# Supplementary Information (SI) for Journal of Materials Chemistry A.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_shs241m
_audit_block_doi                 10.5517/ccdc.csd.cc1nvx3j
_database_code_depnum_ccdc_archive 'CCDC 1545198'
_audit_update_record             
;
2017-04-21 deposited with the CCDC.	2024-07-25 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H28 Br6 N4 Sn'
_chemical_formula_iupac          ?
_chemical_formula_weight         874.57

_chemical_melting_point          ?

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.7578(3)
_cell_length_b                   14.4697(4)
_cell_length_c                   8.5380(3)
_cell_angle_alpha                90
_cell_angle_beta                 103.5453(14)
_cell_angle_gamma                90
_cell_volume                     1292.08(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5322
_cell_measurement_theta_min      2.4028
_cell_measurement_theta_max      30.9005
_cell_measurement_temperature    296.(2)

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_exptl_crystal_density_diffrn    2.248
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             824

_exptl_absorpt_coefficient_mu    10.276
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min  0.44
_exptl_absorpt_correction_T_max  0.68

_exptl_special_details           
;
;

_diffrn_ambient_temperature      296.(2)

_diffrn_source                   'Incoatec microfocus source'
_diffrn_source_type              'Bruker D8 Quest'

_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'Multilayer Mirror'

_diffrn_measurement_device_type  'Photon II CPADs detector'
_diffrn_measurement_method       'phi and omega scans'

_diffrn_detector_area_resol_mean 7.4074

_diffrn_reflns_number            13894
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_theta_min         2.40
_diffrn_reflns_theta_max         31.00
_diffrn_reflns_theta_full        31.00
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12

_refine_special_details          
;
;

_reflns_number_total             4094
_reflns_number_gt                3340
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0281
_refine_ls_wR_factor_gt          0.0575
_refine_ls_wR_factor_ref         0.0605
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_refine_ls_number_reflns         4094
_refine_ls_number_parameters     126
_refine_ls_number_restraints     0
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0225P)²+0.8043P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.044
_refine_diff_density_min         -0.977
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_computing_data_collection       ?
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_solution    'XS, VERSION 2013/1'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br Br1 0.75535(3) 0.02366(2) 0.24581(4) 0.03839(8) Uani d . . . 1 . .
Br Br2 1.05342(3) 0.18743(2) 0.38801(4) 0.03609(8) Uani d . . . 1 . .
Br Br3 0.88715(3) 0.07264(2) 0.76512(4) 0.03891(8) Uani d . . . 1 . .
C C1 0.4193(2) 0.74747(19) 0.9931(3) 0.0298(5) Uani d . . . 1 . .
C C2 0.4475(3) 0.6565(2) 0.9677(3) 0.0345(6) Uani d . . . 1 . .
H H2 0.3973 0.6094 0.9943 0.041 Uiso calc U . R 1 . .
C C3 0.5505(3) 0.6351(2) 0.9025(4) 0.0405(7) Uani d . . . 1 . .
H H3 0.5688 0.5737 0.8853 0.049 Uiso calc U . R 1 . .
C C4 0.6256(2) 0.7042(2) 0.8632(3) 0.0357(6) Uani d . . . 1 . .
H H4 0.6947 0.6892 0.8199 0.043 Uiso calc U . R 1 . .
C C5 0.5987(2) 0.7966(2) 0.8880(3) 0.0311(5) Uani d . . . 1 . .
C C6 0.4960(2) 0.81724(19) 0.9541(3) 0.0304(5) Uani d . . . 1 . .
H H6 0.4781 0.8786 0.9727 0.036 Uiso calc U . R 1 . .
C C7 0.3075(2) 0.7696(2) 1.0654(3) 0.0378(6) Uani d . . . 1 . .
H H7A 0.2987 0.721 1.1404 0.045 Uiso calc U . R 1 . .
H H7B 0.3247 0.8269 1.1255 0.045 Uiso calc U . R 1 . .
C C8 0.6781(3) 0.8717(2) 0.8385(4) 0.0422(7) Uani d . . . 1 . .
H H8A 0.6917 0.8571 0.7329 0.051 Uiso calc U . R 1 . .
H H8B 0.6311 0.9294 0.8297 0.051 Uiso calc U . R 1 . .
N N1 0.18559(19) 0.77873(16) 0.9421(3) 0.0307(5) Uani d . . . 1 . .
H H1A 0.1891 0.8283 0.8816 0.046 Uiso calc U . R 1 . .
H H1B 0.1213 0.7848 0.9906 0.046 Uiso calc U . R 1 . .
H H1C 0.1732 0.7285 0.8802 0.046 Uiso calc U . R 1 . .
N N2 0.8046(2) 0.88440(16) 0.9531(3) 0.0365(5) Uani d . . . 1 . .
H H2A 0.7938 0.9118 1.0423 0.055 Uiso calc U . R 1 . .
H H2B 0.8543 0.9195 0.9075 0.055 Uiso calc U . R 1 . .
H H2C 0.8415 0.8296 0.9779 0.055 Uiso calc U . R 1 . .
Sn Sn1 1.0 0 0.5 0.02449(6) Uani d . P S 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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Br1 Sn1 . 3.0131(3) ?
Br2 Sn1 . 2.9761(3) ?
Br3 Sn1 . 2.9983(3) ?
C1 C2 . 1.379(4) ?
C1 C6 . 1.393(4) ?
C1 C7 . 1.509(3) ?
C2 C3 . 1.386(4) ?
C3 C4 . 1.376(4) ?
C4 C5 . 1.395(4) ?
C5 C6 . 1.385(4) ?
C5 C8 . 1.503(4) ?
C7 N1 . 1.483(3) ?
C8 N2 . 1.490(4) ?
Sn1 Br2 3_756 2.9761(3) ?
Sn1 Br3 3_756 2.9983(3) ?
Sn1 Br1 3_756 3.0130(3) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 C1 C6 . . 119.3(2) ?
C2 C1 C7 . . 119.5(3) ?
C6 C1 C7 . . 121.2(2) ?
C1 C2 C3 . . 120.2(3) ?
C4 C3 C2 . . 120.4(3) ?
C3 C4 C5 . . 120.3(2) ?
C6 C5 C4 . . 118.9(3) ?
C6 C5 C8 . . 121.2(3) ?
C4 C5 C8 . . 119.9(2) ?
C5 C6 C1 . . 121.0(3) ?
N1 C7 C1 . . 112.7(2) ?
N2 C8 C5 . . 113.4(2) ?
Br2 Sn1 Br2 3_756 . 180.0 ?
Br2 Sn1 Br3 3_756 . 86.221(8) ?
Br2 Sn1 Br3 . . 93.779(8) ?
Br2 Sn1 Br3 3_756 3_756 93.779(8) ?
Br2 Sn1 Br3 . 3_756 86.221(8) ?
Br3 Sn1 Br3 . 3_756 180.0 ?
Br2 Sn1 Br1 3_756 3_756 82.349(8) ?
Br2 Sn1 Br1 . 3_756 97.651(8) ?
Br3 Sn1 Br1 . 3_756 86.321(9) ?
Br3 Sn1 Br1 3_756 3_756 93.678(9) ?
Br2 Sn1 Br1 3_756 . 97.652(8) ?
Br2 Sn1 Br1 . . 82.348(8) ?
Br3 Sn1 Br1 . . 93.678(9) ?
Br3 Sn1 Br1 3_756 . 86.323(9) ?
Br1 Sn1 Br1 3_756 . 180.0 ?



####################################################################### 
# 
# 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_phan_PAP_2
_database_code_depnum_ccdc_archive 'CCDC 2300669'
loop_
_audit_author_name
_audit_author_address
'Yongxin Li'
;Nanyang Technological University
Singapore
;
_audit_update_record             
;
2023-10-11 deposited with the CCDC.	2024-07-25 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H14 Br4 N2 Pb'
_chemical_formula_iupac          ?
_chemical_formula_weight         665.04

_chemical_melting_point          ?

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.340(3)
_cell_length_b                   8.1590(15)
_cell_length_c                   8.1725(19)
_cell_angle_alpha                90
_cell_angle_beta                 90.930(10)
_cell_angle_gamma                90
_cell_volume                     822.7(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3597
_cell_measurement_theta_min      2.9932
_cell_measurement_theta_max      32.2902
_cell_measurement_temperature    296.(2)

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_exptl_crystal_density_diffrn    2.685
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             596

_exptl_absorpt_coefficient_mu    19.944
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_absorpt_correction_T_min  0.15
_exptl_absorpt_correction_T_max  0.69

_exptl_special_details           
;
;

_diffrn_ambient_temperature      296.(2)

_diffrn_source                   'Incoatec microfocus source'
_diffrn_source_type              'Bruker D8 Quest'
_diffrn_source_power             0.07
_diffrn_source_current           1.4
_diffrn_source_voltage           50

_diffrn_radiation_probe          X-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'Multilayer Mirror'

_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Photon II CPAD detector'
_diffrn_measurement_method       'phi and omega scans'

_diffrn_detector_area_resol_mean 7.3910

_diffrn_reflns_number            13687
_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_av_unetI/netI     0.0518
_diffrn_reflns_theta_min         2.99
_diffrn_reflns_theta_max         33.71
_diffrn_reflns_theta_full        25.24
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12

_reflns_number_total             3280
_reflns_number_gt                2179
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0707
_refine_ls_R_factor_gt           0.0379
_refine_ls_wR_factor_gt          0.0746
_refine_ls_wR_factor_ref         0.0867
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_restrained_S_all      0.986
_refine_ls_number_reflns         3280
_refine_ls_number_parameters     71
_refine_ls_number_restraints     0
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0322P)²] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.099
_refine_diff_density_min         -0.855
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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'

_computing_data_collection       'APEX4 (Ver 2021.4-0, Bruker AXS Inc., 2021)'
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_structure_solution    'XT, VERSION 2018/2'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  'APEX4 (Ver 2021.4-0, Bruker AXS Inc., 2021)'

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br Br1 0.50038(5) 0.68333(6) 0.81624(7) 0.05220(15) Uani d . . . 1 . .
Br Br2 0.25628(5) 0.52304(7) 0.47993(8) 0.05507(15) Uani d . . . 1 . .
C C1 0.2314(5) 0.4595(8) -0.0364(9) 0.0660(17) Uani d . . . 1 . .
H H1A 0.252536 0.347983 -0.009811 0.079000 Uiso calc U . R 1 . .
H H1B 0.250203 0.480359 -0.149294 0.079000 Uiso calc U . R 1 . .
C C2 0.1116(5) 0.4779(7) -0.0173(8) 0.0590(15) Uani d . . . 1 . .
C C3 0.0572(6) 0.3936(10) 0.0955(10) 0.086(2) Uani d . . . 1 . .
H H3 0.094396 0.319384 0.162025 0.103000 Uiso calc U . R 1 . .
C C4 0.0546(6) 0.5855(11) -0.1157(10) 0.088(2) Uani d . . . 1 . .
H H4 0.090264 0.644482 -0.195934 0.106000 Uiso calc U . R 1 . .
N N1 0.2907(4) 0.5750(6) 0.0721(6) 0.0548(12) Uani d . . . 1 . .
H H1C 0.270812 0.677245 0.048319 0.082000 Uiso calc U . R 1 . .
H H1D 0.361680 0.564103 0.057438 0.082000 Uiso calc U . R 1 . .
H H1E 0.275419 0.553276 0.175945 0.082000 Uiso calc U . R 1 . .
Pb Pb1 0.500000 0.500000 0.500000 0.03972(9) Uani d . P S 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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Br1 Pb1 . 2.9861(7) ?
Br1 Pb1 2_656 2.9885(7) ?
Br2 Pb1 . 3.0151(10) ?
C1 N1 . 1.481(8) ?
C1 C2 . 1.496(9) ?
C2 C3 . 1.340(10) ?
C2 C4 . 1.376(9) ?
C3 C4 3_565 1.402(10) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Pb1 Br1 Pb1 . 2_656 150.23(2) ?
N1 C1 C2 . . 110.7(5) ?
C3 C2 C4 . . 118.1(6) ?
C3 C2 C1 . . 121.8(6) ?
C4 C2 C1 . . 120.0(6) ?
C2 C3 C4 . 3_565 121.6(7) ?
C2 C4 C3 . 3_565 120.3(6) ?
Br1 Pb1 Br1 . 3_666 180.000000 ?
Br1 Pb1 Br1 . 4_575 90.106(15) ?
Br1 Pb1 Br1 3_666 4_575 89.893(16) ?
Br1 Pb1 Br1 . 2_646 89.894(15) ?
Br1 Pb1 Br1 3_666 2_646 90.107(16) ?
Br1 Pb1 Br1 4_575 2_646 180.000000 ?
Br1 Pb1 Br2 . . 90.196(19) ?
Br1 Pb1 Br2 3_666 . 89.805(19) ?
Br1 Pb1 Br2 4_575 . 85.898(17) ?
Br1 Pb1 Br2 2_646 . 94.102(17) ?
Br1 Pb1 Br2 . 3_666 89.804(19) ?
Br1 Pb1 Br2 3_666 3_666 90.195(19) ?
Br1 Pb1 Br2 4_575 3_666 94.102(17) ?
Br1 Pb1 Br2 2_646 3_666 85.898(17) ?
Br2 Pb1 Br2 . 3_666 180.00(2) ?



####################################################################### 
# 
# 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_szx_PAP_41m
_database_code_depnum_ccdc_archive 'CCDC 2350304'
loop_
_audit_author_name
_audit_author_address
'Yongxin Li'
;Nanyang Technological University
Singapore
;
_audit_update_record             
;
2024-04-23 deposited with the CCDC.	2024-07-25 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H28 Cl6 N4 Pb'
_chemical_formula_iupac          ?
_chemical_formula_weight         696.31

_chemical_melting_point          ?

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.5772(11)
_cell_length_b                   13.8645(16)
_cell_length_c                   8.2791(9)
_cell_angle_alpha                90
_cell_angle_beta                 102.816(4)
_cell_angle_gamma                90
_cell_volume                     1183.9(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9953
_cell_measurement_theta_min      2.4613
_cell_measurement_theta_max      25.3785
_cell_measurement_temperature    100.(2)

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.005
_exptl_crystal_density_diffrn    1.953
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             672

_exptl_absorpt_coefficient_mu    7.813
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_absorpt_correction_T_min  0.21
_exptl_absorpt_correction_T_max  0.96

_exptl_special_details           
;
;

_diffrn_ambient_temperature      100.(2)

_diffrn_source                   'Incoatec microfocus source'
_diffrn_source_type              'Bruker D8 Quest'
_diffrn_source_power             0.07
_diffrn_source_current           1.4
_diffrn_source_voltage           50

_diffrn_radiation_probe          X-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'Multilayer Mirror'

_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Photon II CPADs detector'
_diffrn_measurement_method       'phi and omega scans'

_diffrn_detector_area_resol_mean 7.3910

_diffrn_reflns_number            16772
_diffrn_reflns_av_R_equivalents  0.0859
_diffrn_reflns_av_unetI/netI     0.0462
_diffrn_reflns_theta_min         2.46
_diffrn_reflns_theta_max         25.38
_diffrn_reflns_theta_full        25.24
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9

_refine_special_details          
;
;

_reflns_number_total             2166
_reflns_number_gt                1953
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0388
_refine_ls_wR_factor_gt          0.1091
_refine_ls_wR_factor_ref         0.1134
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.059
_refine_ls_number_reflns         2166
_refine_ls_number_parameters     126
_refine_ls_number_restraints     0
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0766P)²+1.5597P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.519
_refine_diff_density_min         -1.792
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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'

_computing_data_collection       'APEX4 (Ver 2021.4-0, Bruker AXS Inc., 2021)'
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_structure_solution    'XT, VERSION 2018/2'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 1242)'
_computing_publication_material  'APEX4 (Ver 2021.4-0, Bruker AXS Inc., 2021)'

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C C1 0.4011(5) 0.7968(4) 0.6186(7) 0.0287(12) Uani d . . . 1 . .
C C2 0.3727(5) 0.7008(4) 0.6440(7) 0.0299(12) Uani d . . . 1 . .
H H2 0.299626 0.685331 0.688148 0.036000 Uiso calc U . R 1 . .
C C3 0.4502(5) 0.6274(4) 0.6055(7) 0.0310(13) Uani d . . . 1 . .
H H3 0.430113 0.561902 0.622693 0.037000 Uiso calc U . R 1 . .
C C4 0.5573(6) 0.6502(4) 0.5417(7) 0.0314(13) Uani d . . . 1 . .
H H4 0.610277 0.600091 0.514803 0.038000 Uiso calc U . R 1 . .
C C5 0.5876(5) 0.7460(4) 0.5168(6) 0.0267(12) Uani d . . . 1 . .
C C6 0.5080(5) 0.8195(4) 0.5548(7) 0.0274(12) Uani d . . . 1 . .
H H6 0.527430 0.885009 0.536831 0.033000 Uiso calc U . R 1 . .
C C7 0.3170(5) 0.8759(4) 0.6668(7) 0.0309(12) Uani d . . . 1 . .
H H7A 0.297393 0.859742 0.775151 0.037000 Uiso calc U . R 1 . .
H H7B 0.365815 0.937364 0.679677 0.037000 Uiso calc U . R 1 . .
C C8 0.7024(5) 0.7683(4) 0.4422(7) 0.0289(12) Uani d . . . 1 . .
H H8A 0.711990 0.716315 0.363826 0.035000 Uiso calc U . R 1 . .
H H8B 0.685828 0.829282 0.378863 0.035000 Uiso calc U . R 1 . .
Cl Cl1 0.10667(11) 0.42730(8) 0.22824(14) 0.0199(3) Uani d . . . 1 . .
Cl Cl2 0.05644(11) 0.69079(8) 0.39330(14) 0.0213(3) Uani d . . . 1 . .
Cl Cl3 0.23793(13) 0.47288(11) 0.75136(16) 0.0233(3) Uani d . . . 1 . .
N N1 0.1927(4) 0.8891(4) 0.5418(6) 0.0308(11) Uani d . . . 1 . .
H H1A 0.209239 0.916240 0.448503 0.046000 Uiso calc U . R 1 . .
H H1B 0.139177 0.928418 0.584156 0.046000 Uiso calc U . R 1 . .
H H1C 0.153861 0.830816 0.516435 0.046000 Uiso calc U . R 1 . .
N N2 0.8259(4) 0.7775(3) 0.5700(6) 0.0270(10) Uani d . . . 1 . .
H H2A 0.822575 0.831279 0.632066 0.040000 Uiso calc U . R 1 . .
H H2B 0.893611 0.782361 0.519251 0.040000 Uiso calc U . R 1 . .
H H2C 0.836706 0.724614 0.636689 0.040000 Uiso calc U . R 1 . .
Pb Pb1 0.000000 0.500000 0.500000 0.02428(17) Uani d . P S 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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 C6 . 1.386(8) ?
C1 C2 . 1.391(9) ?
C1 C7 . 1.520(8) ?
C2 C3 . 1.387(8) ?
C3 C4 . 1.388(8) ?
C4 C5 . 1.392(8) ?
C5 C6 . 1.401(8) ?
C5 C8 . 1.512(8) ?
C7 N1 . 1.493(7) ?
C8 N2 . 1.492(7) ?
Cl1 Pb1 . 2.9116(11) ?
Cl2 Pb1 . 2.8927(12) ?
Cl3 Pb1 . 2.9124(13) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C6 C1 C2 . . 119.8(6) ?
C6 C1 C7 . . 120.7(5) ?
C2 C1 C7 . . 119.5(5) ?
C3 C2 C1 . . 120.6(5) ?
C2 C3 C4 . . 119.5(6) ?
C3 C4 C5 . . 120.5(6) ?
C4 C5 C6 . . 119.4(5) ?
C4 C5 C8 . . 119.2(5) ?
C6 C5 C8 . . 121.3(5) ?
C1 C6 C5 . . 120.1(5) ?
N1 C7 C1 . . 112.6(4) ?
N2 C8 C5 . . 112.6(4) ?
Cl2 Pb1 Cl2 3_566 . 180.000000 ?
Cl2 Pb1 Cl1 3_566 3_566 86.50(3) ?
Cl2 Pb1 Cl1 . 3_566 93.50(3) ?
Cl2 Pb1 Cl1 3_566 . 93.50(3) ?
Cl2 Pb1 Cl1 . . 86.50(3) ?
Cl1 Pb1 Cl1 3_566 . 180.000000 ?
Cl2 Pb1 Cl3 3_566 . 82.41(4) ?
Cl2 Pb1 Cl3 . . 97.59(4) ?
Cl1 Pb1 Cl3 3_566 . 85.07(4) ?
Cl1 Pb1 Cl3 . . 94.93(4) ?
Cl2 Pb1 Cl3 3_566 3_566 97.59(4) ?
Cl2 Pb1 Cl3 . 3_566 82.41(4) ?
Cl1 Pb1 Cl3 3_566 3_566 94.93(4) ?
Cl1 Pb1 Cl3 . 3_566 85.07(4) ?
Cl3 Pb1 Cl3 . 3_566 180.00(4) ?



####################################################################### 
# 
# 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_shs308m
_database_code_depnum_ccdc_archive 'CCDC 2300668'
loop_
_audit_author_name
_audit_author_address
'Yongxin Li'
;Nanyang Technological University
Singapore
;
_audit_update_record             
;
2023-10-11 deposited with the CCDC.	2024-07-25 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H28 Cl6 N4 Sn'
_chemical_formula_iupac          ?
_chemical_formula_weight         607.81

_chemical_melting_point          ?

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.5583(3)
_cell_length_b                   13.7185(4)
_cell_length_c                   8.2248(3)
_cell_angle_alpha                90
_cell_angle_beta                 102.5760(10)
_cell_angle_gamma                90
_cell_volume                     1162.73(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9901
_cell_measurement_theta_min      2.4719
_cell_measurement_theta_max      36.4109
_cell_measurement_temperature    100.(2)

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.120
_exptl_crystal_density_diffrn    1.736
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             608

_exptl_absorpt_coefficient_mu    1.799
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min  0.67
_exptl_absorpt_correction_T_max  0.81

_exptl_special_details           
;
;

_diffrn_ambient_temperature      100.(2)

_diffrn_source                   'Incoatec microfocus source'
_diffrn_source_type              'Bruker D8 Quest'

_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'Multilayer Mirror'

_diffrn_measurement_device_type  'Photon II CPADs detector'
_diffrn_measurement_method       'phi and omega scans'

_diffrn_detector_area_resol_mean 7.4074

_diffrn_reflns_number            29976
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_theta_min         2.47
_diffrn_reflns_theta_max         36.41
_diffrn_reflns_theta_full        36.41
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       13

_refine_special_details          
;
;

_reflns_number_total             5644
_reflns_number_gt                5087
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0229
_refine_ls_wR_factor_gt          0.0489
_refine_ls_wR_factor_ref         0.0510
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_restrained_S_all      1.088
_refine_ls_number_reflns         5644
_refine_ls_number_parameters     126
_refine_ls_number_restraints     0
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0151P)²+0.3581P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.546
_refine_diff_density_min         -0.929
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_computing_data_collection       'APEX3 (Bruker AXS Inc., 2017)'
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_structure_solution    'XT, VERSION 2014/5'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'XP (Bruker AXS Inc., 2017)'
_computing_publication_material  'APEX3 (Bruker AXS Inc., 2017)'

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C C1 0.31666(11) 0.37770(9) 0.16646(15) 0.01456(19) Uani d . . . 1 . .
H H1A 0.297902 0.362326 0.276449 0.017 Uiso calc U . R 1 . .
H H1B 0.364607 0.440208 0.176802 0.017 Uiso calc U . R 1 . .
C C2 0.40092(10) 0.29855(8) 0.11962(13) 0.01125(17) Uani d . . . 1 . .
C C3 0.37285(11) 0.20106(9) 0.14479(14) 0.01299(18) Uani d . . . 1 . .
H H3 0.298888 0.184955 0.187616 0.016 Uiso calc U . R 1 . .
C C4 0.45217(11) 0.12742(8) 0.10774(15) 0.01386(19) Uani d . . . 1 . .
H H4 0.432456 0.061235 0.125578 0.017 Uiso calc U . R 1 . .
C C5 0.56024(11) 0.15025(8) 0.04469(14) 0.01276(18) Uani d . . . 1 . .
H H5 0.614257 0.099605 0.019472 0.015 Uiso calc U . R 1 . .
C C6 0.58986(10) 0.24733(8) 0.01820(13) 0.01110(17) Uani d . . . 1 . .
C C7 0.50929(10) 0.32099(8) 0.05562(14) 0.01156(17) Uani d . . . 1 . .
H H7 0.528623 0.387174 0.03722 0.014 Uiso calc U . R 1 . .
C C8 0.70462(11) 0.27019(9) -0.05524(14) 0.01346(19) Uani d . . . 1 . .
H H8A 0.713172 0.218877 -0.136806 0.016 Uiso calc U . R 1 . .
H H8B 0.689073 0.332865 -0.115975 0.016 Uiso calc U . R 1 . .
Cl Cl1 0.10232(3) 0.57261(2) 0.22888(4) 0.01544(5) Uani d . . . 1 . .
Cl Cl2 -0.05668(3) 0.68873(2) 0.60364(4) 0.01362(5) Uani d . . . 1 . .
Cl Cl3 0.23397(3) 0.52703(2) 0.74641(4) 0.01469(5) Uani d . . . 1 . .
N N1 0.19125(10) 0.38917(7) 0.04140(13) 0.01299(17) Uani d . . . 1 . .
H H1C 0.206503 0.418107 -0.052044 0.019 Uiso calc U . R 1 . .
H H1D 0.136131 0.426861 0.085311 0.019 Uiso calc U . R 1 . .
H H1E 0.154925 0.329501 0.014942 0.019 Uiso calc U . R 1 . .
N N2 0.82899(9) 0.27692(7) 0.07273(12) 0.01121(15) Uani d . . . 1 . .
H H2A 0.826627 0.330021 0.138317 0.017 Uiso calc U . R 1 . .
H H2B 0.896522 0.282672 0.020967 0.017 Uiso calc U . R 1 . .
H H2C 0.839449 0.222172 0.136724 0.017 Uiso calc U . R 1 . .
Sn Sn1 0 0.5 0.5 0.00816(3) Uani d . P S 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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 N1 . 1.4977(14) ?
C1 C2 . 1.5060(17) ?
C1 H1A . 0.99 ?
C1 H1B . 0.99 ?
C2 C7 . 1.3940(17) ?
C2 C3 . 1.3951(16) ?
C3 C4 . 1.3877(17) ?
C3 H3 . 0.95 ?
C4 C5 . 1.3880(18) ?
C4 H4 . 0.95 ?
C5 C6 . 1.3959(16) ?
C5 H5 . 0.95 ?
C6 C7 . 1.3977(16) ?
C6 C8 . 1.5001(17) ?
C7 H7 . 0.95 ?
C8 N2 . 1.4962(14) ?
C8 H8A . 0.99 ?
C8 H8B . 0.99 ?
Cl1 Sn1 . 2.8602(3) ?
Cl2 Sn1 . 2.8302(3) ?
Cl3 Sn1 . 2.8578(3) ?
N1 H1C . 0.91 ?
N1 H1D . 0.91 ?
N1 H1E . 0.91 ?
N2 H2A . 0.91 ?
N2 H2B . 0.91 ?
N2 H2C . 0.91 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 C1 C2 . . 112.53(9) ?
N1 C1 H1A . . 109.1 ?
C2 C1 H1A . . 109.1 ?
N1 C1 H1B . . 109.1 ?
C2 C1 H1B . . 109.1 ?
H1A C1 H1B . . 107.8 ?
C7 C2 C3 . . 119.08(11) ?
C7 C2 C1 . . 121.10(10) ?
C3 C2 C1 . . 119.79(11) ?
C4 C3 C2 . . 120.50(11) ?
C4 C3 H3 . . 119.8 ?
C2 C3 H3 . . 119.8 ?
C5 C4 C3 . . 120.15(11) ?
C5 C4 H4 . . 119.9 ?
C3 C4 H4 . . 119.9 ?
C4 C5 C6 . . 120.26(11) ?
C4 C5 H5 . . 119.9 ?
C6 C5 H5 . . 119.9 ?
C5 C6 C7 . . 119.18(11) ?
C5 C6 C8 . . 119.37(11) ?
C7 C6 C8 . . 121.42(10) ?
C2 C7 C6 . . 120.83(10) ?
C2 C7 H7 . . 119.6 ?
C6 C7 H7 . . 119.6 ?
N2 C8 C6 . . 113.07(9) ?
N2 C8 H8A . . 109.0 ?
C6 C8 H8A . . 109.0 ?
N2 C8 H8B . . 109.0 ?
C6 C8 H8B . . 109.0 ?
H8A C8 H8B . . 107.8 ?
C1 N1 H1C . . 109.5 ?
C1 N1 H1D . . 109.5 ?
H1C N1 H1D . . 109.5 ?
C1 N1 H1E . . 109.5 ?
H1C N1 H1E . . 109.5 ?
H1D N1 H1E . . 109.5 ?
C8 N2 H2A . . 109.5 ?
C8 N2 H2B . . 109.5 ?
H2A N2 H2B . . 109.5 ?
C8 N2 H2C . . 109.5 ?
H2A N2 H2C . . 109.5 ?
H2B N2 H2C . . 109.5 ?
Cl2 Sn1 Cl2 . 3_566 180.0 ?
Cl2 Sn1 Cl3 . . 82.792(8) ?
Cl2 Sn1 Cl3 3_566 . 97.209(8) ?
Cl2 Sn1 Cl3 . 3_566 97.207(8) ?
Cl2 Sn1 Cl3 3_566 3_566 82.792(8) ?
Cl3 Sn1 Cl3 . 3_566 180.0 ?
Cl2 Sn1 Cl1 . . 93.253(9) ?
Cl2 Sn1 Cl1 3_566 . 86.747(8) ?
Cl3 Sn1 Cl1 . . 95.323(9) ?
Cl3 Sn1 Cl1 3_566 . 84.677(9) ?
Cl2 Sn1 Cl1 . 3_566 86.747(8) ?
Cl2 Sn1 Cl1 3_566 3_566 93.253(9) ?
Cl3 Sn1 Cl1 . 3_566 84.677(9) ?
Cl3 Sn1 Cl1 3_566 3_566 95.323(9) ?
Cl1 Sn1 Cl1 . 3_566 180.000(12) ?



####################################################################### 
# 
# 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_szx_PAP_22m
_database_code_depnum_ccdc_archive 'CCDC 2300671'
loop_
_audit_author_name
_audit_author_address
'Yongxin Li'
;Nanyang Technological University
Singapore
;
_audit_update_record             
;
2023-10-11 deposited with the CCDC.	2024-07-25 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H28 Br8 N4 Pb2'
_chemical_formula_iupac          ?
_chemical_formula_weight         1330.08

_chemical_melting_point          ?

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   14.3412(9)
_cell_length_b                   25.4991(18)
_cell_length_c                   8.1894(6)
_cell_angle_alpha                90
_cell_angle_beta                 94.616(3)
_cell_angle_gamma                90
_cell_volume                     2985.0(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9951
_cell_measurement_theta_min      2.6199
_cell_measurement_theta_max      27.8709
_cell_measurement_temperature    100.(2)

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_exptl_crystal_density_diffrn    2.960
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2384

_exptl_absorpt_coefficient_mu    21.987
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_absorpt_correction_T_min  0.16
_exptl_absorpt_correction_T_max  0.81

_exptl_special_details           
;
;

_diffrn_ambient_temperature      100.(2)

_diffrn_source                   'Incoatec microfocus source'
_diffrn_source_type              'Incoatec I\mS 3.0'
_diffrn_source_power             0.07
_diffrn_source_current           1.4
_diffrn_source_voltage           50

_diffrn_radiation_probe          X-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'Multilayer Mirror'

_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       'phi and omega scans'

_diffrn_detector_area_resol_mean 7.3910

_diffrn_reflns_number            31516
_diffrn_reflns_av_R_equivalents  0.0713
_diffrn_reflns_av_unetI/netI     0.0617
_diffrn_reflns_theta_min         2.14
_diffrn_reflns_theta_max         27.89
_diffrn_reflns_theta_full        25.24
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       7

_refine_special_details          
;
;

_reflns_number_total             7105
_reflns_number_gt                5640
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0378
_refine_ls_wR_factor_gt          0.0859
_refine_ls_wR_factor_ref         0.0939
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      1.007
_refine_ls_number_reflns         7105
_refine_ls_number_parameters     275
_refine_ls_number_restraints     0
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0393P)²] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.886
_refine_diff_density_min         -1.229
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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'

_computing_data_collection       'APEX4 (Ver 2021.4-0, Bruker AXS Inc., 2021)'
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_structure_solution    'XT, VERSION 2018/2'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  'APEX4 (Ver 2021.4-0, Bruker AXS Inc., 2021)'

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br Br1 0.62273(5) 0.43786(3) 0.01793(9) 0.02982(17) Uani d . . . 1 . .
Br Br2 0.56498(5) 0.31508(3) 0.29208(10) 0.02881(17) Uani d . . . 1 . .
Br Br3 0.60644(5) 0.45565(3) 0.53261(9) 0.02837(17) Uani d . . . 1 . .
Br Br4 0.85910(6) 0.48444(3) 0.38455(11) 0.0369(2) Uani d . . . 1 . .
Br Br5 0.77606(5) 0.34056(3) 0.64830(10) 0.03196(18) Uani d . . . 1 . .
Br Br6 1.06444(5) 0.27052(3) 0.59015(10) 0.02885(17) Uani d . . . 1 . .
Br Br7 1.00955(5) 0.39098(3) 0.87224(10) 0.02941(17) Uani d . . . 1 . .
Br Br8 0.83218(6) 0.31182(3) 1.15122(11) 0.03505(19) Uani d . . . 1 . .
C C1 0.6158(5) 0.5879(3) 0.3431(10) 0.0326(18) Uani d . . . 1 . .
H H1A 0.673547 0.576542 0.407862 0.039000 Uiso calc U . R 1 . .
H H1B 0.569865 0.598706 0.420604 0.039000 Uiso calc U . R 1 . .
C C2 0.6379(5) 0.6344(3) 0.2367(10) 0.0284(16) Uani d . . . 1 . .
C C3 0.7291(5) 0.6399(3) 0.1921(10) 0.0327(18) Uani d . . . 1 . .
H H3 0.775285 0.614993 0.229696 0.039000 Uiso calc U . R 1 . .
C C4 0.7537(5) 0.6815(4) 0.0925(11) 0.0348(19) Uani d . . . 1 . .
H H4 0.815978 0.684685 0.061949 0.042000 Uiso calc U . R 1 . .
C C5 0.6871(5) 0.7179(3) 0.0393(10) 0.0334(18) Uani d . . . 1 . .
H H5 0.703139 0.746534 -0.026998 0.040000 Uiso calc U . R 1 . .
C C6 0.5973(6) 0.7122(3) 0.0831(10) 0.0333(18) Uani d . . . 1 . .
H H6 0.551462 0.737196 0.044603 0.040000 Uiso calc U . R 1 . .
C C7 0.5710(5) 0.6714(3) 0.1817(9) 0.0279(17) Uani d . . . 1 . .
C C8 0.4720(5) 0.6689(3) 0.2404(11) 0.0323(18) Uani d . . . 1 . .
H H8A 0.456234 0.631935 0.263048 0.039000 Uiso calc U . R 1 . .
H H8B 0.470660 0.688813 0.343966 0.039000 Uiso calc U . R 1 . .
C C9 0.8570(6) 0.5142(3) 0.8589(12) 0.038(2) Uani d . . . 1 . .
H H9A 0.921322 0.517782 0.824690 0.045000 Uiso calc U . R 1 . .
H H9B 0.860927 0.513201 0.980141 0.045000 Uiso calc U . R 1 . .
C C10 0.8003(5) 0.5613(3) 0.8001(10) 0.0279(16) Uani d . . . 1 . .
C C11 0.7047(5) 0.5611(3) 0.8183(10) 0.0323(18) Uani d . . . 1 . .
H H11 0.677472 0.531394 0.865614 0.039000 Uiso calc U . R 1 . .
C C12 0.6478(6) 0.6036(3) 0.7689(10) 0.0309(17) Uani d . . . 1 . .
H H12 0.582743 0.602818 0.783103 0.037000 Uiso calc U . R 1 . .
C C13 0.6870(5) 0.6468(3) 0.6993(10) 0.0311(17) Uani d . . . 1 . .
H H13 0.648822 0.675749 0.664187 0.037000 Uiso calc U . R 1 . .
C C14 0.7829(5) 0.6479(3) 0.6806(10) 0.0303(17) Uani d . . . 1 . .
H H14 0.809711 0.678075 0.634948 0.036000 Uiso calc U . R 1 . .
C C15 0.8394(5) 0.6056(3) 0.7277(10) 0.0311(18) Uani d . . . 1 . .
C C16 0.9432(5) 0.6095(3) 0.7023(10) 0.0318(18) Uani d . . . 1 . .
H H16A 0.966184 0.645031 0.733432 0.038000 Uiso calc U . R 1 . .
H H16B 0.978404 0.583802 0.773762 0.038000 Uiso calc U . R 1 . .
N N1 0.5771(4) 0.5433(2) 0.2417(8) 0.0289(14) Uani d . . . 1 . .
H H1C 0.525768 0.554161 0.178263 0.043000 Uiso calc U . R 1 . .
H H1D 0.560860 0.516851 0.308423 0.043000 Uiso calc U . R 1 . .
H H1E 0.621193 0.531567 0.176439 0.043000 Uiso calc U . R 1 . .
N N2 0.3999(4) 0.6911(3) 0.1154(8) 0.0283(14) Uani d . . . 1 . .
H H2A 0.399935 0.726671 0.122788 0.042000 Uiso calc U . R 1 . .
H H2B 0.342401 0.678559 0.134666 0.042000 Uiso calc U . R 1 . .
H H2C 0.413875 0.681360 0.013261 0.042000 Uiso calc U . R 1 . .
N N3 0.8159(5) 0.4645(2) 0.7936(9) 0.0324(15) Uani d . . . 1 . .
H H3A 0.761076 0.458284 0.838884 0.049000 Uiso calc U . R 1 . .
H H3B 0.856421 0.437687 0.818912 0.049000 Uiso calc U . R 1 . .
H H3C 0.805025 0.466916 0.682845 0.049000 Uiso calc U . R 1 . .
N N4 0.9603(4) 0.5989(3) 0.5256(8) 0.0295(14) Uani d . . . 1 . .
H H4A 0.923899 0.571653 0.487330 0.044000 Uiso calc U . R 1 . .
H H4B 1.021592 0.590773 0.518533 0.044000 Uiso calc U . R 1 . .
H H4C 0.945622 0.628031 0.464423 0.044000 Uiso calc U . R 1 . .
Pb Pb1 0.71394(2) 0.39138(2) 0.33067(3) 0.02482(8) Uani d . . . 1 . .
Pb Pb2 0.93090(2) 0.28713(2) 0.84874(4) 0.02563(8) Uani d . . . 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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Br1 Pb1 . 3.0226(8) ?
Br2 Pb1 . 2.8880(8) ?
Br3 Pb1 . 2.8651(8) ?
Br4 Pb1 . 3.1642(9) ?
Br5 Pb1 . 2.9775(8) ?
Br5 Pb2 . 2.9824(8) ?
Br6 Pb2 . 2.9975(8) ?
Br6 Pb2 4_565 3.0213(8) ?
Br7 Pb2 . 2.8787(8) ?
Br8 Pb2 . 3.0168(9) ?
Br8 Pb1 1_556 3.0906(9) ?
C1 N1 . 1.490(10) ?
C1 C2 . 1.518(12) ?
C2 C3 . 1.393(11) ?
C2 C7 . 1.395(11) ?
C3 C4 . 1.402(12) ?
C4 C5 . 1.376(12) ?
C5 C6 . 1.372(11) ?
C6 C7 . 1.389(12) ?
C7 C8 . 1.536(10) ?
C8 N2 . 1.506(10) ?
C9 N3 . 1.481(10) ?
C9 C10 . 1.507(11) ?
C10 C11 . 1.390(10) ?
C10 C15 . 1.413(11) ?
C11 C12 . 1.396(11) ?
C12 C13 . 1.380(11) ?
C13 C14 . 1.395(10) ?
C14 C15 . 1.385(12) ?
C15 C16 . 1.523(10) ?
C16 N4 . 1.511(10) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Pb1 Br5 Pb2 . . 146.80(3) ?
Pb2 Br6 Pb2 . 4_565 97.10(2) ?
Pb2 Br8 Pb1 . 1_556 147.05(3) ?
N1 C1 C2 . . 111.2(7) ?
C3 C2 C7 . . 118.9(7) ?
C3 C2 C1 . . 118.2(7) ?
C7 C2 C1 . . 122.9(7) ?
C2 C3 C4 . . 121.0(7) ?
C5 C4 C3 . . 119.6(8) ?
C6 C5 C4 . . 119.3(8) ?
C5 C6 C7 . . 122.3(8) ?
C6 C7 C2 . . 118.9(7) ?
C6 C7 C8 . . 121.0(7) ?
C2 C7 C8 . . 120.0(7) ?
N2 C8 C7 . . 111.9(6) ?
N3 C9 C10 . . 112.2(6) ?
C11 C10 C15 . . 118.4(7) ?
C11 C10 C9 . . 118.3(7) ?
C15 C10 C9 . . 123.3(7) ?
C10 C11 C12 . . 121.6(8) ?
C13 C12 C11 . . 119.4(8) ?
C12 C13 C14 . . 119.9(8) ?
C15 C14 C13 . . 120.9(8) ?
C14 C15 C10 . . 119.8(7) ?
C14 C15 C16 . . 117.9(7) ?
C10 C15 C16 . . 122.4(7) ?
N4 C16 C15 . . 110.8(6) ?
Br3 Pb1 Br2 . . 91.19(2) ?
Br3 Pb1 Br5 . . 83.21(2) ?
Br2 Pb1 Br5 . . 88.23(2) ?
Br3 Pb1 Br1 . . 92.78(2) ?
Br2 Pb1 Br1 . . 84.58(2) ?
Br5 Pb1 Br1 . . 171.70(2) ?
Br3 Pb1 Br8 . 1_554 172.44(2) ?
Br2 Pb1 Br8 . 1_554 86.28(2) ?
Br5 Pb1 Br8 . 1_554 89.58(2) ?
Br1 Pb1 Br8 . 1_554 94.08(2) ?
Br3 Pb1 Br4 . . 82.47(2) ?
Br2 Pb1 Br4 . . 173.26(2) ?
Br5 Pb1 Br4 . . 93.29(2) ?
Br1 Pb1 Br4 . . 93.39(2) ?
Br8 Pb1 Br4 1_554 . 100.29(2) ?
Br7 Pb2 Br5 . . 83.51(2) ?
Br7 Pb2 Br6 . . 84.72(2) ?
Br5 Pb2 Br6 . . 99.52(2) ?
Br7 Pb2 Br8 . . 87.73(2) ?
Br5 Pb2 Br8 . . 88.78(2) ?
Br6 Pb2 Br8 . . 168.05(2) ?
Br7 Pb2 Br6 . 4_566 100.34(2) ?
Br5 Pb2 Br6 . 4_566 170.79(2) ?
Br6 Pb2 Br6 . 4_566 89.20(2) ?
Br8 Pb2 Br6 . 4_566 83.05(2) ?



####################################################################### 
# 
# 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_phan_PAP_3
_database_code_depnum_ccdc_archive 'CCDC 2300670'
loop_
_audit_author_name
_audit_author_address
'Yongxin Li'
;Nanyang Technological University
Singapore
;
_audit_update_record             
;
2023-10-11 deposited with the CCDC.	2024-07-25 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H28 Br6 N4 Pb'
_chemical_formula_iupac          ?
_chemical_formula_weight         963.07

_chemical_melting_point          ?

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.7441(12)
_cell_length_b                   14.5106(17)
_cell_length_c                   8.5473(12)
_cell_angle_alpha                90
_cell_angle_beta                 103.625(5)
_cell_angle_gamma                90
_cell_volume                     1295.1(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5050
_cell_measurement_theta_min      2.8075
_cell_measurement_theta_max      28.1499
_cell_measurement_temperature    296.(2)

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_exptl_crystal_density_diffrn    2.470
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             888

_exptl_absorpt_coefficient_mu    15.780
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_absorpt_correction_T_min  0.14
_exptl_absorpt_correction_T_max  0.74

_exptl_special_details           
;
;

_diffrn_ambient_temperature      296.(2)

_diffrn_source                   'Incoatec microfocus source'
_diffrn_source_type              'Bruker D8 Quest'
_diffrn_source_power             0.07
_diffrn_source_current           1.4
_diffrn_source_voltage           50

_diffrn_radiation_probe          X-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'Multilayer Mirror'

_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Photon II CPAD detector'
_diffrn_measurement_method       'phi and omega scans'

_diffrn_detector_area_resol_mean 7.3910

_diffrn_reflns_number            19517
_diffrn_reflns_av_R_equivalents  0.0995
_diffrn_reflns_av_unetI/netI     0.0874
_diffrn_reflns_theta_min         2.40
_diffrn_reflns_theta_max         32.61
_diffrn_reflns_theta_full        25.24
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       11

_refine_special_details          
;
;

_reflns_number_total             4727
_reflns_number_gt                2939
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0955
_refine_ls_R_factor_gt           0.0515
_refine_ls_wR_factor_gt          0.1152
_refine_ls_wR_factor_ref         0.1367
_refine_ls_goodness_of_fit_ref   0.949
_refine_ls_restrained_S_all      0.949
_refine_ls_number_reflns         4727
_refine_ls_number_parameters     114
_refine_ls_number_restraints     0
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0581P)²] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.916
_refine_diff_density_min         -1.607
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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'

_computing_data_collection       'APEX4 (Ver 2021.4-0, Bruker AXS Inc., 2021)'
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_structure_solution    'XT, VERSION 2018/2'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  'APEX4 (Ver 2021.4-0, Bruker AXS Inc., 2021)'

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br Br1 0.88468(8) 0.42693(5) 0.76645(10) 0.0474(2) Uani d . . . 1 . .
Br Br2 0.75287(7) 0.47571(5) 0.24198(11) 0.04658(19) Uani d . . . 1 . .
Br Br3 1.05298(7) 0.31084(5) 0.38594(10) 0.04500(19) Uani d . . . 1 . .
C C1 0.3235(7) 0.1286(6) 0.6615(11) 0.055(2) Uani d . . . 1 . .
H H1A 0.371479 0.071534 0.668280 0.065000 Uiso calc U . R 1 . .
H H1B 0.310665 0.142028 0.767728 0.065000 Uiso calc U . R 1 . .
C C2 0.4005(4) 0.2051(3) 0.6115(6) 0.0424(16) Uani d . . G 1 . .
C C3 0.3733(4) 0.2967(3) 0.6374(6) 0.0432(17) Uani d . . G 1 . .
H H3 0.304275 0.311352 0.680983 0.052000 Uiso calc U . R 1 . .
C C4 0.4493(5) 0.3664(2) 0.5980(6) 0.0502(19) Uani d . . G 1 . .
H H4 0.431127 0.427681 0.615313 0.060000 Uiso calc U . R 1 . .
C C5 0.5525(4) 0.3445(3) 0.5329(6) 0.0464(17) Uani d . . G 1 . .
H H5 0.603383 0.391088 0.506531 0.056000 Uiso calc U . R 1 . .
C C6 0.5797(4) 0.2528(3) 0.5070(6) 0.0421(16) Uani d . . G 1 . .
C C7 0.5037(4) 0.1831(2) 0.5464(6) 0.0433(16) Uani d . . G 1 . .
H H7 0.521936 0.121836 0.529088 0.052000 Uiso calc U . R 1 . .
C C8 0.6920(7) 0.2308(6) 0.4321(10) 0.0480(18) Uani d . . . 1 . .
H H8A 0.674867 0.173646 0.372120 0.058000 Uiso calc U . R 1 . .
H H8B 0.700378 0.279378 0.357219 0.058000 Uiso calc U . R 1 . .
N N1 0.1954(6) 0.1158(4) 0.5466(8) 0.0439(14) Uani d . . . 1 . .
H H1C 0.156628 0.170210 0.526237 0.066000 Uiso calc U . R 1 . .
H H1D 0.147414 0.078353 0.590347 0.066000 Uiso calc U . R 1 . .
H H1E 0.206251 0.091402 0.455270 0.066000 Uiso calc U . R 1 . .
N N2 0.8139(6) 0.2221(4) 0.5562(8) 0.0434(14) Uani d . . . 1 . .
H H2A 0.822816 0.270160 0.622628 0.065000 Uiso calc U . R 1 . .
H H2B 0.879172 0.220520 0.508660 0.065000 Uiso calc U . R 1 . .
H H2C 0.812784 0.170368 0.611828 0.065000 Uiso calc U . R 1 . .
Pb Pb1 1.000000 0.500000 0.500000 0.03655(11) Uani d . P S 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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Br1 Pb1 . 3.0291(8) ?
Br2 Pb1 . 3.0462(9) ?
Br3 Pb1 . 3.0116(8) ?
C1 N1 . 1.502(10) ?
C1 C2 . 1.505(9) ?
C2 C3 . 1.390000 ?
C2 C7 . 1.390000 ?
C3 C4 . 1.390000 ?
C4 C5 . 1.390000 ?
C5 C6 . 1.390000 ?
C6 C7 . 1.390000 ?
C6 C8 . 1.527(8) ?
C8 N2 . 1.484(10) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 C1 C2 . . 112.7(6) ?
C3 C2 C7 . . 120.000000 ?
C3 C2 C1 . . 120.7(4) ?
C7 C2 C1 . . 119.3(4) ?
C2 C3 C4 . . 120.000000 ?
C5 C4 C3 . . 120.000000 ?
C4 C5 C6 . . 120.000000 ?
C7 C6 C5 . . 120.000000 ?
C7 C6 C8 . . 121.1(4) ?
C5 C6 C8 . . 118.9(4) ?
C6 C7 C2 . . 120.000000 ?
N2 C8 C6 . . 111.7(6) ?
Br3 Pb1 Br3 . 3_766 180.000000 ?
Br3 Pb1 Br1 . . 93.80(2) ?
Br3 Pb1 Br1 3_766 . 86.20(2) ?
Br3 Pb1 Br1 . 3_766 86.20(2) ?
Br3 Pb1 Br1 3_766 3_766 93.80(2) ?
Br1 Pb1 Br1 . 3_766 180.000000 ?
Br3 Pb1 Br2 . 3_766 98.10(2) ?
Br3 Pb1 Br2 3_766 3_766 81.90(2) ?
Br1 Pb1 Br2 . 3_766 86.41(2) ?
Br1 Pb1 Br2 3_766 3_766 93.59(2) ?
Br3 Pb1 Br2 . . 81.91(2) ?
Br3 Pb1 Br2 3_766 . 98.10(2) ?
Br1 Pb1 Br2 . . 93.59(3) ?
Br1 Pb1 Br2 3_766 . 86.41(2) ?
Br2 Pb1 Br2 3_766 . 180.000000 ?



