# Supplementary Information (SI) for Chemical Science.
# 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_exp_300K
_database_code_depnum_ccdc_archive 'CCDC 2405625'
loop_
_audit_author_name
_audit_author_address
ClPAPbBrL
;Institute of Crystalline Materials, Shanxi University, Taiyuan
China
;
_audit_update_record             
;
2024-11-27 deposited with the CCDC.	2025-09-30 downloaded from the CCDC.
;
_audit_creation_date             2024-11-10
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br4 Pb, 2(C3 H9 Cl N)'
_chemical_formula_sum            'C6 H18 Br4 Cl2 N2 Pb'
_chemical_formula_weight         715.92
_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'
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      orthorhombic
_space_group_IT_number           36
_space_group_name_H-M_alt        'C m c 21'
_space_group_name_Hall           'C 2c -2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   27.1369(14)
_cell_length_b                   8.3450(3)
_cell_length_c                   8.1438(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1844.22(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5141
_cell_measurement_temperature    300.15
_cell_measurement_theta_max      30.6950
_cell_measurement_theta_min      2.5140
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    18.084
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.579
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1296
_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  0.0767
_diffrn_reflns_av_unetI/netI     0.0581
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.917
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            12754
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.860
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.719
_diffrn_reflns_theta_min         2.553
_diffrn_ambient_temperature      300.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.758
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.794
_reflns_number_gt                1920
_reflns_number_total             2509
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         2.164
_refine_diff_density_min         -1.777
_refine_diff_density_rms         0.293
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.492(14)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     75
_refine_ls_number_reflns         2509
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0803
_refine_ls_R_factor_gt           0.0577
_refine_ls_restrained_S_all      1.012
_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)+(0.1078P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1512
_refine_ls_wR_factor_ref         0.1597
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.508(14)
 0.492(14)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
3. Restrained distances
 C2-C3
 1.5 with sigma of 0.02
 C2-C1
 1.5 with sigma of 0.02
 N1-C1
 1.47 with sigma of 0.02
 Pb1-Br1
 3.04 with sigma of 0.001
4. Rigid bond restraints
 N1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C2, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
Uanis(C3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C2) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
6.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C2(H2A,H2B), C1(H1D,H1E)
6.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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 0.500000 0.73797(4) 0.50161(4) 0.04245(9) Uani 1 2 d DS T P . .
Br3 Br 0.500000 0.42308(16) 0.6763(2) 0.0844(5) Uani 1 2 d S T P . .
Br1 Br 0.500000 1.05128(8) 0.30988(11) 0.0580(3) Uani 1 2 d DS T P . .
Br2 Br 0.60944(4) 0.76930(12) 0.48298(16) 0.0712(3) Uani 1 1 d . . . . .
N1 N 0.5919(4) 0.1617(11) 0.5751(11) 0.083(3) Uani 1 1 d D . . . .
H1A H 0.611664 0.078862 0.595420 0.100 Uiso 1 1 calc R U . . .
H1B H 0.564069 0.126695 0.529893 0.100 Uiso 1 1 calc R U . . .
H1C H 0.585139 0.212259 0.668573 0.100 Uiso 1 1 calc R U . . .
C3 C 0.6939(4) 0.3898(18) 0.3616(18) 0.109(4) Uani 1 1 d D U . . .
H3A H 0.684327 0.500709 0.377356 0.131 Uiso 1 1 calc R U . . .
H3B H 0.687268 0.357554 0.249351 0.131 Uiso 1 1 calc R U . . .
Cl1 Cl 0.76171(7) 0.3516(3) 0.4238(3) 0.0597(6) Uani 1 1 d . . . . .
C2 C 0.6697(4) 0.2783(17) 0.486(2) 0.136(4) Uani 1 1 d D U . . .
H2A H 0.683596 0.171675 0.475075 0.163 Uiso 1 1 calc R U . . .
H2B H 0.677018 0.316074 0.596421 0.163 Uiso 1 1 calc R U . . .
C1 C 0.6159(4) 0.2699(14) 0.4644(18) 0.121(5) Uani 1 1 d D U . . .
H1D H 0.602204 0.376230 0.479593 0.146 Uiso 1 1 calc R U . . .
H1E H 0.608914 0.236946 0.352647 0.146 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 Br3 2.9704(16) 2_664 ?
Pb1 Br3 2.9883(14) . ?
Pb1 Br1 3.0653(9) 2_675 ?
Pb1 Br1 3.0453(7) . ?
Pb1 Br2 2.9851(11) 3_655 ?
Pb1 Br2 2.9852(11) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.432(14) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 Cl1 1.934(13) . ?
C3 C2 1.527(17) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C1 1.473(14) . ?
C1 H1D 0.9700 . ?
C1 H1E 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
Br3 Pb1 Br3 91.533(19) 2_664 . ?
Br3 Pb1 Br1 177.59(4) . . ?
Br3 Pb1 Br1 96.58(4) . 2_675 ?
Br3 Pb1 Br1 86.06(3) 2_664 . ?
Br3 Pb1 Br1 171.89(3) 2_664 2_675 ?
Br3 Pb1 Br2 89.67(3) 2_664 . ?
Br3 Pb1 Br2 89.67(3) 2_664 3_655 ?
Br1 Pb1 Br1 85.833(11) . 2_675 ?
Br2 Pb1 Br3 95.81(2) . . ?
Br2 Pb1 Br3 95.81(2) 3_655 . ?
Br2 Pb1 Br1 89.51(2) 3_655 2_675 ?
Br2 Pb1 Br1 84.19(2) 3_655 . ?
Br2 Pb1 Br1 89.51(2) . 2_675 ?
Br2 Pb1 Br1 84.19(2) . . ?
Br2 Pb1 Br2 168.38(4) 3_655 . ?
Pb1 Br3 Pb1 145.34(6) 2_665 . ?
Pb1 Br1 Pb1 155.86(3) . 2_674 ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
H3A C3 H3B 109.8 . . ?
Cl1 C3 H3A 112.2 . . ?
Cl1 C3 H3B 112.2 . . ?
C2 C3 H3A 112.2 . . ?
C2 C3 H3B 112.2 . . ?
C2 C3 Cl1 97.7(8) . . ?
C3 C2 H2A 109.2 . . ?
C3 C2 H2B 109.2 . . ?
H2A C2 H2B 107.9 . . ?
C1 C2 C3 112.0(12) . . ?
C1 C2 H2A 109.2 . . ?
C1 C2 H2B 109.2 . . ?
N1 C1 C2 113.8(11) . . ?
N1 C1 H1D 108.8 . . ?
N1 C1 H1E 108.8 . . ?
C2 C1 H1D 108.8 . . ?
C2 C1 H1E 108.8 . . ?
H1D C1 H1E 107.7 . . ?

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
C3 C2 C1 N1 177.7(11) . . . . ?
Cl1 C3 C2 C1 -176.0(11) . . . . ?


_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.508(14)
2 0.492(14)

####################################################################### 
# 
# 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_exp_355K
_database_code_depnum_ccdc_archive 'CCDC 2405626'
loop_
_audit_author_name
_audit_author_address
ClPAPbBrI
;Institute of Crystalline Materials, Shanxi University, Taiyuan
China
;
_audit_update_record             
;
2024-11-27 deposited with the CCDC.	2025-09-30 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, 2(C3 H9 Cl N)'
_chemical_formula_sum            'C6 H18 Br4 Cl2 N2 Pb'
_chemical_formula_weight         715.92

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'
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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_H-M_alt        'C m c 21'
_space_group_name_Hall           'C 2c -2'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   27.3369(18)
_cell_length_b                   8.3933(4)
_cell_length_c                   8.1734(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1875.36(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    355(2)
_cell_measurement_reflns_used    5206
_cell_measurement_theta_min      2.5260
_cell_measurement_theta_max      29.6090

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.536
_exptl_crystal_F_000             1296
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    17.783
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      355(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10585
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_av_R_equivalents  0.0564
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.538
_diffrn_reflns_theta_max         30.820
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.879
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.879
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.794
_diffrn_reflns_point_group_measured_fraction_full 0.959
_reflns_number_total             2378
_reflns_number_gt                1848
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.695
_reflns_Friedel_fraction_max     0.698
_reflns_Friedel_fraction_full    0.912

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)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_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.073(19)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2378
_refine_ls_number_parameters     75
_refine_ls_number_restraints     17
_refine_ls_R_factor_all          0.0915
_refine_ls_R_factor_gt           0.0698
_refine_ls_wR_factor_ref         0.2274
_refine_ls_wR_factor_gt          0.2085
_refine_ls_goodness_of_fit_ref   0.902
_refine_ls_restrained_S_all      0.901
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Pb01 Pb 0.500000 0.76079(5) 0.56087(8) 0.04703(12) Uani 1 2 d S T P . .
Br2 Br 0.500000 0.55264(19) 0.8644(2) 0.0661(5) Uani 1 2 d S T P . .
Br1 Br 0.39127(6) 0.72859(17) 0.5439(3) 0.0842(5) Uani 1 1 d . . . . .
Br3 Br 0.500000 0.9267(2) 0.2361(3) 0.0918(7) Uani 1 2 d S T P . .
Cl1 Cl 0.26196(10) 0.6500(3) 0.4816(4) 0.0667(8) Uani 1 1 d D . . . .
C3 C 0.1982(4) 0.633(2) 0.423(2) 0.158(4) Uani 1 1 d D U . . .
H3A H 0.193337 0.676301 0.313949 0.189 Uiso 1 1 calc R U . . .
H3B H 0.188235 0.522200 0.422431 0.189 Uiso 1 1 calc R U . . .
N1 N 0.0914(5) 0.8308(13) 0.6333(14) 0.092(4) Uani 1 1 d D . . . .
H1A H 0.059107 0.820998 0.625822 0.110 Uiso 1 1 calc R U . . .
H1B H 0.099947 0.931090 0.612436 0.110 Uiso 1 1 calc R U . . .
H1C H 0.101031 0.804649 0.733870 0.110 Uiso 1 1 calc R U . . .
C1 C 0.1146(4) 0.7262(19) 0.516(2) 0.160(4) Uani 1 1 d D U . . .
H1D H 0.107733 0.762792 0.405981 0.191 Uiso 1 1 calc R U . . .
H1E H 0.101649 0.619183 0.527734 0.191 Uiso 1 1 calc R U . . .
C2 C 0.1687(4) 0.725(2) 0.545(2) 0.160(3) Uani 1 1 d D U . . .
H2A H 0.174786 0.680876 0.652674 0.192 Uiso 1 1 calc R U . . .
H2B H 0.180195 0.834286 0.545572 0.192 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
Pb01 Br1 2.9877(16) 4_655 ?
Pb01 Br1 2.9878(16) . ?
Pb01 Br3 2.989(2) 2_675 ?
Pb01 Br3 2.998(2) . ?
Pb01 Br2 3.0342(17) . ?
Pb01 Br2 3.0822(17) 2_664 ?
Cl1 C3 1.814(11) . ?
C3 C2 1.497(18) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
N1 C1 1.445(17) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
C1 C2 1.497(15) . ?
C1 H1D 0.9700 . ?
C1 H1E 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 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 Pb01 Br1 168.34(7) 4_655 . ?
Br1 Pb01 Br3 95.83(3) 4_655 2_675 ?
Br1 Pb01 Br3 95.83(3) . 2_675 ?
Br1 Pb01 Br3 90.06(4) 4_655 . ?
Br1 Pb01 Br3 90.06(4) . . ?
Br3 Pb01 Br3 90.95(3) 2_675 . ?
Br1 Pb01 Br2 89.19(4) 4_655 . ?
Br1 Pb01 Br2 89.19(4) . . ?
Br3 Pb01 Br2 96.53(6) 2_675 . ?
Br3 Pb01 Br2 172.52(5) . . ?
Br1 Pb01 Br2 84.18(3) 4_655 2_664 ?
Br1 Pb01 Br2 84.18(3) . 2_664 ?
Br3 Pb01 Br2 177.23(6) 2_675 2_664 ?
Br3 Pb01 Br2 86.27(5) . 2_664 ?
Br2 Pb01 Br2 86.248(17) . 2_664 ?
Pb01 Br2 Pb01 156.56(6) . 2_665 ?
Pb01 Br3 Pb01 146.31(8) 2_674 . ?
C2 C3 Cl1 107.6(10) . . ?
C2 C3 H3A 110.2 . . ?
Cl1 C3 H3A 110.2 . . ?
C2 C3 H3B 110.2 . . ?
Cl1 C3 H3B 110.2 . . ?
H3A C3 H3B 108.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
H1A N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
N1 C1 C2 109.4(13) . . ?
N1 C1 H1D 109.8 . . ?
C2 C1 H1D 109.8 . . ?
N1 C1 H1E 109.8 . . ?
C2 C1 H1E 109.8 . . ?
H1D C1 H1E 108.2 . . ?
C1 C2 C3 115.6(13) . . ?
C1 C2 H2A 108.4 . . ?
C3 C2 H2A 108.4 . . ?
C1 C2 H2B 108.4 . . ?
C3 C2 H2B 108.4 . . ?
H2A C2 H2B 107.5 . . ?

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 -174.7(15) . . . . ?
Cl1 C3 C2 C1 179.6(13) . . . . ?

_refine_diff_density_max         3.307
_refine_diff_density_min         -1.390
_refine_diff_density_rms         0.396

####################################################################### 
# 
# 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_exp_375K
_database_code_depnum_ccdc_archive 'CCDC 2405627'
loop_
_audit_author_name
_audit_author_address
ClPAPbBrH
;Institute of Crystalline Materials, Shanxi University, Taiyuan
China
;
_audit_update_record             
;
2024-11-27 deposited with the CCDC.	2025-09-30 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, 2(C3 H9 Cl N)'
_chemical_formula_sum            'C6 H18 Br4 Cl2 N2 Pb'
_chemical_formula_weight         715.92

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'
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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

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

_cell_length_a                   8.3957(5)
_cell_length_b                   8.2101(5)
_cell_length_c                   27.289(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1881.0(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    375(2)
_cell_measurement_reflns_used    3135
_cell_measurement_theta_min      2.8440
_cell_measurement_theta_max      29.9650

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.528
_exptl_crystal_F_000             1296
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    17.730
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      375(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9088
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         2.849
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_full        25.025
_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             1636
_reflns_number_gt                1121
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_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)+(0.0800P)²+50.0000P] 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         1636
_refine_ls_number_parameters     80
_refine_ls_number_restraints     63
_refine_ls_R_factor_all          0.1003
_refine_ls_R_factor_gt           0.0730
_refine_ls_wR_factor_ref         0.2109
_refine_ls_wR_factor_gt          0.1940
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_restrained_S_all      1.118
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001

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 1.000000 0.500000 0.05336(15) Uani 1 2 d S . P . .
Br2 Br 1.19381(16) 0.69205(16) 0.49679(6) 0.0906(5) Uani 1 1 d . . . . .
Br1 Br 1.0316(2) 1.0167(2) 0.60845(6) 0.0966(5) Uani 1 1 d . . . . .
Cl1 Cl 0.8981(3) 0.5770(4) 0.76053(10) 0.0759(9) Uani 1 1 d D . . . .
N1 N 1.0753(11) 0.4213(12) 0.5916(5) 0.2140(7) Uani 1 1 d D U . . .
H1A H 1.061298 0.421489 0.559298 0.257 Uiso 1 1 calc R U . . .
H1B H 1.060688 0.320927 0.603127 0.257 Uiso 1 1 calc R U . . .
H1C H 1.173753 0.454118 0.598579 0.257 Uiso 1 1 calc R U . . .
C4 C 0.8591(8) 0.6234(9) 0.6980(2) 0.2145(2) Uani 1 1 d D U . . .
H4BC H 0.761027 0.571252 0.687643 0.257 Uiso 0.5 1 calc R U P A 2
H4BD H 0.847208 0.740108 0.693896 0.257 Uiso 0.5 1 calc R U P A 2
H4AA H 0.745436 0.620963 0.691635 0.257 Uiso 0.5 1 calc R U P B 1
H4AB H 0.899208 0.730865 0.689931 0.257 Uiso 0.5 1 calc R U P B 1
C1 C 0.9600(10) 0.5323(11) 0.61453(13) 0.2145(2) Uani 1 1 d D U . . .
H1BC H 0.854020 0.486110 0.611663 0.257 Uiso 0.5 1 calc R U P C 2
H1BD H 0.960667 0.635208 0.597078 0.257 Uiso 0.5 1 calc R U P C 2
H1AA H 0.857348 0.520820 0.598562 0.257 Uiso 0.5 1 calc R U P D 1
H1AB H 0.995313 0.643893 0.610321 0.257 Uiso 0.5 1 calc R U P D 1
C3 C 0.9959(8) 0.5628(16) 0.66763(15) 0.21452(18) Uani 0.5 1 d D U P E 2
H3A H 1.081544 0.641806 0.669620 0.257 Uiso 0.5 1 calc R U P E 2
H3B H 1.034466 0.462160 0.681978 0.257 Uiso 0.5 1 calc R U P E 2
C2 C 0.9429(14) 0.4957(10) 0.66820(18) 0.21452(18) Uani 0.5 1 d D U P E 1
H2A H 1.048355 0.479475 0.681865 0.257 Uiso 0.5 1 calc R U P E 1
H2B H 0.885281 0.393887 0.671666 0.257 Uiso 0.5 1 calc R U P E 1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br1 2.9746(16) . ?
Pb1 Br1 2.9746(16) 5_776 ?
Pb1 Br2 3.0079(13) . ?
Pb1 Br2 3.0079(13) 5_776 ?
Pb1 Br2 3.0170(13) 4_466 ?
Pb1 Br2 3.0170(13) 8_865 ?
Cl1 C4 1.778(7) . ?
N1 C1 1.469(8) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
C4 C3 1.502(7) . ?
C4 C2 1.502(7) . ?
C4 H4BC 0.9700 . ?
C4 H4BD 0.9700 . ?
C4 H4AA 0.9700 . ?
C4 H4AB 0.9700 . ?
C1 C3 1.501(5) . ?
C1 C2 1.502(6) . ?
C1 H1BC 0.9700 . ?
C1 H1BD 0.9700 . ?
C1 H1AA 0.9700 . ?
C1 H1AB 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 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 180.00(6) . 5_776 ?
Br1 Pb1 Br2 91.12(4) . . ?
Br1 Pb1 Br2 88.88(4) 5_776 . ?
Br1 Pb1 Br2 88.88(4) . 5_776 ?
Br1 Pb1 Br2 91.12(4) 5_776 5_776 ?
Br2 Pb1 Br2 180.0 . 5_776 ?
Br1 Pb1 Br2 94.07(4) . 4_466 ?
Br1 Pb1 Br2 85.92(4) 5_776 4_466 ?
Br2 Pb1 Br2 91.289(12) . 4_466 ?
Br2 Pb1 Br2 88.711(12) 5_776 4_466 ?
Br1 Pb1 Br2 85.93(4) . 8_865 ?
Br1 Pb1 Br2 94.08(4) 5_776 8_865 ?
Br2 Pb1 Br2 88.711(12) . 8_865 ?
Br2 Pb1 Br2 91.289(12) 5_776 8_865 ?
Br2 Pb1 Br2 180.0 4_466 8_865 ?
Pb1 Br2 Pb1 154.08(5) . 4_566 ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
H1A N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C3 C4 Cl1 108.5(4) . . ?
C2 C4 Cl1 106.5(5) . . ?
C3 C4 H4BC 110.0 . . ?
Cl1 C4 H4BC 110.0 . . ?
C3 C4 H4BD 110.0 . . ?
Cl1 C4 H4BD 110.0 . . ?
H4BC C4 H4BD 108.4 . . ?
C2 C4 H4AA 110.4 . . ?
Cl1 C4 H4AA 110.4 . . ?
C2 C4 H4AB 110.4 . . ?
Cl1 C4 H4AB 110.4 . . ?
H4AA C4 H4AB 108.6 . . ?
N1 C1 C3 112.4(8) . . ?
N1 C1 C2 110.7(8) . . ?
N1 C1 H1BC 109.1 . . ?
C3 C1 H1BC 109.1 . . ?
N1 C1 H1BD 109.1 . . ?
C3 C1 H1BD 109.1 . . ?
H1BC C1 H1BD 107.8 . . ?
N1 C1 H1AA 109.5 . . ?
C2 C1 H1AA 109.5 . . ?
N1 C1 H1AB 109.5 . . ?
C2 C1 H1AB 109.5 . . ?
H1AA C1 H1AB 108.1 . . ?
C1 C3 C4 115.8(6) . . ?
C1 C3 H3A 108.3 . . ?
C4 C3 H3A 108.3 . . ?
C1 C3 H3B 108.3 . . ?
C4 C3 H3B 108.3 . . ?
H3A C3 H3B 107.4 . . ?
C1 C2 C4 115.7(6) . . ?
C1 C2 H2A 108.4 . . ?
C4 C2 H2A 108.4 . . ?
C1 C2 H2B 108.4 . . ?
C4 C2 H2B 108.4 . . ?
H2A C2 H2B 107.4 . . ?

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 C3 C4 -159.3(9) . . . . ?
Cl1 C4 C3 C1 157.5(8) . . . . ?
N1 C1 C2 C4 166.2(9) . . . . ?
Cl1 C4 C2 C1 -165.8(7) . . . . ?

_refine_diff_density_max         2.287
_refine_diff_density_min         -1.170
_refine_diff_density_rms         0.283

