andrews
United Kingdom
;
_audit_update_record             
;
2019-05-21 deposited with the CCDC.	2019-07-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Pb0  Br0  N2  C0  H1'
_chemical_formula_sum            'C4 H11 Br4 N5 Pb'
_chemical_formula_weight         656.01

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

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   6.0602(16)
_cell_length_b                   9.3286(2)
_cell_length_c                   12.8673(3)
_cell_angle_alpha                95.127(2)
_cell_angle_beta                 93.490(2)
_cell_angle_gamma                92.402(2)
_cell_volume                     722.35(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    93(2)
_cell_measurement_reflns_used    13257
_cell_measurement_theta_min      2.175
_cell_measurement_theta_max      27.987

_exptl_crystal_description       Platelet
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    3.016
_exptl_crystal_F_000             584
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    22.718
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.14880
_exptl_absorpt_correction_T_max  0.17222
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      93(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Fine-Focus Sealed X-ray Tube'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15685
_diffrn_reflns_av_unetI/netI     0.0159
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.590
_diffrn_reflns_theta_max         24.993
_diffrn_reflns_theta_full        24.993
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2539
_reflns_number_gt                2422
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_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)+(0.0458P)²+3.7621P] 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         2539
_refine_ls_number_parameters     140
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0256
_refine_ls_wR_factor_ref         0.0720
_refine_ls_wR_factor_gt          0.0717
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_restrained_S_all      1.143
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.48606(3) 0.27091(2) 0.16192(2) 0.01334(10) Uani 1 1 d . . . . .
Br1 Br 0.52532(10) 0.50284(6) 0.33301(5) 0.01942(15) Uani 1 1 d . . . . .
Br2 Br 0.500000 0.000000 0.000000 0.01840(19) Uani 1 2 d S . P . .
Br3 Br 0.98089(8) 0.28185(6) 0.15483(4) 0.01792(15) Uani 1 1 d . . . . .
Br4 Br 0.50364(10) 0.06477(6) 0.32023(5) 0.01964(15) Uani 1 1 d . . . . .
Br5 Br 0.500000 0.500000 0.000000 0.0268(2) Uani 1 2 d S . P . .
N4 N 0.1218(10) 0.2157(7) 0.4620(5) 0.0333(14) Uani 1 1 d . . . . .
H7 H 0.231725 0.188681 0.427080 0.040 Uiso 1 1 calc R U . . .
N5 N -0.1626(9) 0.3254(6) 0.5078(5) 0.0263(12) Uani 1 1 d . . . . .
H8 H -0.269787 0.382958 0.508374 0.032 Uiso 1 1 calc R U . . .
C2 C -0.0226(11) 0.3120(7) 0.4341(5) 0.0248(14) Uani 1 1 d . . . . .
H9 H -0.023593 0.360216 0.373845 0.030 Uiso 1 1 calc R U . . .
C3 C 0.0679(12) 0.1667(8) 0.5545(6) 0.0317(16) Uani 1 1 d . . . . .
H10 H 0.142357 0.099267 0.590524 0.038 Uiso 1 1 calc R U . . .
C4 C -0.1152(11) 0.2351(7) 0.5841(5) 0.0265(14) Uani 1 1 d . . . . .
H11 H -0.191995 0.223351 0.643430 0.032 Uiso 1 1 calc R U . . .
C1 C 0.0606(12) 0.2249(7) 0.8591(7) 0.061(3) Uani 0.7 1 d D . P A 1
N1 N 0.2551(12) 0.2273(8) 0.8060(6) 0.0245(17) Uani 0.7 1 d D . P A 1
H1 H 0.316194 0.148057 0.788094 0.029 Uiso 0.7 1 calc R U P A 1
H2 H 0.313593 0.307984 0.791283 0.029 Uiso 0.7 1 calc R U P A 1
N2 N -0.0693(14) 0.3466(8) 0.8681(6) 0.0255(18) Uani 0.7 1 d D . P A 1
H3 H -0.029371 0.423597 0.840819 0.031 Uiso 0.7 1 calc R U P A 1
H4 H -0.188648 0.343797 0.900978 0.031 Uiso 0.7 1 calc R U P A 1
N3 N -0.0316(15) 0.0912(8) 0.8822(8) 0.042(2) Uani 0.7 1 d D . P A 1
H5 H 0.031620 0.013007 0.863715 0.050 Uiso 0.7 1 calc R U P A 1
H6 H -0.151227 0.087829 0.914810 0.050 Uiso 0.7 1 calc R U P A 1
C1' C 0.0606(12) 0.2249(7) 0.8591(7) 0.061(3) Uani 0.3 1 d D . P B 2
N1' N 0.084(4) 0.3667(15) 0.824(2) 0.058(4) Uiso 0.3 1 d D . P B 2
H1' H 0.139790 0.377988 0.765269 0.070 Uiso 0.3 1 calc R U P B 2
H2' H 0.041958 0.440037 0.861785 0.070 Uiso 0.3 1 calc R U P B 2
N2' N -0.1664(19) 0.185(3) 0.876(2) 0.058(4) Uiso 0.3 1 d D . P B 2
H3' H -0.268602 0.244645 0.865653 0.070 Uiso 0.3 1 calc R U P B 2
H4' H -0.199306 0.102796 0.897574 0.070 Uiso 0.3 1 calc R U P B 2
N3' N 0.116(4) 0.0861(15) 0.812(2) 0.058(4) Uiso 0.3 1 d D . P B 2
H5' H 0.174312 0.079418 0.752557 0.070 Uiso 0.3 1 calc R U P B 2
H6' H 0.091641 0.010065 0.843511 0.070 Uiso 0.3 1 calc R U P B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br4 2.9240(6) . ?
Pb1 Br1 2.9370(6) . ?
Pb1 Br3 3.0035(10) . ?
Pb1 Br3 3.0635(10) 1_455 ?
Pb1 Br5 3.1172(2) . ?
Pb1 Br2 3.1358(2) . ?
N4 C2 1.337(9) . ?
N4 C3 1.365(10) . ?
N5 C2 1.313(8) . ?
N5 C4 1.374(9) . ?
C3 C4 1.361(10) . ?
C1 N1 1.398(5) . ?
C1 N3 1.409(5) . ?
C1 N2 1.408(5) . ?
C1' N1' 1.439(5) . ?
C1' N3' 1.442(5) . ?
C1' N2' 1.445(5) . ?

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
Br4 Pb1 Br1 88.000(17) . . ?
Br4 Pb1 Br3 91.480(17) . . ?
Br1 Pb1 Br3 89.628(16) . . ?
Br4 Pb1 Br3 93.901(17) . 1_455 ?
Br1 Pb1 Br3 90.145(16) . 1_455 ?
Br3 Pb1 Br3 174.60(2) . 1_455 ?
Br4 Pb1 Br5 175.904(14) . . ?
Br1 Pb1 Br5 89.817(13) . . ?
Br3 Pb1 Br5 85.038(12) . . ?
Br3 Pb1 Br5 89.569(12) 1_455 . ?
Br4 Pb1 Br2 85.322(13) . . ?
Br1 Pb1 Br2 171.066(14) . . ?
Br3 Pb1 Br2 84.626(12) . . ?
Br3 Pb1 Br2 96.217(12) 1_455 . ?
Br5 Pb1 Br2 96.478(6) . . ?
Pb1 Br2 Pb1 180.0 . 2_655 ?
Pb1 Br3 Pb1 174.60(2) . 1_655 ?
Pb1 Br5 Pb1 180.0 2_665 . ?
C2 N4 C3 109.6(6) . . ?
C2 N5 C4 111.0(6) . . ?
N5 C2 N4 106.9(6) . . ?
C4 C3 N4 107.1(6) . . ?
C3 C4 N5 105.4(6) . . ?
N1 C1 N3 118.8(7) . . ?
N1 C1 N2 120.9(7) . . ?
N3 C1 N2 118.7(7) . . ?
N1' C1' N3' 131.3(16) . . ?
N1' C1' N2' 112.2(15) . . ?
N3' C1' N2' 96.7(13) . . ?

_refine_diff_density_max         2.231
_refine_diff_density_min         -1.575
_refine_diff_density_rms         0.201

####################################################################### 
# 
# 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_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1917734'
loop_
_audit_author_name
_audit_author_address
'Yuan-Yuan Guo'
;University of St Andrews
United Kingdom
;
_audit_update_record             
;
2019-05-21 deposited with the CCDC.	2019-07-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Br4 Pb, C2 H4 N3, C H6 N3'
_chemical_formula_sum            'C3 H10 Br4 N6 Pb'
_chemical_formula_weight         657.00

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   6.003(2)
_cell_length_b                   26.969(9)
_cell_length_c                   8.613(3)
_cell_angle_alpha                90
_cell_angle_beta                 96.470(8)
_cell_angle_gamma                90
_cell_volume                     1385.5(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    93(2)
_cell_measurement_reflns_used    3386
_cell_measurement_theta_min      2.5
_cell_measurement_theta_max      27.6

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    3.150
_exptl_crystal_F_000             1168
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    23.690
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.3
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      93(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating Anode'
_diffrn_measurement_device_type  
;
Rigaku Pilatus 200K
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_reflns_number            16723
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_av_R_equivalents  0.0671
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.497
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_full        24.998
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.988
_reflns_number_total             2411
_reflns_number_gt                2180
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_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)+(0.0480P)²] 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         2411
_refine_ls_number_parameters     127
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0291
_refine_ls_wR_factor_ref         0.0782
_refine_ls_wR_factor_gt          0.0775
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_restrained_S_all      1.089
_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_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 0.41556(4) 0.33256(2) 0.88284(3) 0.01553(12) Uani 1 1 d . . . . .
Br1 Br -0.07474(10) 0.32357(3) 0.87224(8) 0.02194(19) Uani 1 1 d . . . . .
Br2 Br 0.40827(10) 0.42004(3) 1.07013(8) 0.02275(18) Uani 1 1 d . . . . .
Br3 Br 0.42223(10) 0.25887(3) 1.15165(8) 0.02317(18) Uani 1 1 d . . . . .
Br4 Br 0.39470(11) 0.40404(3) 0.61714(8) 0.02371(19) Uani 1 1 d . . . . .
N1 N 1.0814(9) 0.5498(2) 0.1652(7) 0.0280(15) Uani 1 1 d . . . . .
H1 H 0.982670 0.557968 0.089325 0.034 Uiso 1 1 calc R U . . .
H2 H 1.200945 0.567276 0.185271 0.034 Uiso 1 1 calc R U . . .
N2 N 1.2036(10) 0.4991(3) 0.3667(7) 0.0302(15) Uani 1 1 d . . . . .
H3 H 1.321972 0.517003 0.385825 0.036 Uiso 1 1 calc R U . . .
H4 H 1.184949 0.473479 0.423358 0.036 Uiso 1 1 calc R U . . .
N3 N 0.8666(10) 0.4841(2) 0.2186(7) 0.0273(14) Uani 1 1 d . . . . .
H5 H 0.767993 0.492357 0.142730 0.033 Uiso 1 1 calc R U . . .
H6 H 0.845498 0.458422 0.274269 0.033 Uiso 1 1 calc R U . . .
N4 N 1.0129(10) 0.3048(2) 0.3511(7) 0.0271(15) Uani 1 1 d . . . . .
H7 H 1.091757 0.279578 0.329868 0.033 Uiso 1 1 calc R U . . .
N5 N 0.7811(10) 0.3509(3) 0.4419(8) 0.0286(15) Uani 1 1 d . . . . .
H8 H 0.674969 0.360972 0.493407 0.034 Uiso 1 1 calc R U . . .
N6 N 0.8916(9) 0.3805(2) 0.3504(7) 0.0253(14) Uani 1 1 d . . . . .
C1 C 1.0499(11) 0.5109(3) 0.2496(8) 0.0255(17) Uani 1 1 d . . . . .
C2 C 0.8544(13) 0.3048(3) 0.4433(10) 0.0296(18) Uani 1 1 d . . . . .
H9 H 0.804109 0.278132 0.498131 0.035 Uiso 1 1 calc R U . . .
C3 C 1.0315(12) 0.3507(3) 0.2956(9) 0.0280(17) Uani 1 1 d . . . . .
H10 H 1.132217 0.360013 0.226396 0.034 Uiso 1 1 calc R U . . .


_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 2.8613(10) . ?
Pb1 Br1 2.9444(11) . ?
Pb1 Br4 2.9841(11) . ?
Pb1 Br3 3.0480(10) . ?
Pb1 Br1 3.0809(12) 1_655 ?
Pb1 Br3 3.1723(11) 4_565 ?
N1 C1 1.303(9) . ?
N2 C1 1.326(9) . ?
N3 C1 1.318(9) . ?
N4 C2 1.306(11) . ?
N4 C3 1.337(10) . ?
N5 C2 1.318(10) . ?
N5 N6 1.347(8) . ?
N6 C3 1.289(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
Br2 Pb1 Br1 90.38(2) . . ?
Br2 Pb1 Br4 84.12(3) . . ?
Br1 Pb1 Br4 94.24(2) . . ?
Br2 Pb1 Br3 96.26(3) . . ?
Br1 Pb1 Br3 84.11(2) . . ?
Br4 Pb1 Br3 178.308(19) . . ?
Br2 Pb1 Br1 99.20(2) . 1_655 ?
Br1 Pb1 Br1 170.14(3) . 1_655 ?
Br4 Pb1 Br1 89.09(2) . 1_655 ?
Br3 Pb1 Br1 92.47(2) . 1_655 ?
Br2 Pb1 Br3 175.45(2) . 4_565 ?
Br1 Pb1 Br3 89.99(2) . 4_565 ?
Br4 Pb1 Br3 91.33(3) . 4_565 ?
Br3 Pb1 Br3 88.28(3) . 4_565 ?
Br1 Pb1 Br3 80.645(19) 1_655 4_565 ?
Pb1 Br1 Pb1 170.14(3) . 1_455 ?
Pb1 Br3 Pb1 169.58(3) . 4_566 ?
C2 N4 C3 108.2(6) . . ?
C2 N5 N6 112.2(6) . . ?
C3 N6 N5 103.3(6) . . ?
N1 C1 N3 119.9(7) . . ?
N1 C1 N2 119.0(7) . . ?
N3 C1 N2 121.1(7) . . ?
N4 C2 N5 105.1(7) . . ?
N6 C3 N4 111.2(7) . . ?

_refine_diff_density_max         2.040
_refine_diff_density_min         -1.416
_refine_diff_density_rms         0.241

####################################################################### 
# 
# 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_shelx_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1917735'
loop_
_audit_author_name
_audit_author_address
'Yuan-Yuan Guo'
;University of St Andrews
United Kingdom
;
_audit_update_record             
;
2019-05-21 deposited with the CCDC.	2019-07-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Br4 Pb, C2 H4 N3, C H6 N3'
_chemical_formula_sum            'C3 H10 Br4 N6 Pb'
_chemical_formula_weight         657.00

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 2/c'
_space_group_name_Hall           '-P 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, -y, -z'
'x, -y, z-1/2'

_cell_length_a                   6.0734(4)
_cell_length_b                   14.0000(9)
_cell_length_c                   8.5374(5)
_cell_angle_alpha                90
_cell_angle_beta                 94.866(8)
_cell_angle_gamma                90
_cell_volume                     723.30(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    935
_cell_measurement_theta_min      1.5
_cell_measurement_theta_max      27.5

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.017
_exptl_crystal_F_000             584
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.153
_exptl_crystal_size_mid          0.061
_exptl_crystal_size_min          0.044
_exptl_absorpt_coefficient_mu    22.690
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.484
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed Tube'
_diffrn_measurement_device_type  
;
Rigaku Mercury2 (2x2 bin mode)
;
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6554
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.668
_diffrn_reflns_theta_max         25.995
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             1428
_reflns_number_gt                1274
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0362P)²] 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         1428
_refine_ls_number_parameters     68
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0261
_refine_ls_wR_factor_ref         0.0624
_refine_ls_wR_factor_gt          0.0604
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_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_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 0.500000 0.66246(2) 0.250000 0.03458(12) Uani 1 2 d S T P . .
Br1 Br 0.000000 0.64636(6) 0.250000 0.0516(2) Uani 1 2 d S T P . .
Br2 Br 0.49934(12) 0.81608(5) 0.48079(9) 0.0657(2) Uani 1 1 d . . . . .
Br3 Br 0.500000 0.500000 0.000000 0.0639(3) Uani 1 2 d S . P . .
C1 C 0.000000 0.9794(7) 0.250000 0.076(3) Uani 1 2 d S T P . .
N1 N 0.000000 0.8901(6) 0.250000 0.097(4) Uani 1 2 d S T P . .
H1 H 0.114496 0.859383 0.288907 0.116 Uiso 0.5 1 calc R U P . .
H2 H -0.114496 0.859383 0.211093 0.116 Uiso 0.5 1 calc R U P . .
N2 N 0.1714(17) 1.0252(6) 0.3083(13) 0.153(4) Uani 1 1 d . . . . .
H3 H 0.285807 0.994440 0.347121 0.184 Uiso 1 1 calc R U . . .
H4 H 0.171645 1.086673 0.308327 0.184 Uiso 1 1 calc R U . . .
N3 N 0.000000 0.7525(6) 0.750000 0.077(3) Uani 1 2 d S T P . .
N4 N 0.0815(12) 0.6064(5) 0.7087(9) 0.077(2) Uani 0.5 1 d . . P . .
H5 H 0.148123 0.556796 0.676870 0.093 Uiso 0.5 1 calc R U P . .
C-N4 C 0.0815(12) 0.6064(5) 0.7087(9) 0.077(2) Uani 0.5 1 d . . P . .
H6 H 0.153549 0.552755 0.674276 0.093 Uiso 0.5 1 calc R U P . .
C2 C 0.1293(11) 0.6925(6) 0.6812(8) 0.0744(19) Uani 0.5 1 d . . P . .
H7 H 0.241484 0.711213 0.620135 0.089 Uiso 0.5 1 calc R U P . .
N-C2 N 0.1293(11) 0.6925(6) 0.6812(8) 0.0744(19) Uani 0.5 1 d . . P . .
H8 H 0.233038 0.709808 0.624731 0.089 Uiso 0.5 1 calc R U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br2 2.9170(7) . ?
Pb1 Br2 2.9170(7) 2_655 ?
Pb1 Br1 3.0451(2) . ?
Pb1 Br1 3.0451(2) 1_655 ?
Pb1 Br3 3.1191(2) . ?
Pb1 Br3 3.1191(2) 2_655 ?
C1 N1 1.251(12) . ?
C1 N2 1.286(8) . ?
C1 N2 1.286(8) 2 ?
N3 C2 1.321(8) 2_556 ?
N3 C2 1.321(8) . ?
N4 N4 1.262(14) 2_556 ?
N4 C2 1.267(10) . ?
C2 C2 2.039(13) 2_556 ?

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 Br2 85.00(3) . 2_655 ?
Br2 Pb1 Br1 89.774(19) . . ?
Br2 Pb1 Br1 96.494(19) 2_655 . ?
Br2 Pb1 Br1 96.493(19) . 1_655 ?
Br2 Pb1 Br1 89.774(19) 2_655 1_655 ?
Br1 Pb1 Br1 171.51(3) . 1_655 ?
Br2 Pb1 Br3 179.316(18) . . ?
Br2 Pb1 Br3 94.322(17) 2_655 . ?
Br1 Pb1 Br3 90.224(13) . . ?
Br1 Pb1 Br3 83.577(12) 1_655 . ?
Br2 Pb1 Br3 94.321(17) . 2_655 ?
Br2 Pb1 Br3 179.315(18) 2_655 2_655 ?
Br1 Pb1 Br3 83.577(12) . 2_655 ?
Br1 Pb1 Br3 90.224(13) 1_655 2_655 ?
Br3 Pb1 Br3 86.359(8) . 2_655 ?
Pb1 Br1 Pb1 171.51(3) 1_455 . ?
Pb1 Br3 Pb1 180.0 3_665 . ?
N1 C1 N2 119.9(6) . . ?
N1 C1 N2 119.9(6) . 2 ?
N2 C1 N2 120.2(11) . 2 ?
C2 N3 C2 101.0(8) 2_556 . ?
N4 N4 C2 107.8(4) 2_556 . ?
N4 C2 N3 111.6(6) . . ?
N4 C2 C2 72.1(4) . 2_556 ?
N3 C2 C2 39.5(4) . 2_556 ?

_refine_diff_density_max         0.711
_refine_diff_density_min         -1.790
_refine_diff_density_rms         0.271

####################################################################### 
# 
# 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_shelx_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 1917736'
loop_
_audit_author_name
_audit_author_address
'Yuan-Yuan Guo'
;University of St Andrews
United Kingdom
;
_audit_update_record             
;
2019-05-30 deposited with the CCDC.	2019-07-24 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT972_shelx               
;
PROBLEM: Check Calcd Resid. Dens.  0.87A   From Pb1            -3.75 eA-3
RESPONSE: Caused by the massive atom Pb.
;
_vrf_PLAT342_shelx               
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............       0.04 Ang.
RESPONSE: The disorder of imidazolium at room temperature.
;
_vrf_PLAT971_shelx               
;
PROBLEM: Check Calcd Resid. Dens.  1.12A   From Pb1             2.89 eA-3
RESPONSE: Caused by the massive atom Pb.
;
# Added during the CSD deposition process: Thursday 30 May 2019 11:16 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Br4 Pb, C3 H5 N2, C H6 N3'
_chemical_formula_sum            'C4 H11 Br4 N5 Pb'
_chemical_formula_weight         656.01

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

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   6.1106(4)
_cell_length_b                   9.2753(5)
_cell_length_c                   13.0429(9)
_cell_angle_alpha                93.474(9)
_cell_angle_beta                 92.726(9)
_cell_angle_gamma                91.258(8)
_cell_volume                     736.82(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    851
_cell_measurement_theta_min      2.6
_cell_measurement_theta_max      27.5

_exptl_crystal_description       Platelet
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.957
_exptl_crystal_F_000             584
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.191
_exptl_crystal_size_mid          0.122
_exptl_crystal_size_min          0.073
_exptl_absorpt_coefficient_mu    22.272
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.461
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed Tube'
_diffrn_measurement_device_type  
;
Rigaku Mercury2 (2x2 bin mode)
;
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6253
_diffrn_reflns_av_unetI/netI     0.0920
_diffrn_reflns_av_R_equivalents  0.0831
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.779
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             2580
_reflns_number_gt                1857
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0589P)²] 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         2580
_refine_ls_number_parameters     140
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0518
_refine_ls_wR_factor_ref         0.1224
_refine_ls_wR_factor_gt          0.1197
_refine_ls_goodness_of_fit_ref   0.926
_refine_ls_restrained_S_all      0.931
_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 0.48974(7) 0.26367(5) 0.16235(4) 0.03507(19) Uani 1 1 d . . . . .
Br1 Br 0.5104(3) 0.49288(17) 0.32790(13) 0.0564(4) Uani 1 1 d . . . . .
Br2 Br 0.500000 0.000000 0.000000 0.0536(6) Uani 1 2 d S . P . .
Br3 Br 0.9862(2) 0.26693(17) 0.15938(14) 0.0541(4) Uani 1 1 d . . . . .
Br4 Br 0.5037(3) 0.05380(18) 0.31944(14) 0.0592(4) Uani 1 1 d . . . . .
Br5 Br 0.500000 0.500000 0.000000 0.0550(6) Uani 1 2 d S . P . .
N4 N 0.129(3) 0.218(2) 0.4644(18) 0.104(7) Uani 1 1 d . . . . .
H7 H 0.241240 0.195517 0.430006 0.125 Uiso 1 1 calc R U . . .
N5 N -0.153(3) 0.321(2) 0.5018(18) 0.109(7) Uani 1 1 d . . . . .
H8 H -0.260796 0.379197 0.500670 0.131 Uiso 1 1 calc R U . . .
C2 C -0.025(4) 0.307(3) 0.4360(18) 0.092(7) Uani 1 1 d . . . . .
H9 H -0.033193 0.351334 0.373935 0.111 Uiso 1 1 calc R U . . .
C3 C 0.084(5) 0.170(3) 0.554(2) 0.117(10) Uani 1 1 d . . . . .
H10 H 0.162825 0.106282 0.592091 0.141 Uiso 1 1 calc R U . . .
C4 C -0.105(4) 0.236(3) 0.5770(17) 0.095(7) Uani 1 1 d . . . . .
H11 H -0.184780 0.223732 0.634826 0.114 Uiso 1 1 calc R U . . .
C1 C 0.045(5) 0.236(3) 0.855(2) 0.158(16) Uani 0.7 1 d D . P A 1
N1 N 0.228(3) 0.236(2) 0.8122(17) 0.068(6) Uani 0.7 1 d D . P A 1
H1 H 0.282196 0.315033 0.791688 0.081 Uiso 0.7 1 calc R U P A 1
H2 H 0.297993 0.156896 0.803846 0.081 Uiso 0.7 1 calc R U P A 1
N2 N -0.058(3) 0.350(2) 0.8676(17) 0.063(6) Uani 0.7 1 d D . P A 1
H3 H -0.188374 0.347303 0.889494 0.075 Uiso 0.7 1 calc R U P A 1
H4 H 0.001666 0.431228 0.854349 0.075 Uiso 0.7 1 calc R U P A 1
N3 N -0.040(3) 0.117(2) 0.8740(19) 0.076(7) Uani 0.7 1 d D . P A 1
H5 H -0.170599 0.113115 0.895967 0.091 Uiso 0.7 1 calc R U P A 1
H6 H 0.031789 0.038688 0.865143 0.091 Uiso 0.7 1 calc R U P A 1
C1' C 0.045(5) 0.236(3) 0.855(2) 0.158(16) Uani 0.3 1 d D . P B 2
N1' N 0.099(10) 0.368(5) 0.822(5) 0.115(13) Uiso 0.3 1 d D . P B 2
H1' H 0.199070 0.376255 0.778932 0.138 Uiso 0.3 1 calc R U P B 2
H2' H 0.032806 0.443301 0.845492 0.138 Uiso 0.3 1 calc R U P B 2
N2' N -0.178(7) 0.220(7) 0.882(5) 0.115(13) Uiso 0.3 1 d D . P B 2
H3' H -0.241075 0.136216 0.876864 0.138 Uiso 0.3 1 calc R U P B 2
H4' H -0.248280 0.294667 0.902566 0.138 Uiso 0.3 1 calc R U P B 2
N3' N 0.138(9) 0.114(5) 0.824(5) 0.115(13) Uiso 0.3 1 d D . P B 2
H5' H 0.239248 0.115664 0.780218 0.138 Uiso 0.3 1 calc R U P B 2
H6' H 0.096997 0.033603 0.847075 0.138 Uiso 0.3 1 calc R U P B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br4 2.9101(18) . ?
Pb1 Br1 2.9332(16) . ?
Pb1 Br3 3.0355(14) . ?
Pb1 Br3 3.0759(14) 1_455 ?
Pb1 Br2 3.1402(6) . ?
Pb1 Br5 3.1404(6) . ?
N4 C3 1.31(3) . ?
N4 C2 1.32(3) . ?
N5 C2 1.19(3) . ?
N5 C4 1.32(3) . ?
C3 C4 1.35(3) . ?
C1 N2 1.25(3) . ?
C1 N3 1.26(3) . ?
C1 N1 1.27(3) . ?
C1' N3' 1.33(4) . ?
C1' N1' 1.36(4) . ?
C1' N2' 1.43(4) . ?

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
Br4 Pb1 Br1 88.21(5) . . ?
Br4 Pb1 Br3 90.35(5) . . ?
Br1 Pb1 Br3 90.57(5) . . ?
Br4 Pb1 Br3 91.54(5) . 1_455 ?
Br1 Pb1 Br3 89.66(5) . 1_455 ?
Br3 Pb1 Br3 178.10(7) . 1_455 ?
Br4 Pb1 Br2 86.92(4) . . ?
Br1 Pb1 Br2 174.02(4) . . ?
Br3 Pb1 Br2 86.00(3) . . ?
Br3 Pb1 Br2 93.93(3) 1_455 . ?
Br4 Pb1 Br5 176.44(4) . . ?
Br1 Pb1 Br5 89.51(4) . . ?
Br3 Pb1 Br5 86.95(4) . . ?
Br3 Pb1 Br5 91.17(4) 1_455 . ?
Br2 Pb1 Br5 95.193(16) . . ?
Pb1 Br2 Pb1 180.0 . 2_655 ?
Pb1 Br3 Pb1 178.10(7) . 1_655 ?
Pb1 Br5 Pb1 180.0 2_665 . ?
C3 N4 C2 108.9(19) . . ?
C2 N5 C4 110(2) . . ?
N5 C2 N4 110(2) . . ?
N4 C3 C4 104.0(18) . . ?
N5 C4 C3 107(2) . . ?
N2 C1 N3 121(3) . . ?
N2 C1 N1 121(3) . . ?
N3 C1 N1 118(3) . . ?
N3' C1' N1' 124(4) . . ?
N3' C1' N2' 115(3) . . ?
N1' C1' N2' 114(3) . . ?

_refine_diff_density_max         2.833
_refine_diff_density_min         -3.571
_refine_diff_density_rms         0.313

