# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2022

####################################################################### 
# 
# 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_20210706-LDFD-57
_database_code_depnum_ccdc_archive 'CCDC 2189149'
loop_
_audit_author_name
_audit_author_address
'yan sui'
;School of Chemistry and Chemical Engineering, Jinggangshan University
China
;
_audit_update_record             
;
2022-07-09 deposited with the CCDC.	2022-09-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C5 H13 Br3 Cl N Pb'
_chemical_formula_sum            'C5 H13 Br3 Cl N Pb'
_chemical_formula_weight         569.53

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'C c'
_space_group_name_Hall           'C -2yc'

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

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

_cell_length_a                   8.9465(5)
_cell_length_b                   17.4587(9)
_cell_length_c                   8.1154(4)
_cell_angle_alpha                90
_cell_angle_beta                 96.586(5)
_cell_angle_gamma                90
_cell_volume                     1259.21(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1755
_cell_measurement_theta_min      3.8070
_cell_measurement_theta_max      28.6100

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.004
_exptl_crystal_F_000             1016
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    23.082
_shelx_estimated_absorpt_T_min   0.065
_shelx_estimated_absorpt_T_max   0.097
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.43751
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            2493
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         3.417
_diffrn_reflns_theta_max         25.491
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.634
_diffrn_reflns_point_group_measured_fraction_full 0.638
_reflns_number_total             1487
_reflns_number_gt                1438
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.266
_reflns_Friedel_fraction_max     0.267
_reflns_Friedel_fraction_full    0.275

_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       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_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)+(0.0442P)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     SHELXL
_refine_ls_extinction_coef       0.0038(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.005(17)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1487
_refine_ls_number_parameters     104
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0342
_refine_ls_wR_factor_ref         0.0817
_refine_ls_wR_factor_gt          0.0812
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.064
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.5181(2) 0.63226(10) 0.4742(2) 0.0239(4) Uani 1 1 d . . . . .
Br2 Br 0.2722(2) 0.45128(11) 0.5186(2) 0.0279(5) Uani 1 1 d . . . . .
Br3 Br 0.7289(2) 0.43680(12) 0.5784(2) 0.0336(5) Uani 1 1 d . . . . .
C1 C 0.572(2) 0.1276(11) 0.349(2) 0.032(5) Uani 1 1 d . . . . .
H1A H 0.5584 0.0826 0.2787 0.039 Uiso 1 1 calc R U . . .
H1B H 0.6758 0.1273 0.4003 0.039 Uiso 1 1 calc R U . . .
C2 C 0.468(2) 0.1215(10) 0.4857(19) 0.027(4) Uani 1 1 d . . . . .
H2A H 0.3645 0.1244 0.4343 0.032 Uiso 1 1 calc R U . . .
H2B H 0.4815 0.0714 0.5371 0.032 Uiso 1 1 calc R U . . .
C3 C 0.4125(19) 0.2543(11) 0.575(2) 0.031(4) Uani 1 1 d . . . . .
H3A H 0.3075 0.2445 0.5442 0.047 Uiso 1 1 calc R U . . .
H3B H 0.4551 0.2773 0.4841 0.047 Uiso 1 1 calc R U . . .
H3C H 0.4241 0.2884 0.6688 0.047 Uiso 1 1 calc R U . . .
C4 C 0.6537(18) 0.1982(13) 0.674(2) 0.036(5) Uani 1 1 d . . . . .
H4A H 0.7022 0.2123 0.5784 0.054 Uiso 1 1 calc R U . . .
H4B H 0.7011 0.1533 0.7239 0.054 Uiso 1 1 calc R U . . .
H4C H 0.6621 0.2395 0.7521 0.054 Uiso 1 1 calc R U . . .
C5 C 0.424(2) 0.1487(14) 0.766(2) 0.041(6) Uani 1 1 d . . . . .
H5A H 0.4333 0.1851 0.8558 0.061 Uiso 1 1 calc R U . . .
H5B H 0.4761 0.1025 0.8016 0.061 Uiso 1 1 calc R U . . .
H5C H 0.3193 0.1375 0.7354 0.061 Uiso 1 1 calc R U . . .
Cl1 Cl 0.5443(6) 0.2107(3) 0.2214(5) 0.0362(11) Uani 1 1 d . . . . .
N1 N 0.4903(14) 0.1817(8) 0.6205(16) 0.020(3) Uani 1 1 d . . . . .
Pb1 Pb 0.50903(13) 0.49624(4) 0.27975(13) 0.0209(2) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 Pb1 2.8473(18) . ?
Br2 Pb1 2.965(2) 2_565 ?
Br2 Pb1 3.131(2) . ?
Br3 Pb1 2.940(2) 2_565 ?
Br3 Pb1 3.118(2) . ?
C1 C2 1.54(2) . ?
C1 Cl1 1.783(18) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N1 1.51(2) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 N1 1.47(2) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 N1 1.503(19) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 N1 1.50(2) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
Pb1 Br3 2.940(2) 2_564 ?
Pb1 Br2 2.965(2) 2_564 ?

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
Pb1 Br2 Pb1 83.46(5) 2_565 . ?
Pb1 Br3 Pb1 84.10(5) 2_565 . ?
C2 C1 Cl1 114.7(13) . . ?
C2 C1 H1A 108.6 . . ?
Cl1 C1 H1A 108.6 . . ?
C2 C1 H1B 108.6 . . ?
Cl1 C1 H1B 108.6 . . ?
H1A C1 H1B 107.6 . . ?
N1 C2 C1 115.6(15) . . ?
N1 C2 H2A 108.4 . . ?
C1 C2 H2A 108.4 . . ?
N1 C2 H2B 108.4 . . ?
C1 C2 H2B 108.4 . . ?
H2A C2 H2B 107.5 . . ?
N1 C3 H3A 109.5 . . ?
N1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N1 C5 H5A 109.5 . . ?
N1 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N1 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C3 N1 C5 107.9(15) . . ?
C3 N1 C4 108.9(14) . . ?
C5 N1 C4 107.9(12) . . ?
C3 N1 C2 113.5(12) . . ?
C5 N1 C2 105.7(13) . . ?
C4 N1 C2 112.6(13) . . ?
Br1 Pb1 Br3 89.89(6) . 2_564 ?
Br1 Pb1 Br2 96.37(6) . 2_564 ?
Br3 Pb1 Br2 87.05(6) 2_564 2_564 ?
Br1 Pb1 Br3 82.62(6) . . ?
Br3 Pb1 Br3 99.31(7) 2_564 . ?
Br2 Pb1 Br3 173.54(7) 2_564 . ?
Br1 Pb1 Br2 81.04(6) . . ?
Br3 Pb1 Br2 170.79(6) 2_564 . ?
Br2 Pb1 Br2 92.35(6) 2_564 . ?
Br3 Pb1 Br2 81.19(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
Cl1 C1 C2 N1 -66.4(19) . . . . ?
C1 C2 N1 C3 83.0(18) . . . . ?
C1 C2 N1 C5 -158.9(15) . . . . ?
C1 C2 N1 C4 -41(2) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C4 H4B Br2 0.96 3.02 3.89(2) 150.9 4
C3 H3C Br1 0.96 2.88 3.819(17) 166.5 2_565
C3 H3B Cl1 0.96 2.63 3.318(17) 128.7 .
C1 H1B Br1 0.97 3.05 4.00(2) 165.8 3_545
C1 H1A Br2 0.97 3.06 3.656(19) 120.8 4_554
C4 H4B Br2 0.96 3.02 3.89(2) 150.9 4
C3 H3C Br1 0.96 2.88 3.819(17) 166.5 2_565
C3 H3B Cl1 0.96 2.63 3.318(17) 128.7 .
C1 H1B Br1 0.97 3.05 4.00(2) 165.8 3_545
C1 H1A Br2 0.97 3.06 3.656(19) 120.8 4_554
C1 H1A Br2 0.97 3.06 3.656(19) 120.8 4_554
C1 H1B Br1 0.97 3.05 4.00(2) 165.8 3_545
C3 H3B Cl1 0.96 2.63 3.318(17) 128.7 .
C3 H3C Br1 0.96 2.88 3.819(17) 166.5 2_565
C4 H4B Br2 0.96 3.02 3.89(2) 150.9 4
C1 H1A Br2 0.97 3.06 3.656(19) 120.8 4_554
C1 H1B Br1 0.97 3.05 4.00(2) 165.8 3_545
C3 H3B Cl1 0.96 2.63 3.318(17) 128.7 .
C3 H3C Br1 0.96 2.88 3.819(17) 166.5 2_565
C4 H4B Br2 0.96 3.02 3.89(2) 150.9 4

_refine_diff_density_max         1.857
_refine_diff_density_min         -2.071
_refine_diff_density_rms         0.255

_shelxl_version_number           2014-3

####################################################################### 
# 
# 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_cc
_database_code_depnum_ccdc_archive 'CCDC 2189151'
loop_
_audit_author_name
_audit_author_address
'yan sui'
;School of Chemistry and Chemical Engineering, Jinggangshan University
China
;
_audit_update_record             
;
2022-07-09 deposited with the CCDC.	2022-09-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C5 H13 Br3 Cl N Pb'
_chemical_formula_sum            'C5 H13 Br3 Cl N Pb'
_chemical_formula_weight         569.53

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'C c'
_space_group_name_Hall           'C -2yc'

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

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

_cell_length_a                   9.0546(5)
_cell_length_b                   17.6736(8)
_cell_length_c                   8.1163(3)
_cell_angle_alpha                90
_cell_angle_beta                 96.279(4)
_cell_angle_gamma                90
_cell_volume                     1291.04(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    332.99(11)
_cell_measurement_reflns_used    3708
_cell_measurement_theta_min      2.2930
_cell_measurement_theta_max      30.9150

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.930
_exptl_crystal_F_000             1016
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    22.513
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.21586
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      332.99(11)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6242
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.305
_diffrn_reflns_theta_max         25.482
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.917
_diffrn_reflns_point_group_measured_fraction_full 0.923
_reflns_number_total             2189
_reflns_number_gt                2037
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.827
_reflns_Friedel_fraction_max     0.834
_reflns_Friedel_fraction_full    0.846

_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       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_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)+(0.0260P)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     SHELXL
_refine_ls_extinction_coef       0.00173(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 869 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.009(11)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2189
_refine_ls_number_parameters     104
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0283
_refine_ls_R_factor_gt           0.0256
_refine_ls_wR_factor_ref         0.0576
_refine_ls_wR_factor_gt          0.0569
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_restrained_S_all      1.004
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.08938(11) -0.00285(2) -0.00474(11) 0.03983(16) Uani 1 1 d . . . . .
Br1 Br 0.32296(14) 0.04930(8) 0.25800(15) 0.0537(4) Uani 1 1 d . . . . .
Br3 Br 0.08162(14) 0.13147(6) -0.19921(15) 0.0493(3) Uani 1 1 d . . . . .
Br2 Br -0.12861(16) 0.06258(9) 0.20095(16) 0.0642(4) Uani 1 1 d . . . . .
Cl1 Cl 0.0549(5) 0.2896(2) 0.5572(4) 0.0709(10) Uani 1 1 d . . . . .
C1 C 0.0252(17) 0.3706(8) 0.4295(16) 0.061(4) Uani 1 1 d . . . . .
H1A H -0.0766 0.3695 0.3777 0.073 Uiso 1 1 calc R U . . .
H1B H 0.0359 0.4152 0.4995 0.073 Uiso 1 1 calc R U . . .
N1 N 0.1056(11) 0.3203(6) 0.1569(12) 0.045(2) Uani 1 1 d . . . . .
C2 C 0.1270(16) 0.3790(7) 0.2950(15) 0.055(3) Uani 1 1 d . . . . .
H2A H 0.2289 0.3762 0.3456 0.065 Uiso 1 1 calc R U . . .
H2B H 0.1122 0.4288 0.2461 0.065 Uiso 1 1 calc R U . . .
C4 C 0.1865(17) 0.2480(9) 0.2036(18) 0.072(4) Uani 1 1 d . . . . .
H4A H 0.1359 0.2213 0.2838 0.108 Uiso 1 1 calc R U . . .
H4B H 0.2861 0.2593 0.2502 0.108 Uiso 1 1 calc R U . . .
H4C H 0.1894 0.2171 0.1067 0.108 Uiso 1 1 calc R U . . .
C3 C -0.0542(16) 0.3026(10) 0.1016(19) 0.076(4) Uani 1 1 d . . . . .
H3A H -0.1055 0.3484 0.0664 0.114 Uiso 1 1 calc R U . . .
H3B H -0.0995 0.2807 0.1920 0.114 Uiso 1 1 calc R U . . .
H3C H -0.0599 0.2675 0.0110 0.114 Uiso 1 1 calc R U . . .
C5 C 0.177(2) 0.3521(12) 0.0115(19) 0.089(6) Uani 1 1 d . . . . .
H5A H 0.1669 0.3164 -0.0782 0.133 Uiso 1 1 calc R U . . .
H5B H 0.2804 0.3614 0.0445 0.133 Uiso 1 1 calc R U . . .
H5C H 0.1288 0.3986 -0.0240 0.133 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 2.8474(12) . ?
Pb1 Br2 2.9565(15) . ?
Pb1 Br1 2.9806(17) . ?
Pb1 Br2 3.1121(18) 2_554 ?
Pb1 Br1 3.1219(15) 2_554 ?
Br1 Pb1 3.1219(15) 2 ?
Br2 Pb1 3.1121(18) 2 ?
Cl1 C1 1.770(14) . ?
C1 C2 1.511(17) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
N1 C3 1.500(18) . ?
N1 C4 1.501(17) . ?
N1 C5 1.514(16) . ?
N1 C2 1.523(15) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 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
Br3 Pb1 Br2 90.54(4) . . ?
Br3 Pb1 Br1 96.39(4) . . ?
Br2 Pb1 Br1 86.58(5) . . ?
Br3 Pb1 Br2 83.23(4) . 2_554 ?
Br2 Pb1 Br2 99.18(6) . 2_554 ?
Br1 Pb1 Br2 174.22(5) . 2_554 ?
Br3 Pb1 Br1 81.64(4) . 2_554 ?
Br2 Pb1 Br1 172.02(5) . 2_554 ?
Br1 Pb1 Br1 92.70(5) . 2_554 ?
Br2 Pb1 Br1 81.54(4) 2_554 2_554 ?
Pb1 Br1 Pb1 83.36(4) . 2 ?
Pb1 Br2 Pb1 83.93(4) . 2 ?
C2 C1 Cl1 115.9(10) . . ?
C2 C1 H1A 108.3 . . ?
Cl1 C1 H1A 108.3 . . ?
C2 C1 H1B 108.3 . . ?
Cl1 C1 H1B 108.3 . . ?
H1A C1 H1B 107.4 . . ?
C3 N1 C4 109.1(11) . . ?
C3 N1 C5 108.9(12) . . ?
C4 N1 C5 105.9(11) . . ?
C3 N1 C2 113.7(10) . . ?
C4 N1 C2 112.0(10) . . ?
C5 N1 C2 106.9(11) . . ?
C1 C2 N1 115.2(11) . . ?
C1 C2 H2A 108.5 . . ?
N1 C2 H2A 108.5 . . ?
C1 C2 H2B 108.5 . . ?
N1 C2 H2B 108.5 . . ?
H2A C2 H2B 107.5 . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N1 C3 H3A 109.5 . . ?
N1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N1 C5 H5A 109.5 . . ?
N1 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N1 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?

_refine_diff_density_max         0.793
_refine_diff_density_min         -0.745
_refine_diff_density_rms         0.131

_shelxl_version_number           2014-3

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 2189150'
loop_
_audit_author_name
_audit_author_address
'yan sui'
;School of Chemistry and Chemical Engineering, Jinggangshan University
China
;
_audit_update_record             
;
2022-07-09 deposited with the CCDC.	2022-09-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C5 H13 Br3 Cl N Pb'
_chemical_formula_sum            'C5 H13 Br3 Cl N Pb'
_chemical_formula_weight         569.53

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'C c'
_space_group_name_Hall           'C -2yc'

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

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

_cell_length_a                   9.0521(5)
_cell_length_b                   17.6601(11)
_cell_length_c                   8.1063(5)
_cell_angle_alpha                90
_cell_angle_beta                 96.332(6)
_cell_angle_gamma                90
_cell_volume                     1287.98(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    328.00(10)
_cell_measurement_reflns_used    1773
_cell_measurement_theta_min      4.6050
_cell_measurement_theta_max      4.6050

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.937
_exptl_crystal_F_000             1016
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    22.567
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.50546
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      328.00(10)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            2667
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         3.404
_diffrn_reflns_theta_max         25.498
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.686
_diffrn_reflns_point_group_measured_fraction_full 0.690
_reflns_number_total             1634
_reflns_number_gt                1563
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.369
_reflns_Friedel_fraction_max     0.371
_reflns_Friedel_fraction_full    0.379

_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       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_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)+(0.0252P)²+2.7775P] 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     SHELXL
_refine_ls_extinction_coef       0.00390(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 419 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.002(11)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1634
_refine_ls_number_parameters     104
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0260
_refine_ls_R_factor_gt           0.0242
_refine_ls_wR_factor_ref         0.0602
_refine_ls_wR_factor_gt          0.0597
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_restrained_S_all      1.122
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.95021(18) 0.06260(10) 0.80893(18) 0.0586(5) Uani 1 1 d . . . . .
Br2 Br 0.73964(16) -0.13145(7) 0.70912(16) 0.0448(4) Uani 1 1 d . . . . .
Br3 Br 0.49807(17) 0.04917(9) 0.75159(17) 0.0505(4) Uani 1 1 d . . . . .
C1 C 0.794(2) 0.6291(9) 0.079(2) 0.069(5) Uani 1 1 d . . . . .
H1A H 0.7809 0.5847 0.0085 0.083 Uiso 1 1 calc R U . . .
H1B H 0.8957 0.6292 0.1302 0.083 Uiso 1 1 calc R U . . .
C2 C 0.6916(17) 0.6218(7) 0.2150(16) 0.047(4) Uani 1 1 d . . . . .
H2A H 0.5896 0.6255 0.1646 0.056 Uiso 1 1 calc R U . . .
H2B H 0.7046 0.5717 0.2636 0.056 Uiso 1 1 calc R U . . .
C3 C 0.6456(19) 0.6470(11) 0.4975(18) 0.069(5) Uani 1 1 d . . . . .
H3A H 0.6936 0.6001 0.5305 0.103 Uiso 1 1 calc R U . . .
H3B H 0.5418 0.6381 0.4655 0.103 Uiso 1 1 calc R U . . .
H3C H 0.6572 0.6820 0.5886 0.103 Uiso 1 1 calc R U . . .
C4 C 0.8751(19) 0.6968(12) 0.408(2) 0.086(6) Uani 1 1 d . . . . .
H4A H 0.8815 0.7327 0.4971 0.129 Uiso 1 1 calc R U . . .
H4B H 0.9208 0.7177 0.3165 0.129 Uiso 1 1 calc R U . . .
H4C H 0.9255 0.6510 0.4447 0.129 Uiso 1 1 calc R U . . .
C5 C 0.6366(18) 0.7526(10) 0.3060(19) 0.063(4) Uani 1 1 d . . . . .
H5A H 0.5317 0.7435 0.2842 0.095 Uiso 1 1 calc R U . . .
H5B H 0.6730 0.7729 0.2083 0.095 Uiso 1 1 calc R U . . .
H5C H 0.6548 0.7882 0.3955 0.095 Uiso 1 1 calc R U . . .
Cl1 Cl 0.7656(5) 0.7102(3) -0.0467(5) 0.0678(12) Uani 1 1 d . . . . .
N1 N 0.7152(12) 0.6797(6) 0.3528(13) 0.040(3) Uani 1 1 d . . . . .
Pb1 Pb 0.73169(12) 0.00293(3) 0.51472(12) 0.03642(18) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 Pb1 2.9602(19) 2 ?
Br1 Pb1 3.1098(19) . ?
Br2 Pb1 2.8451(14) . ?
Br3 Pb1 2.9789(19) 2 ?
Br3 Pb1 3.1180(18) . ?
C1 C2 1.52(2) . ?
C1 Cl1 1.760(16) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N1 1.513(16) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 N1 1.506(18) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 N1 1.497(19) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 N1 1.499(18) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
Pb1 Br1 2.9602(19) 2_554 ?
Pb1 Br3 2.9788(19) 2_554 ?

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
Pb1 Br1 Pb1 83.78(5) 2 . ?
Pb1 Br3 Pb1 83.33(5) 2 . ?
C2 C1 Cl1 115.4(12) . . ?
C2 C1 H1A 108.4 . . ?
Cl1 C1 H1A 108.4 . . ?
C2 C1 H1B 108.4 . . ?
Cl1 C1 H1B 108.4 . . ?
H1A C1 H1B 107.5 . . ?
N1 C2 C1 115.5(12) . . ?
N1 C2 H2A 108.4 . . ?
C1 C2 H2A 108.4 . . ?
N1 C2 H2B 108.4 . . ?
C1 C2 H2B 108.4 . . ?
H2A C2 H2B 107.5 . . ?
N1 C3 H3A 109.5 . . ?
N1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N1 C5 H5A 109.5 . . ?
N1 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N1 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 N1 C5 108.5(12) . . ?
C4 N1 C3 108.6(12) . . ?
C5 N1 C3 107.4(12) . . ?
C4 N1 C2 114.1(12) . . ?
C5 N1 C2 111.7(10) . . ?
C3 N1 C2 106.2(11) . . ?
Br2 Pb1 Br1 90.48(5) . 2_554 ?
Br2 Pb1 Br3 96.41(5) . 2_554 ?
Br1 Pb1 Br3 86.64(5) 2_554 2_554 ?
Br2 Pb1 Br1 83.27(5) . . ?
Br1 Pb1 Br1 99.01(7) 2_554 . ?
Br3 Pb1 Br1 174.34(6) 2_554 . ?
Br2 Pb1 Br3 81.65(5) . . ?
Br1 Pb1 Br3 171.98(5) 2_554 . ?
Br3 Pb1 Br3 92.62(6) 2_554 . ?
Br1 Pb1 Br3 81.73(5) . . ?

_refine_diff_density_max         0.864
_refine_diff_density_min         -0.808
_refine_diff_density_rms         0.142

_shelxl_version_number           2014-3

####################################################################### 
# 
# 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_33
_database_code_depnum_ccdc_archive 'CCDC 2208090'
loop_
_audit_author_name
_audit_author_address
'yan sui'
;School of Chemistry and Chemical Engineering, Jinggangshan University
China
;
_audit_update_record             
;
2022-09-19 deposited with the CCDC.	2022-09-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H26 Br6 Cl2 N2 Pb2'
_chemical_formula_sum            'C10 H26 Br6 Cl2 N2 Pb2'
_chemical_formula_weight         1139.07

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'

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

_cell_length_a                   7.9300(7)
_cell_length_b                   17.238(2)
_cell_length_c                   9.7334(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1330.5(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    340(2)
_cell_measurement_reflns_used    1574
_cell_measurement_theta_min      4.1040
_cell_measurement_theta_max      17.3070

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.843
_exptl_crystal_F_000             1016
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    21.845
_shelx_estimated_absorpt_T_min   0.070
_shelx_estimated_absorpt_T_max   0.104
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.24206
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      340(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10745
_diffrn_reflns_av_unetI/netI     0.1751
_diffrn_reflns_av_R_equivalents  0.1180
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.491
_diffrn_reflns_theta_max         29.264
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.919
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.919
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3181
_reflns_number_gt                914
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.896
_reflns_Friedel_fraction_max     0.920
_reflns_Friedel_fraction_full    0.999

_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       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXL-2014 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'

_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)+(0.1139P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.24(13)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3181
_refine_ls_number_parameters     96
_refine_ls_number_restraints     33
_refine_ls_R_factor_all          0.3323
_refine_ls_R_factor_gt           0.1035
_refine_ls_wR_factor_ref         0.3304
_refine_ls_wR_factor_gt          0.2319
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.377
_refine_ls_shift/su_mean         0.027

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 1.05507(14) 0.24827(6) 0.8502(9) 0.1107(5) Uani 1 1 d . . . . .
Br3 Br 0.7917(6) 0.1842(4) 0.6473(6) 0.168(2) Uani 1 1 d . . . . .
Br1 Br 0.8302(5) 0.3827(2) 0.8585(12) 0.1579(15) Uani 1 1 d . . . . .
Br4 Br 0.8038(8) 0.1854(4) 1.0572(6) 0.184(3) Uani 1 1 d . . . . .
C5 C 0.7247(7) 0.9486(3) 0.7442(3) 0.19(2) Uiso 0.819(19) 1 d D . P A 1
N1 N 0.63657(17) 0.90579(10) 0.87119(12) 0.232(19) Uiso 0.819(19) 1 d D . P A 1
C1 C 0.8516(3) 0.85712(14) 0.9850(4) 0.9(2) Uiso 0.61(3) 1 d D . P A 1
C3 C 0.4425(2) 0.88139(17) 0.8580(3) 0.22(2) Uiso 0.819(19) 1 d D . P A 1
Cl1 Cl 0.9306(2) 0.9527(3) 0.9120(5) 0.87(7) Uiso 0.61(3) 1 d D . P A 1
C2 C 0.6614(3) 0.82913(14) 0.9616(3) 0.34(7) Uiso 0.61(3) 1 d D . P A 1
C4 C 0.6359(2) 0.96243(12) 1.0014(2) 0.33(5) Uiso 0.819(19) 1 d D . P A 1
C5A C 0.655(6) 0.913(2) 0.694(2) 0.09(5) Uiso 0.181(19) 1 d D . P A 2
N1A N 0.5881(19) 0.8771(10) 0.8348(15) 0.7(4) Uiso 0.181(19) 1 d D . P A 2
C3A C 0.442(3) 0.8132(15) 0.827(5) 0.08(4) Uiso 0.181(19) 1 d D . P A 2
C4A C 0.507(5) 0.9422(13) 0.932(3) -0.001(19) Uiso 0.181(19) 1 d D . P A 2
Cl1A Cl 1.036(4) 0.9753(13) 0.886(6) 0.35(3) Uiso 0.39(3) 1 d D . P A 2
C1A C 0.896(3) 0.8882(15) 0.926(3) 0.7(2) Uiso 0.39(3) 1 d D . P A 2
C2A C 0.7782(19) 0.8498(14) 0.811(3) 0.13(3) Uiso 0.39(3) 1 d D . P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br1 2.925(4) . ?
Pb1 Br3 2.962(8) 3 ?
Pb1 Br4 3.034(8) . ?
Pb1 Br4 3.042(8) 3 ?
Pb1 Br3 3.079(7) . ?
Pb1 Br1 3.141(4) 3 ?
Br3 Pb1 2.962(8) 3_455 ?
Br1 Pb1 3.140(4) 3_455 ?
Br4 Pb1 3.042(8) 3_455 ?
C5 N1 1.600(2) . ?
N1 C2 1.600(2) . ?
N1 C4 1.6001(19) . ?
N1 C3 1.6002(18) . ?
C1 C2 1.600(3) . ?
C1 Cl1 1.901(5) . ?
C5A N1A 1.60(2) . ?
N1A C2A 1.596(19) . ?
N1A C3A 1.60(2) . ?
N1A C4A 1.60(2) . ?
Cl1A C1A 1.90(2) . ?
C1A C2A 1.60(2) . ?

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 Br3 95.4(2) . 3 ?
Br1 Pb1 Br4 82.2(2) . . ?
Br3 Pb1 Br4 177.54(19) 3 . ?
Br1 Pb1 Br4 94.6(2) . 3 ?
Br3 Pb1 Br4 83.30(14) 3 3 ?
Br4 Pb1 Br4 96.9(3) . 3 ?
Br1 Pb1 Br3 83.6(2) . . ?
Br3 Pb1 Br3 98.2(3) 3 . ?
Br4 Pb1 Br3 81.52(14) . . ?
Br4 Pb1 Br3 177.7(2) 3 . ?
Br1 Pb1 Br1 172.9(2) . 3 ?
Br3 Pb1 Br1 81.9(2) 3 3 ?
Br4 Pb1 Br1 100.5(2) . 3 ?
Br4 Pb1 Br1 78.62(19) 3 3 ?
Br3 Pb1 Br1 103.3(2) . 3 ?
Pb1 Br3 Pb1 82.0(2) 3_455 . ?
Pb1 Br1 Pb1 81.57(9) . 3_455 ?
Pb1 Br4 Pb1 81.5(2) . 3_455 ?
C2 N1 C4 93.93(16) . . ?
C2 N1 C5 138.8(3) . . ?
C4 N1 C5 109.4(2) . . ?
C2 N1 C3 86.86(13) . . ?
C4 N1 C3 102.73(13) . . ?
C5 N1 C3 118.6(2) . . ?
C2 C1 Cl1 121.26(16) . . ?
N1 C2 C1 86.85(15) . . ?
C2A N1A C5A 71(2) . . ?
C2A N1A C3A 118.2(18) . . ?
C5A N1A C3A 118(2) . . ?
C2A N1A C4A 132.0(19) . . ?
C5A N1A C4A 111.4(19) . . ?
C3A N1A C4A 102.8(18) . . ?
C2A C1A Cl1A 122(2) . . ?
C1A C2A N1A 109.4(15) . . ?

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
C4_a N1_a C2_a C1_a -73.12(19) . . . . ?
C5 N1 C2 C1 52.6(4) . . . . ?
C3 N1 C2 C1 -175.7(2) . . . . ?
Cl1 C1 C2 N1 2.5(3) . . . . ?
Cl1A C1A C2A N1A -102(2) . . . . ?
C5A N1A C2A C1A 113(2) . . . . ?
C3A N1A C2A C1A -135(2) . . . . ?
C4A N1A C2A C1A 10(3) . . . . ?

_refine_diff_density_max         2.921
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.207

_shelxl_version_number           2014-3

