# Supplementary Information (SI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2025

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

data_1
_database_code_depnum_ccdc_archive 'CCDC 2390413'
loop_
_audit_author_name
_audit_author_address
'Yang Zhu'
;southeast university
China
;
_audit_update_record             
;
2024-10-12 deposited with the CCDC.	2025-03-18 downloaded from the CCDC.
;
_audit_creation_date             2022-09-19
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Cl3 Pb, C6 H14 N'
_chemical_formula_sum            'C6 H14 Cl3 N Pb'
_chemical_formula_weight         413.72
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           169
_space_group_name_H-M_alt        'P 61'
_space_group_name_Hall           'P 61'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'-x, -y, z+1/2'
'y, -x+y, z+5/6'
'x-y, x, z+1/6'

_cell_length_a                   9.3571(10)
_cell_length_b                   9.3571(10)
_cell_length_c                   22.408(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1699.1(5)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    3907
_cell_measurement_temperature    245.0
_cell_measurement_theta_max      27.17
_cell_measurement_theta_min      2.67
_shelx_estimated_absorpt_T_max   0.305
_shelx_estimated_absorpt_T_min   0.305
_exptl_absorpt_coefficient_mu    15.548
_exptl_absorpt_correction_T_max  0.0289
_exptl_absorpt_correction_T_min  0.0099
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0680 before and 0.0383 after correction.
The Ratio of minimum to maximum transmission is 0.3426.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.426
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1140
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            8695
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.535
_diffrn_reflns_theta_min         2.673
_diffrn_ambient_temperature      245.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.817
_reflns_Friedel_fraction_full    0.920
_reflns_Friedel_fraction_max     0.858
_reflns_number_gt                2156
_reflns_number_total             2420
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.689
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.112
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.509(17)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     103
_refine_ls_number_reflns         2420
_refine_ls_number_restraints     66
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0262
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0203P)²+2.0661P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0532
_refine_ls_wR_factor_ref         0.0568
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.491(17)
 0.509(17)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B)
5.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 1.98832(11) 1.04701(8) 0.67430(8) 0.04377(12) Uani 1 1 d . U . . .
Cl1 Cl 2.1953(4) 0.9680(3) 0.60430(12) 0.0509(7) Uani 1 1 d . U . . .
Cl2 Cl 1.7530(4) 0.8909(3) 0.57876(13) 0.0532(8) Uani 1 1 d . U . . .
Cl3 Cl 1.7887(4) 1.1155(5) 0.75831(16) 0.0545(7) Uani 1 1 d . U . . .
N1 N 1.7168(12) 0.3963(10) 0.5739(4) 0.049(2) Uani 1 1 d . U . . .
C1 C 1.5764(16) 0.4289(17) 0.5772(6) 0.061(3) Uani 1 1 d . U . . .
H1A H 1.480318 0.344340 0.555427 0.074 Uiso 1 1 calc R U . . .
H1B H 1.607600 0.537412 0.560387 0.074 Uiso 1 1 calc R U . . .
C2 C 1.5397(16) 0.4233(17) 0.6426(6) 0.065(3) Uani 1 1 d . U . . .
H2A H 1.421105 0.376454 0.649339 0.078 Uiso 1 1 calc R U . . .
H2B H 1.598463 0.534175 0.660001 0.078 Uiso 1 1 calc R U . . .
C3 C 1.5994(15) 0.3141(15) 0.6698(8) 0.065(3) Uani 1 1 d . U . . .
H3A H 1.683995 0.374771 0.700078 0.078 Uiso 1 1 calc R U . . .
H3B H 1.507587 0.216787 0.688485 0.078 Uiso 1 1 calc R U . . .
C4 C 1.6704(16) 0.2637(15) 0.6186(6) 0.062(3) Uani 1 1 d . U . . .
H4A H 1.767134 0.257420 0.631535 0.074 Uiso 1 1 calc R U . . .
H4B H 1.588033 0.156459 0.602370 0.074 Uiso 1 1 calc R U . . .
C5 C 1.8742(15) 0.5484(13) 0.5918(6) 0.054(3) Uani 1 1 d . U . . .
H5A H 1.907624 0.630778 0.560583 0.081 Uiso 1 1 calc R U . . .
H5B H 1.960000 0.520439 0.597838 0.081 Uiso 1 1 calc R U . . .
H5C H 1.856524 0.592002 0.628589 0.081 Uiso 1 1 calc R U . . .
C6 C 1.7398(19) 0.3444(17) 0.5129(8) 0.080(4) Uani 1 1 d . U . . .
H6A H 1.765608 0.432596 0.484630 0.120 Uiso 1 1 calc R U . . .
H6B H 1.639004 0.246203 0.500716 0.120 Uiso 1 1 calc R U . . .
H6C H 1.829568 0.320738 0.513857 0.120 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 Cl1 2.862(3) . ?
Pb1 Cl1 2.918(3) 6_645 ?
Pb1 Cl2 2.873(4) 6_645 ?
Pb1 Cl2 2.890(4) . ?
Pb1 Cl3 2.930(3) 5_674 ?
Pb1 Cl3 2.940(3) . ?
N1 C1 1.492(15) . ?
N1 C4 1.481(15) . ?
N1 C5 1.503(14) . ?
N1 C6 1.502(18) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 C2 1.501(18) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 C3 1.515(18) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 C4 1.514(19) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 H5C 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 H6C 0.9700 . ?

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
Cl1 Pb1 Cl1 94.19(7) . 6_645 ?
Cl1 Pb1 Cl2 84.63(9) . . ?
Cl1 Pb1 Cl2 93.67(8) . 6_645 ?
Cl1 Pb1 Cl3 99.90(11) 6_645 5_674 ?
Cl1 Pb1 Cl3 173.34(10) . . ?
Cl1 Pb1 Cl3 81.91(10) . 5_674 ?
Cl1 Pb1 Cl3 80.82(9) 6_645 . ?
Cl2 Pb1 Cl1 178.14(8) . 6_645 ?
Cl2 Pb1 Cl1 83.91(10) 6_645 6_645 ?
Cl2 Pb1 Cl2 94.73(7) 6_645 . ?
Cl2 Pb1 Cl3 100.25(11) . . ?
Cl2 Pb1 Cl3 81.36(10) . 5_674 ?
Cl2 Pb1 Cl3 174.33(11) 6_645 5_674 ?
Cl2 Pb1 Cl3 81.47(11) 6_645 . ?
Cl3 Pb1 Cl3 103.20(5) 5_674 . ?
Pb1 Cl1 Pb1 81.38(9) . 5_674 ?
Pb1 Cl2 Pb1 81.68(9) 5_674 . ?
Pb1 Cl3 Pb1 79.88(6) 6_645 . ?
C1 N1 C5 109.8(9) . . ?
C1 N1 C6 113.2(11) . . ?
C4 N1 C1 102.6(10) . . ?
C4 N1 C5 110.5(10) . . ?
C4 N1 C6 112.0(10) . . ?
C6 N1 C5 108.6(10) . . ?
N1 C1 H1A 110.9 . . ?
N1 C1 H1B 110.9 . . ?
N1 C1 C2 104.5(10) . . ?
H1A C1 H1B 108.9 . . ?
C2 C1 H1A 110.9 . . ?
C2 C1 H1B 110.9 . . ?
C1 C2 H2A 110.7 . . ?
C1 C2 H2B 110.7 . . ?
C1 C2 C3 105.2(11) . . ?
H2A C2 H2B 108.8 . . ?
C3 C2 H2A 110.7 . . ?
C3 C2 H2B 110.7 . . ?
C2 C3 H3A 110.6 . . ?
C2 C3 H3B 110.6 . . ?
H3A C3 H3B 108.7 . . ?
C4 C3 C2 105.8(12) . . ?
C4 C3 H3A 110.6 . . ?
C4 C3 H3B 110.6 . . ?
N1 C4 C3 104.0(10) . . ?
N1 C4 H4A 110.9 . . ?
N1 C4 H4B 110.9 . . ?
C3 C4 H4A 110.9 . . ?
C3 C4 H4B 110.9 . . ?
H4A C4 H4B 109.0 . . ?
N1 C5 H5A 109.5 . . ?
N1 C5 H5B 109.5 . . ?
N1 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N1 C6 H6A 109.5 . . ?
N1 C6 H6B 109.5 . . ?
N1 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 -25.6(13) . . . . ?
C1 N1 C4 C3 -40.2(12) . . . . ?
C1 C2 C3 C4 0.8(14) . . . . ?
C2 C3 C4 N1 24.4(13) . . . . ?
C4 N1 C1 C2 41.1(12) . . . . ?
C5 N1 C1 C2 -76.4(13) . . . . ?
C5 N1 C4 C3 76.8(12) . . . . ?
C6 N1 C1 C2 162.0(11) . . . . ?
C6 N1 C4 C3 -162.0(12) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.491(17)
2 0.509(17)

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

data_3
_database_code_depnum_ccdc_archive 'CCDC 2390414'
loop_
_audit_author_name
_audit_author_address
'Yang Zhu'
;southeast university
China
;
_audit_update_record             
;
2024-10-12 deposited with the CCDC.	2025-03-18 downloaded from the CCDC.
;
_audit_creation_date             2024-10-12
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Cl3 Pb1, 2(C3 N0.5)'
_chemical_formula_sum            'C6 Cl3 N Pb'
_chemical_formula_weight         399.61
_chemical_absolute_configuration ?
_chemical_melting_point          ?
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           186
_space_group_name_H-M_alt        'P 63 m c'
_space_group_name_Hall           'P 6c -2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'y, x, z+1/2'
'x-y, -y, z+1/2'
'-x, -x+y, z+1/2'

_cell_length_a                   9.4432(4)
_cell_length_b                   9.4432(4)
_cell_length_c                   7.6506(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     590.83(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1389
_cell_measurement_temperature    323(2)
_cell_measurement_theta_max      25.14
_cell_measurement_theta_min      3.65
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    14.902
_exptl_absorpt_correction_T_max  0.0468
_exptl_absorpt_correction_T_min  0.0208
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0735 before and 0.0388 after correction.
The Ratio of minimum to maximum transmission is 0.4444.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.246
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             352
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_unetI/netI     0.0135
_diffrn_reflns_Laue_measured_fraction_full 0.962
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            3654
_diffrn_reflns_point_group_measured_fraction_full 0.924
_diffrn_reflns_point_group_measured_fraction_max 0.917
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.972
_diffrn_reflns_theta_min         5.330
_diffrn_ambient_temperature      323.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.758
_reflns_Friedel_fraction_full    0.879
_reflns_Friedel_fraction_max     0.860
_reflns_number_gt                311
_reflns_number_total             429
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.468
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.51(19)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     32
_refine_ls_number_reflns         429
_refine_ls_number_restraints     49
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0299
_refine_ls_restrained_S_all      1.023
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0459P)²+0.7933P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0830
_refine_ls_wR_factor_ref         0.0916
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.49(19)
 0.51(19)
2. Restrained distances
 C1-C2
 1.6 with sigma of 0.01
 C2-C3
 1.5 with sigma of 0.01
 C3-N1
 1.7 with sigma of 0.01
 C2-N1
 1.4 with sigma of 0.01
 C1-N1
 2.2 with sigma of 0.01
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(N1) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.1 and sigma
for terminal atoms of 0.2
5. Others
 Fixed Sof: C1(0.33334) C2(0.33334) C3(0.33334)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 1.000000 0.000000 1.099(6) 0.0963(5) Uani 1 6 d S TU P . .
Cl1 Cl 0.8662(2) 0.1338(2) 0.861(5) 0.1453(19) Uani 1 2 d S TU P . .
N1 N 0.333333 0.666667 0.884(2) 0.233(10) Uani 1 6 d DS TU P . .
C1 C 0.322(4) 0.644(9) 0.598(3) 0.258(14) Uani 0.6667 2 d DS TU P . .
C2 C 0.391(2) 0.781(4) 0.747(2) 0.251(14) Uani 0.6667 2 d DS TU P . .
C3 C 0.4354(10) 0.871(2) 0.919(5) 0.244(14) Uani 0.6667 2 d DS TU 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 Cl1 2.85(2) . ?
Pb1 Cl1 2.97(2) 6_545 ?
Pb1 Cl1 2.97(2) 5_665 ?
Pb1 Cl1 2.85(2) 2_645 ?
Pb1 Cl1 2.85(2) 3_765 ?
Pb1 Cl1 2.97(2) 4_755 ?
N1 C2 1.406(14) 2_665 ?
N1 C2 1.406(14) . ?
N1 C2 1.406(14) 3_565 ?
N1 C3 1.689(14) . ?
N1 C3 1.689(14) 3_565 ?
N1 C3 1.689(14) 2_665 ?
C1 C1 0.32(12) 3_565 ?
C1 C1 0.32(12) 2_665 ?
C1 C2 1.43(6) 2_665 ?
C1 C2 1.604(14) . ?
C1 C2 1.43(6) 3_565 ?
C2 C2 1.63(6) 3_565 ?
C2 C2 1.63(6) 2_665 ?
C2 C3 1.500(14) . ?

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
Cl1 Pb1 Cl1 83.5(8) . 2_645 ?
Cl1 Pb1 Cl1 177.2(10) 3_765 6_545 ?
Cl1 Pb1 Cl1 98.55(9) 3_765 4_755 ?
Cl1 Pb1 Cl1 83.5(8) . 3_765 ?
Cl1 Pb1 Cl1 177.2(10) . 4_755 ?
Cl1 Pb1 Cl1 83.5(8) 2_645 3_765 ?
Cl1 Pb1 Cl1 79.3(7) 6_545 4_755 ?
Cl1 Pb1 Cl1 98.55(9) . 5_665 ?
Cl1 Pb1 Cl1 79.3(7) 5_665 6_545 ?
Cl1 Pb1 Cl1 177.2(10) 2_645 5_665 ?
Cl1 Pb1 Cl1 98.55(9) 2_645 4_755 ?
Cl1 Pb1 Cl1 98.55(9) 3_765 5_665 ?
Cl1 Pb1 Cl1 79.3(7) 5_665 4_755 ?
Cl1 Pb1 Cl1 98.55(9) . 6_545 ?
Cl1 Pb1 Cl1 98.55(9) 2_645 6_545 ?
Pb1 Cl1 Pb1 82.26(11) . 4_754 ?
C2 N1 C2 71(3) 2_665 . ?
C2 N1 C2 71(3) 2_665 3_565 ?
C2 N1 C2 71(3) . 3_565 ?
C2 N1 C3 116.5(18) 2_665 . ?
C2 N1 C3 57.1(7) 3_565 3_565 ?
C2 N1 C3 116.5(18) 2_665 3_565 ?
C2 N1 C3 116.5(18) 3_565 . ?
C2 N1 C3 57.1(7) 2_665 2_665 ?
C2 N1 C3 116.5(18) . 3_565 ?
C2 N1 C3 116.5(18) . 2_665 ?
C2 N1 C3 116.5(18) 3_565 2_665 ?
C2 N1 C3 57.1(7) . . ?
C3 N1 C3 117.6(9) . 3_565 ?
C3 N1 C3 117.6(9) 2_665 . ?
C3 N1 C3 117.6(9) 2_665 3_565 ?
C1 C1 C1 60.00(8) 3_565 2_665 ?
C1 C1 C2 83(3) 3_565 2_665 ?
C1 C1 C2 52.5(16) 2_665 . ?
C1 C1 C2 83(3) 2_665 3_565 ?
C1 C1 C2 117(3) 2_665 2_665 ?
C1 C1 C2 117(3) 3_565 3_565 ?
C1 C1 C2 52.5(16) 3_565 . ?
C2 C1 C2 69.3(14) 2_665 3_565 ?
C2 C1 C2 64.5(16) 2_665 . ?
C2 C1 C2 64.5(16) 3_565 . ?
N1 C2 C1 102(3) . 3_565 ?
N1 C2 C1 102(3) . 2_665 ?
N1 C2 C1 93.5(11) . . ?
N1 C2 C2 54.7(14) . 3_565 ?
N1 C2 C2 54.7(14) . 2_665 ?
N1 C2 C3 71.0(9) . . ?
C1 C2 C1 10(4) 3_565 . ?
C1 C2 C1 10(4) 2_665 . ?
C1 C2 C1 13(5) 3_565 2_665 ?
C1 C2 C2 52.5(16) . 2_665 ?
C1 C2 C2 52.5(15) . 3_565 ?
C1 C2 C2 55.3(7) 2_665 3_565 ?
C1 C2 C2 55.3(7) 3_565 2_665 ?
C1 C2 C2 63(3) 3_565 3_565 ?
C1 C2 C2 63(3) 2_665 2_665 ?
C1 C2 C3 170.2(12) 3_565 . ?
C1 C2 C3 170.2(12) 2_665 . ?
C2 C2 C2 60.000(4) 2_665 3_565 ?
C3 C2 C1 164.5(16) . . ?
C3 C2 C2 114.9(15) . 2_665 ?
C3 C2 C2 114.9(15) . 3_565 ?
C2 C3 N1 51.9(7) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C1 C2 N1 141.0(9) 3_565 . . . ?
C1 C1 C2 N1 -141.0(11) 2_665 . . . ?
C1 C1 C2 C1 -78.1(19) 3_565 . . 2_665 ?
C1 C1 C2 C1 78(2) 2_665 . . 3_565 ?
C1 C1 C2 C2 102(2) 3_565 . . 2_665 ?
C1 C1 C2 C2 180.00(11) 2_665 . . 2_665 ?
C1 C1 C2 C2 -102(2) 2_665 . . 3_565 ?
C1 C1 C2 C2 180.00(9) 3_565 . . 3_565 ?
C1 C1 C2 C3 141.0(9) 3_565 . . . ?
C1 C1 C2 C3 -141.0(10) 2_665 . . . ?
C1 C2 C3 N1 0.00(5) . . . . ?
C2 N1 C2 C1 31(4) 3_565 . . 2_665 ?
C2 N1 C2 C1 -31(4) 2_665 . . 3_565 ?
C2 N1 C2 C1 -37.8(8) 2_665 . . . ?
C2 N1 C2 C1 -44(2) 2_665 . . 2_665 ?
C2 N1 C2 C1 37.8(8) 3_565 . . . ?
C2 N1 C2 C1 44(2) 3_565 . . 3_565 ?
C2 N1 C2 C2 75.6(16) 3_565 . . 2_665 ?
C2 N1 C2 C2 -75.6(16) 2_665 . . 3_565 ?
C2 N1 C2 C3 142.2(8) 2_665 . . . ?
C2 N1 C2 C3 -142.2(8) 3_565 . . . ?
C2 N1 C3 C2 -40(2) 2_665 . . . ?
C2 N1 C3 C2 40(2) 3_565 . . . ?
C2 C1 C2 N1 39.0(10) 2_665 . . . ?
C2 C1 C2 N1 -39.0(10) 3_565 . . . ?
C2 C1 C2 C1 102(2) 3_565 . . 2_665 ?
C2 C1 C2 C1 180.00(6) 2_665 . . 2_665 ?
C2 C1 C2 C1 180.00(17) 3_565 . . 3_565 ?
C2 C1 C2 C1 -102(2) 2_665 . . 3_565 ?
C2 C1 C2 C2 78.1(19) 2_665 . . 3_565 ?
C2 C1 C2 C2 -78(2) 3_565 . . 2_665 ?
C2 C1 C2 C3 -39.0(10) 3_565 . . . ?
C2 C1 C2 C3 39.0(10) 2_665 . . . ?
C2 C2 C3 N1 -33.5(5) 3_565 . . . ?
C2 C2 C3 N1 33.5(5) 2_665 . . . ?
C3 N1 C2 C1 -66(5) 2_665 . . 3_565 ?
C3 N1 C2 C1 79.6(13) 3_565 . . 3_565 ?
C3 N1 C2 C1 180.000(6) . . . . ?
C3 N1 C2 C1 73(2) 3_565 . . . ?
C3 N1 C2 C1 66(5) 3_565 . . 2_665 ?
C3 N1 C2 C1 -79.6(13) 2_665 . . 2_665 ?
C3 N1 C2 C1 173(3) . . . 2_665 ?
C3 N1 C2 C1 -73(2) 2_665 . . . ?
C3 N1 C2 C1 -173(3) . . . 3_565 ?
C3 N1 C2 C2 -142.2(8) . . . 2_665 ?
C3 N1 C2 C2 111(3) 3_565 . . 2_665 ?
C3 N1 C2 C2 142.2(8) . . . 3_565 ?
C3 N1 C2 C2 -35.1(13) 2_665 . . 2_665 ?
C3 N1 C2 C2 -111(3) 2_665 . . 3_565 ?
C3 N1 C2 C2 35.1(13) 3_565 . . 3_565 ?
C3 N1 C2 C3 -107(2) 3_565 . . . ?
C3 N1 C2 C3 107(2) 2_665 . . . ?
C3 N1 C3 C2 -105(3) 2_665 . . . ?
C3 N1 C3 C2 105(3) 3_565 . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.49(19)
2 0.51(19)

####################################################################### 
# 
# 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_6
_database_code_depnum_ccdc_archive 'CCDC 2390417'
loop_
_audit_author_name
_audit_author_address
'Yang Zhu'
;southeast university
China
;
_audit_update_record             
;
2024-10-12 deposited with the CCDC.	2025-03-18 downloaded from the CCDC.
;
_audit_creation_date             2023-05-27
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br3 Pb1, 2(C3 N0.5)'
_chemical_formula_sum            'C6 Br3 N Pb'
_chemical_formula_weight         532.99
_chemical_absolute_configuration ?
_chemical_melting_point          ?
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'
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'

_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.
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           186
_space_group_name_H-M_alt        'P 63 m c'
_space_group_name_Hall           'P 6c -2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'y, x, z+1/2'
'x-y, -y, z+1/2'
'-x, -x+y, z+1/2'

_cell_length_a                   9.7180(6)
_cell_length_b                   9.7180(6)
_cell_length_c                   7.7965(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     637.65(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    846
_cell_measurement_temperature    323(2)
_cell_measurement_theta_max      25.3440
_cell_measurement_theta_min      2.4210
_shelx_estimated_absorpt_T_max   0.211
_shelx_estimated_absorpt_T_min   0.211
_exptl_absorpt_coefficient_mu    22.579
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.776
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             460
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0556
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            2411
_diffrn_reflns_point_group_measured_fraction_full 0.926
_diffrn_reflns_point_group_measured_fraction_max 0.911
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.984
_diffrn_reflns_theta_min         2.420
_diffrn_ambient_temperature      323.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.703
_reflns_Friedel_fraction_full    0.849
_reflns_Friedel_fraction_max     0.817
_reflns_number_gt                329
_reflns_number_total             453
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.501
_refine_diff_density_min         -0.656
_refine_diff_density_rms         0.118
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.5(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     32
_refine_ls_number_reflns         453
_refine_ls_number_restraints     49
_refine_ls_R_factor_all          0.0802
_refine_ls_R_factor_gt           0.0546
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0602P)²+3.0756P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1266
_refine_ls_wR_factor_ref         0.1363
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.5(3)
 0.5(3)
2. Restrained distances
 C1-C2
 1.6 with sigma of 0.01
 C2-C3
 1.5 with sigma of 0.01
 C3-N1
 1.7 with sigma of 0.01
 C2-N1
 1.4 with sigma of 0.01
 C1-N1
 2.2 with sigma of 0.01
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(N1) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.1 and sigma
for terminal atoms of 0.2
5. Others
 Fixed Sof: C1(0.33334) C2(0.33334) C3(0.33334)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 1.000000 0.000000 1.056(6) 0.0785(8) Uani 1 6 d S TU P . .
Br1 Br 0.86199(18) 0.13801(18) 0.809(6) 0.1221(15) Uani 1 2 d S TU P . .
N1 N 0.333333 0.666667 0.851(4) 0.173(12) Uani 1 6 d DS TU P . .
C1 C 0.368(5) 0.736(10) 0.5789(19) 0.184(16) Uani 0.6667 2 d DS TU P . .
C2 C 0.4069(18) 0.814(4) 0.767(3) 0.186(14) Uani 0.6667 2 d DS TU P . .
C3 C 0.422(2) 0.843(4) 0.956(4) 0.183(15) Uani 0.6667 2 d DS TU 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 Br1 3.018(14) 2_645 ?
Pb1 Br1 3.047(16) 6_545 ?
Pb1 Br1 3.047(16) 4_755 ?
Pb1 Br1 3.018(14) 3_765 ?
Pb1 Br1 3.018(14) . ?
Pb1 Br1 3.047(16) 5_665 ?
N1 C2 1.402(14) 2_665 ?
N1 C2 1.402(14) 3_565 ?
N1 C2 1.402(14) . ?
N1 C3 1.700(14) . ?
N1 C3 1.700(14) 3_565 ?
N1 C3 1.700(14) 2_665 ?
C1 C1 1.02(15) 2_665 ?
C1 C1 1.02(14) 3_565 ?
C1 C2 1.602(14) . ?
C2 C3 1.501(14) . ?

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 83.6(5) 2_645 3_765 ?
Br1 Pb1 Br1 82.6(5) 5_665 4_755 ?
Br1 Pb1 Br1 82.6(5) 5_665 6_545 ?
Br1 Pb1 Br1 83.6(5) 2_645 . ?
Br1 Pb1 Br1 179.3(7) 3_765 6_545 ?
Br1 Pb1 Br1 83.6(5) 3_765 . ?
Br1 Pb1 Br1 96.87(6) 3_765 4_755 ?
Br1 Pb1 Br1 179.3(7) 2_645 5_665 ?
Br1 Pb1 Br1 96.87(6) 2_645 6_545 ?
Br1 Pb1 Br1 96.87(6) 3_765 5_665 ?
Br1 Pb1 Br1 96.87(6) . 6_545 ?
Br1 Pb1 Br1 96.87(6) . 5_665 ?
Br1 Pb1 Br1 82.6(5) 4_755 6_545 ?
Br1 Pb1 Br1 96.87(6) 2_645 4_755 ?
Br1 Pb1 Br1 179.3(7) . 4_755 ?
Pb1 Br1 Pb1 79.99(8) . 4_754 ?
C2 N1 C2 100(3) 2_665 3_565 ?
C2 N1 C2 100(3) 2_665 . ?
C2 N1 C2 100(3) . 3_565 ?
C2 N1 C3 127.8(2) 2_665 . ?
C2 N1 C3 127.8(2) . 2_665 ?
C2 N1 C3 127.8(2) 2_665 3_565 ?
C2 N1 C3 56.9(7) . . ?
C2 N1 C3 127.8(2) 3_565 2_665 ?
C2 N1 C3 127.8(2) 3_565 . ?
C2 N1 C3 127.8(2) . 3_565 ?
C2 N1 C3 56.9(7) 2_665 2_665 ?
C2 N1 C3 56.9(7) 3_565 3_565 ?
C3 N1 C3 99(3) . 3_565 ?
C3 N1 C3 99(3) . 2_665 ?
C3 N1 C3 99(3) 2_665 3_565 ?
C1 C1 C1 60.000(15) 3_565 2_665 ?
C1 C1 C2 111(2) 2_665 . ?
C1 C1 C2 111(2) 3_565 . ?
N1 C2 C1 93.9(11) . . ?
N1 C2 C3 71.6(9) . . ?
C3 C2 C1 165.5(16) . . ?
C2 C3 N1 51.5(7) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C1 C2 N1 -32.3(5) 3_565 . . . ?
C1 C1 C2 N1 32.3(5) 2_665 . . . ?
C1 C1 C2 C3 -32.3(6) 3_565 . . . ?
C1 C1 C2 C3 32.3(4) 2_665 . . . ?
C1 C2 C3 N1 0.01(5) . . . . ?
C2 N1 C2 C1 -51(2) 2_665 . . . ?
C2 N1 C2 C1 51(2) 3_565 . . . ?
C2 N1 C2 C3 129(2) 2_665 . . . ?
C2 N1 C2 C3 -129(2) 3_565 . . . ?
C2 N1 C3 C2 -76(5) 2_665 . . . ?
C2 N1 C3 C2 76(5) 3_565 . . . ?
C3 N1 C2 C1 180.002(6) . . . . ?
C3 N1 C2 C1 106(5) 3_565 . . . ?
C3 N1 C2 C1 -106(5) 2_665 . . . ?
C3 N1 C2 C3 74(5) 2_665 . . . ?
C3 N1 C2 C3 -74(5) 3_565 . . . ?
C3 N1 C3 C2 -130(2) 2_665 . . . ?
C3 N1 C3 C2 130(2) 3_565 . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.5(3)
2 0.5(3)

####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 2390416'
loop_
_audit_author_name
_audit_author_address
'Yang Zhu'
;southeast university
China
;
_audit_update_record             
;
2025-02-20 deposited with the CCDC.	2025-03-18 downloaded from the CCDC.
;
_audit_creation_date             2023-11-25
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '3(Br3 Pb1), 3(C6 H14 N)'
_chemical_formula_sum            'C18 H42 Br9 N3 Pb3'
_chemical_formula_weight         1641.30
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           173
_space_group_name_H-M_alt        'P 63'
_space_group_name_Hall           'P 6c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'

_cell_length_a                   16.7130(7)
_cell_length_b                   16.7130(7)
_cell_length_c                   7.7768(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1881.2(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2571
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      29.558
_cell_measurement_theta_min      2.438
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    22.963
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.898
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1383
_diffrn_reflns_av_unetI/netI     0.1700
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            4385
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.973
_diffrn_reflns_theta_max         24.973
_diffrn_reflns_theta_min         2.437
_diffrn_ambient_temperature      293.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.846
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                881
_reflns_number_total             2197
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.036
_refine_diff_density_min         -1.180
_refine_diff_density_rms         0.195
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.69(9)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     102
_refine_ls_number_reflns         2197
_refine_ls_number_restraints     119
_refine_ls_R_factor_all          0.1355
_refine_ls_R_factor_gt           0.0547
_refine_ls_restrained_S_all      1.001
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[σ²(Fo²)] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0934
_refine_ls_wR_factor_ref         0.1319
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.31(9)
 0.69(9)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C4-C3 = C3-C2
 1.53 with sigma of 0.02
 C1-C2 = C2-C3
 1.53 with sigma of 0.02
 C6-N1 = N1-C1
 1.45 with sigma of 0.02
 C6-N1 = N1-C5
 1.45 with sigma of 0.02
 C6-N1 = N1-C4
 1.45 with sigma of 0.02
 C4-C3 = C3-C2 = C1-C2
 1.53 with sigma of 0.01
 N1-C6 = N1-C5 = N1-C4 = N1-C1
 1.46 with sigma of 0.01
 C1-C3
 2.499 with sigma of 0.04
 C4-C2
 2.499 with sigma of 0.04
 C6-C5
 2.368 with sigma of 0.04
 C6-C4
 2.368 with sigma of 0.04
 C6-C1
 2.368 with sigma of 0.04
4. Restrained planarity
 C1, C2, C3, C4
 with sigma of 0.1
5. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Uanis(N1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C6) \\sim Ueq, Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C4) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
7.a Riding coordinates:
 C6(H6A,H6B,H6C)
7.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B)
7.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.000000 0.000000 -0.83679(13) 0.0526(5) Uani 1 3 d S TU P . .
Br1 Br -0.0189(2) -0.1473(2) -1.0827(4) 0.0795(12) Uani 1 1 d . U . . .
Pb2 Pb -0.333333 -0.666667 -0.4063(3) 0.0717(7) Uani 1 3 d S TU P . .
Pb3 Pb -0.333333 -0.666667 0.0951(3) 0.0753(7) Uani 1 3 d S TU P . .
Br2 Br -0.3154(2) -0.5192(2) -0.6557(7) 0.1005(15) Uani 1 1 d . U . . .
Br3 Br -0.4615(2) -0.6482(2) -0.1558(6) 0.0973(14) Uani 1 1 d . U . . .
N1 N -0.3251(6) -0.3285(6) -1.0925(13) 0.136(5) Uani 1 1 d D U . . .
C1 C -0.4231(9) -0.3980(16) -1.0911(15) 0.190(10) Uani 1 1 d D U . . .
H1A H -0.460754 -0.381031 -1.022211 0.228 Uiso 1 1 calc R U . . .
H1B H -0.435508 -0.459677 -1.062883 0.228 Uiso 1 1 calc R U . . .
C2 C -0.4258(8) -0.3812(14) -1.2843(15) 0.195(11) Uani 1 1 d D U . . .
H2A H -0.473097 -0.437552 -1.337769 0.234 Uiso 1 1 calc R U . . .
H2B H -0.442476 -0.333901 -1.301009 0.234 Uiso 1 1 calc R U . . .
C3 C -0.3333(7) -0.3511(13) -1.3726(16) 0.1647(13) Uani 1 1 d D U . . .
H3A H -0.306474 -0.288980 -1.418687 0.198 Uiso 1 1 calc R U . . .
H3B H -0.339274 -0.393331 -1.463683 0.198 Uiso 1 1 calc R U . . .
C4 C -0.2768(8) -0.3555(10) -1.2201(15) 0.1662(13) Uani 1 1 d D U . . .
H4A H -0.286417 -0.417018 -1.200585 0.199 Uiso 1 1 calc R U . . .
H4B H -0.211374 -0.311032 -1.229094 0.199 Uiso 1 1 calc R U . . .
C5 C -0.3036(14) -0.2328(7) -1.107(4) 0.136(7) Uani 1 1 d D U . . .
H5A H -0.310206 -0.219574 -1.224802 0.204 Uiso 1 1 calc R U . . .
H5B H -0.241284 -0.192341 -1.070076 0.204 Uiso 1 1 calc R U . . .
H5C H -0.345300 -0.223419 -1.036380 0.204 Uiso 1 1 calc R U . . .
C6 C -0.2858(12) -0.3302(17) -0.9255(15) 0.193(9) Uani 1 1 d D U . . .
H6A H -0.221326 -0.284601 -0.922788 0.289 Uiso 1 1 d R U . . .
H6B H -0.293116 -0.390441 -0.909048 0.289 Uiso 1 1 d R U . . .
H6C H -0.317436 -0.317851 -0.835449 0.289 Uiso 1 1 d 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 Br1 3.007(3) . ?
Pb1 Br1 3.047(3) 6 ?
Pb1 Br1 3.047(3) 4 ?
Pb1 Br1 3.007(3) 3 ?
Pb1 Br1 3.007(3) 2 ?
Pb1 Br1 3.047(3) 5 ?
Pb2 Br2 3.031(5) . ?
Pb2 Br2 3.031(5) 2_445 ?
Pb2 Br2 3.031(5) 3_545 ?
Pb2 Br3 3.023(5) 3_545 ?
Pb2 Br3 3.023(4) 2_445 ?
Pb2 Br3 3.023(4) . ?
Pb3 Br2 3.030(5) 2_446 ?
Pb3 Br2 3.030(5) 3_546 ?
Pb3 Br2 3.030(5) 1_556 ?
Pb3 Br3 3.025(5) 3_545 ?
Pb3 Br3 3.025(5) 2_445 ?
Pb3 Br3 3.025(5) . ?
N1 C1 1.460(10) . ?
N1 C4 1.484(11) . ?
N1 C5 1.458(11) . ?
N1 C6 1.462(9) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C2 1.533(11) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C3 1.528(10) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.540(11) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9601 . ?
C6 H6C 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 Br1 83.86(10) . 3 ?
Br1 Pb1 Br1 96.82(6) 2 6 ?
Br1 Pb1 Br1 179.08(11) 2 5 ?
Br1 Pb1 Br1 83.86(10) . 2 ?
Br1 Pb1 Br1 96.82(6) . 5 ?
Br1 Pb1 Br1 83.86(10) 3 2 ?
Br1 Pb1 Br1 179.08(11) 3 6 ?
Br1 Pb1 Br1 179.08(11) . 4 ?
Br1 Pb1 Br1 82.50(10) 4 6 ?
Br1 Pb1 Br1 96.82(6) 3 4 ?
Br1 Pb1 Br1 96.82(6) 3 5 ?
Br1 Pb1 Br1 96.82(6) 2 4 ?
Br1 Pb1 Br1 82.50(10) 4 5 ?
Br1 Pb1 Br1 96.82(6) . 6 ?
Br1 Pb1 Br1 82.50(10) 6 5 ?
Pb1 Br1 Pb1 79.92(8) . 4_554 ?
Br2 Pb2 Br2 83.44(14) 3_545 2_445 ?
Br2 Pb2 Br2 83.44(14) 3_545 . ?
Br2 Pb2 Br2 83.44(14) 2_445 . ?
Br3 Pb2 Br2 96.69(11) 2_445 2_445 ?
Br3 Pb2 Br2 179.63(14) 2_445 . ?
Br3 Pb2 Br2 96.69(11) . . ?
Br3 Pb2 Br2 96.92(10) 2_445 3_545 ?
Br3 Pb2 Br2 96.92(10) 3_545 . ?
Br3 Pb2 Br2 96.92(10) . 2_445 ?
Br3 Pb2 Br2 179.63(14) . 3_545 ?
Br3 Pb2 Br2 96.69(11) 3_545 3_545 ?
Br3 Pb2 Br2 179.63(14) 3_545 2_445 ?
Br3 Pb2 Br3 82.95(14) 2_445 . ?
Br3 Pb2 Br3 82.95(14) 3_545 . ?
Br3 Pb2 Br3 82.95(14) 2_445 3_545 ?
Br2 Pb3 Br2 83.47(14) 3_546 2_446 ?
Br2 Pb3 Br2 83.47(14) 2_446 1_556 ?
Br2 Pb3 Br2 83.47(14) 3_546 1_556 ?
Br3 Pb3 Br2 96.95(10) 2_445 3_546 ?
Br3 Pb3 Br2 179.57(15) 3_545 2_446 ?
Br3 Pb3 Br2 179.57(14) 2_445 1_556 ?
Br3 Pb3 Br2 96.71(11) 3_545 3_546 ?
Br3 Pb3 Br2 96.95(10) . 2_446 ?
Br3 Pb3 Br2 179.57(14) . 3_546 ?
Br3 Pb3 Br2 96.71(11) . 1_556 ?
Br3 Pb3 Br2 96.71(11) 2_445 2_446 ?
Br3 Pb3 Br2 96.95(10) 3_545 1_556 ?
Br3 Pb3 Br3 82.87(14) 2_445 3_545 ?
Br3 Pb3 Br3 82.87(14) 3_545 . ?
Br3 Pb3 Br3 82.87(14) 2_445 . ?
Pb3 Br2 Pb2 79.55(10) 1_554 . ?
Pb2 Br3 Pb3 80.28(10) . . ?
C1 N1 C4 109.1(12) . . ?
C1 N1 C6 108.3(11) . . ?
C5 N1 C1 115.8(16) . . ?
C5 N1 C4 114.1(15) . . ?
C5 N1 C6 103.0(15) . . ?
C6 N1 C4 105.7(12) . . ?
N1 C1 H1A 113.9 . . ?
N1 C1 H1B 113.9 . . ?
N1 C1 C2 88.3(9) . . ?
H1A C1 H1B 111.1 . . ?
C2 C1 H1A 113.9 . . ?
C2 C1 H1B 113.9 . . ?
C1 C2 H2A 109.1 . . ?
C1 C2 H2B 109.1 . . ?
H2A C2 H2B 107.8 . . ?
C3 C2 C1 112.6(11) . . ?
C3 C2 H2A 109.1 . . ?
C3 C2 H2B 109.1 . . ?
C2 C3 H3A 111.7 . . ?
C2 C3 H3B 111.7 . . ?
C2 C3 C4 100.4(10) . . ?
H3A C3 H3B 109.5 . . ?
C4 C3 H3A 111.7 . . ?
C4 C3 H3B 111.7 . . ?
N1 C4 C3 93.5(10) . . ?
N1 C4 H4A 113.0 . . ?
N1 C4 H4B 113.0 . . ?
C3 C4 H4A 113.0 . . ?
C3 C4 H4B 113.0 . . ?
H4A C4 H4B 110.4 . . ?
N1 C5 H5A 109.5 . . ?
N1 C5 H5B 109.5 . . ?
N1 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N1 C6 H6A 109.9 . . ?
N1 C6 H6B 108.4 . . ?
N1 C6 H6C 110.1 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 29.6(18) . . . . ?
C1 N1 C4 C3 61.7(14) . . . . ?
C1 C2 C3 C4 2.5(17) . . . . ?
C2 C3 C4 N1 -32.8(13) . . . . ?
C4 N1 C1 C2 -56.6(17) . . . . ?
C5 N1 C1 C2 74(2) . . . . ?
C5 N1 C4 C3 -69.6(14) . . . . ?
C6 N1 C1 C2 -171.2(16) . . . . ?
C6 N1 C4 C3 178.0(12) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.31(9)
2 0.69(9)

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

data_1_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2390415'
loop_
_audit_author_name
_audit_author_address
'Yang Zhu'
;southeast university
China
;
_audit_update_record             
;
2024-10-12 deposited with the CCDC.	2025-03-18 downloaded from the CCDC.
;
_audit_creation_date             2022-09-19
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br3 Pb, C6 H14 N'
_chemical_formula_sum            'C6 H14 Br3 N Pb'
_chemical_formula_weight         547.10
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           169
_space_group_name_H-M_alt        'P 61'
_space_group_name_Hall           'P 61'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'-x, -y, z+1/2'
'y, -x+y, z+5/6'
'x-y, x, z+1/6'

_cell_length_a                   9.6156(3)
_cell_length_b                   9.6156(3)
_cell_length_c                   22.9958(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1841.33(14)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    4587
_cell_measurement_temperature    252.97(10)
_cell_measurement_theta_max      28.7480
_cell_measurement_theta_min      2.4160
_shelx_estimated_absorpt_T_max   0.203
_shelx_estimated_absorpt_T_min   0.203
_exptl_absorpt_coefficient_mu    23.460
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.16764
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.960
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0729
_diffrn_reflns_av_unetI/netI     0.0657
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            8199
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        24.984
_diffrn_reflns_theta_max         24.984
_diffrn_reflns_theta_min         2.446
_diffrn_ambient_temperature      252.97(10)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.917
_reflns_Friedel_fraction_full    0.969
_reflns_Friedel_fraction_max     0.969
_reflns_number_gt                1892
_reflns_number_total             2139
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.109a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.109a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.109a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.961
_refine_diff_density_min         -1.814
_refine_diff_density_rms         0.205
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.50(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     103
_refine_ls_number_reflns         2139
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0408
_refine_ls_restrained_S_all      1.017
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0430P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0830
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.50(2)
 0.50(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B)
3.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.99048(7) -0.05226(4) 0.42225(5) 0.01872(10) Uani 1 1 d . . . . .
Br1 Br 0.74293(15) -0.14005(16) 0.51660(6) 0.0282(4) Uani 1 1 d . . . . .
Br2 Br 1.19815(16) 0.24050(15) 0.49334(6) 0.0278(4) Uani 1 1 d . . . . .
Br3 Br 1.12106(15) -0.20827(14) 0.50485(7) 0.0295(3) Uani 1 1 d . . . . .
N1 N 0.7151(11) 0.3275(11) 0.5224(5) 0.024(3) Uani 1 1 d . . . . .
C1 C 0.6772(15) 0.4111(15) 0.4748(7) 0.030(4) Uani 1 1 d . . . . .
H1A H 0.774989 0.507590 0.461886 0.036 Uiso 1 1 calc R U . . .
H1B H 0.600137 0.442278 0.488433 0.036 Uiso 1 1 calc R U . . .
C2 C 0.6056(17) 0.2896(16) 0.4254(7) 0.035(4) Uani 1 1 d . . . . .
H2A H 0.687767 0.308740 0.396292 0.042 Uiso 1 1 calc R U . . .
H2B H 0.518314 0.297004 0.406382 0.042 Uiso 1 1 calc R U . . .
C3 C 0.5413(18) 0.1230(18) 0.4539(8) 0.040(5) Uani 1 1 d . . . . .
H3A H 0.425885 0.054810 0.446854 0.048 Uiso 1 1 calc R U . . .
H3B H 0.597138 0.068997 0.438574 0.048 Uiso 1 1 calc R U . . .
C4 C 0.5749(18) 0.1577(15) 0.5181(7) 0.037(4) Uani 1 1 d . . . . .
H4A H 0.602324 0.081847 0.535864 0.044 Uiso 1 1 calc R U . . .
H4B H 0.480647 0.148662 0.537993 0.044 Uiso 1 1 calc R U . . .
C5 C 0.7364(18) 0.4025(18) 0.5781(8) 0.049(5) Uani 1 1 d . . . . .
H5A H 0.821563 0.513677 0.575754 0.074 Uiso 1 1 calc R U . . .
H5B H 0.764858 0.346465 0.606604 0.074 Uiso 1 1 calc R U . . .
H5C H 0.637300 0.398048 0.589747 0.074 Uiso 1 1 calc R U . . .
C6 C 0.8662(16) 0.3267(17) 0.5053(9) 0.038(4) Uani 1 1 d . . . . .
H6A H 0.952053 0.436077 0.498968 0.058 Uiso 1 1 calc R U . . .
H6B H 0.847101 0.265225 0.469808 0.058 Uiso 1 1 calc R U . . .
H6C H 0.896467 0.278238 0.536151 0.058 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 Br1 3.0055(15) 5_664 ?
Pb1 Br1 3.0129(16) . ?
Pb1 Br2 2.9939(15) . ?
Pb1 Br2 3.0414(16) 5_664 ?
Pb1 Br3 3.0526(17) . ?
Pb1 Br3 3.0654(17) 5_664 ?
N1 C1 1.506(19) . ?
N1 C4 1.514(15) . ?
N1 C5 1.43(2) . ?
N1 C6 1.509(18) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 C2 1.52(2) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 C3 1.55(2) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 C4 1.51(2) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 H5C 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 H6C 0.9700 . ?

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 93.72(3) 5_664 . ?
Br1 Pb1 Br2 178.92(4) . 5_664 ?
Br1 Pb1 Br2 85.41(4) 5_664 5_664 ?
Br1 Pb1 Br3 82.77(5) 5_664 5_664 ?
Br1 Pb1 Br3 175.00(5) 5_664 . ?
Br1 Pb1 Br3 82.86(5) . . ?
Br1 Pb1 Br3 98.56(4) . 5_664 ?
Br2 Pb1 Br1 93.20(4) . 5_664 ?
Br2 Pb1 Br1 86.12(4) . . ?
Br2 Pb1 Br2 93.30(3) . 5_664 ?
Br2 Pb1 Br3 173.98(5) . 5_664 ?
Br2 Pb1 Br3 97.98(4) 5_664 . ?
Br2 Pb1 Br3 82.96(5) . . ?
Br2 Pb1 Br3 81.97(4) 5_664 5_664 ?
Br3 Pb1 Br3 101.31(3) . 5_664 ?
Pb1 Br1 Pb1 79.80(3) 6_545 . ?
Pb1 Br2 Pb1 79.53(3) . 6_545 ?
Pb1 Br3 Pb1 78.25(3) . 6_545 ?
C1 N1 C4 101.9(10) . . ?
C1 N1 C6 107.7(11) . . ?
C5 N1 C1 113.2(12) . . ?
C5 N1 C4 115.3(12) . . ?
C5 N1 C6 109.8(12) . . ?
C6 N1 C4 108.5(10) . . ?
N1 C1 H1A 110.6 . . ?
N1 C1 H1B 110.6 . . ?
N1 C1 C2 105.7(11) . . ?
H1A C1 H1B 108.7 . . ?
C2 C1 H1A 110.6 . . ?
C2 C1 H1B 110.6 . . ?
C1 C2 H2A 110.6 . . ?
C1 C2 H2B 110.6 . . ?
C1 C2 C3 105.7(13) . . ?
H2A C2 H2B 108.7 . . ?
C3 C2 H2A 110.6 . . ?
C3 C2 H2B 110.6 . . ?
C2 C3 H3A 110.8 . . ?
C2 C3 H3B 110.8 . . ?
H3A C3 H3B 108.9 . . ?
C4 C3 C2 104.8(12) . . ?
C4 C3 H3A 110.8 . . ?
C4 C3 H3B 110.8 . . ?
N1 C4 H4A 110.5 . . ?
N1 C4 H4B 110.5 . . ?
C3 C4 N1 106.2(12) . . ?
C3 C4 H4A 110.5 . . ?
C3 C4 H4B 110.5 . . ?
H4A C4 H4B 108.7 . . ?
N1 C5 H5A 109.5 . . ?
N1 C5 H5B 109.5 . . ?
N1 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N1 C6 H6A 109.5 . . ?
N1 C6 H6B 109.5 . . ?
N1 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 22.4(14) . . . . ?
C1 N1 C4 C3 38.9(15) . . . . ?
C1 C2 C3 C4 1.7(16) . . . . ?
C2 C3 C4 N1 -25.2(17) . . . . ?
C4 N1 C1 C2 -37.4(13) . . . . ?
C5 N1 C1 C2 -161.8(11) . . . . ?
C5 N1 C4 C3 161.9(14) . . . . ?
C6 N1 C1 C2 76.6(12) . . . . ?
C6 N1 C4 C3 -74.5(16) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.50(2)
2 0.50(2)

