# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 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_x2
_database_code_depnum_ccdc_archive 'CCDC 2116502'
loop_
_audit_author_name
_audit_author_address
'liwei tang'
;Fujian Institute of Research on the Structure of Matter
China
;
_audit_update_record             
;
2021-10-19 deposited with the CCDC.	2021-12-20 downloaded from the CCDC.
;
_audit_creation_date             2021-10-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br14 Pb4, 4(C5 H14 N), 2(C2 H8 N)'
_chemical_formula_sum            'C24 H72 Br14 N6 Pb4'
_chemical_formula_weight         2392.37
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           69
_space_group_name_H-M_alt        'F m m m'
_space_group_name_Hall           '-F 2 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x, -y, -z'
'-x, y, -z'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x, -y+1/2, -z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+1/2, -y, -z+1/2'
'-x+1/2, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, y, -z'
'-x, y, z'
'x, -y, z'
'-x, -y+1/2, -z+1/2'
'x, y+1/2, -z+1/2'
'-x, y+1/2, z+1/2'
'x, -y+1/2, z+1/2'
'-x+1/2, -y, -z+1/2'
'x+1/2, y, -z+1/2'
'-x+1/2, y, z+1/2'
'x+1/2, -y, z+1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z'
'-x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z'

_cell_length_a                   8.333(2)
_cell_length_b                   8.372(2)
_cell_length_c                   43.928(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3064.7(14)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2136
_cell_measurement_temperature    249.99
_cell_measurement_theta_max      25.654
_cell_measurement_theta_min      2.782
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    20.103
_exptl_absorpt_correction_T_max  0.0949
_exptl_absorpt_correction_T_min  0.0435
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1483 before and 0.0977 after correction.
The Ratio of minimum to maximum transmission is 0.4584.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.593
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2152
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0860
_diffrn_reflns_av_unetI/netI     0.0686
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            5089
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.578
_diffrn_reflns_theta_min         3.481
_diffrn_ambient_temperature      249.99
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX2 microsource'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                773
_reflns_number_total             1016
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         1.917
_refine_diff_density_min         -1.970
_refine_diff_density_rms         0.389
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     105
_refine_ls_number_reflns         1016
_refine_ls_number_restraints     111
_refine_ls_R_factor_all          0.1093
_refine_ls_R_factor_gt           0.0870
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1340P)²+323.5944P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2397
_refine_ls_wR_factor_ref         0.2582
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C3-C2 = C2-C1 = C5-C3 = N1-C1
 1.5 with sigma of 0.02
 C7-N2
 1.5 with sigma of 0.02
 C3-C4
 1.5 with sigma of 0.02
 N2-C6
 1.5 with sigma of 0.02
 N1-Br2_$1
 2.5 with sigma of 0.02
 C6-C7
 2.5 with sigma of 0.04
 C7-Br3
 3 with sigma of 0.04
 C1-C3 = C2-N1 = C2-C5
 2.5 with sigma of 0.04
 C5-C4
 2.5 with sigma of 0.04
 N2_$1-N2_$2
 2.5 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C5 \\sim C4 \\sim C7 \\sim C6 \\sim N1 \\sim N2:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C5) \\sim
Ueq, Uanis(C4) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(N1)
\\sim Ueq, Uanis(N2) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
4. Others
 Fixed Sof: Br1(0.25) C1(0.25) H1A(0.25) H1B(0.25) C2(0.25) H2A(0.25)
 H2B(0.25) C3(0.25) H3(0.25) C5(0.25) H5A(0.25) H5B(0.25) H5C(0.25) N1(0.25)
 H1C(0.25) H1D(0.25) H1E(0.25) C4(0.25) H4A(0.25) H4B(0.25) H4C(0.25) C7(0.125)
 H7A(0.125) H7B(0.125) H7C(0.125) N2(0.125) H2C(0.125) H2D(0.125) C6(0.125)
 H6A(0.125) H6B(0.125) H6C(0.125)
5.a Ternary CH refined with riding coordinates:
 C3(H3)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), N2(H2C,H2D)
5.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), N1(H1C,H1D,H1E), C4(H4A,H4B,H4C), C7(H7A,H7B,H7C), C6(H6A,
 H6B,H6C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.500000 0.500000 0.42731(2) 0.04754(14) Uani 1 4 d S T P . .
Br2 Br 0.750000 0.250000 0.42406(6) 0.1429(11) Uani 1 2 d DS T P . .
Br1 Br 0.500000 0.4517(3) 0.36418(7) 0.137(2) Uani 0.5 2 d S T P . .
Br3 Br 0.500000 0.500000 0.500000 0.147(2) Uani 1 8 d DS T P . .
C1 C -0.0175(13) 0.4835(14) 0.37867(19) 0.1279(3) Uani 0.25 1 d D U . A -1
H1A H -0.113812 0.431158 0.386718 0.153 Uiso 0.25 1 calc R . . A -1
H1B H 0.010539 0.570852 0.392530 0.153 Uiso 0.25 1 calc R . . A -1
C2 C -0.055(2) 0.5512(12) 0.34818(16) 0.1290(3) Uani 0.25 1 d D U . A -1
H2A H 0.037932 0.614612 0.341643 0.155 Uiso 0.25 1 calc R . . A -1
H2B H -0.145194 0.624941 0.350507 0.155 Uiso 0.25 1 calc R . . A -1
C3 C -0.0948(11) 0.4376(11) 0.32319(17) 0.1305(3) Uani 0.25 1 d D U . A -1
H3 H -0.170704 0.356539 0.331046 0.157 Uiso 0.25 1 calc R . . A -1
C5 C 0.0455(12) 0.3538(16) 0.3087(3) 0.1336(7) Uani 0.25 1 d D U . A -1
H5A H 0.085019 0.417001 0.291812 0.200 Uiso 0.25 1 calc GR . . A -1
H5B H 0.011722 0.249850 0.301406 0.200 Uiso 0.25 1 calc GR . . A -1
H5C H 0.130214 0.340633 0.323669 0.200 Uiso 0.25 1 calc GR . . A -1
N1 N 0.1173(11) 0.3653(12) 0.3781(2) 0.1381(7) Uani 0.25 1 d D U . A -1
H1C H 0.076953 0.265678 0.377143 0.166 Uiso 0.25 1 calc GR . . A -1
H1D H 0.176583 0.375775 0.395084 0.166 Uiso 0.25 1 calc GR . . A -1
H1E H 0.179245 0.383374 0.361662 0.166 Uiso 0.25 1 calc GR . . A -1
C4 C -0.1795(17) 0.5392(16) 0.2999(3) 0.1314(7) Uani 0.25 1 d D U . A -1
H4A H -0.245624 0.471786 0.287068 0.197 Uiso 0.25 1 calc GR . . A -1
H4B H -0.100803 0.594315 0.287513 0.197 Uiso 0.25 1 calc GR . . A -1
H4C H -0.246741 0.616850 0.310215 0.197 Uiso 0.25 1 calc GR . . A -1
C7 C 0.1430(13) 0.5293(16) 0.5077(3) 0.0947(7) Uani 0.125 1 d D U . B -1
H7A H 0.178119 0.579846 0.526412 0.142 Uiso 0.125 1 calc GR . . B -1
H7B H 0.235718 0.491253 0.496483 0.142 Uiso 0.125 1 calc GR . . B -1
H7C H 0.073295 0.439999 0.512467 0.142 Uiso 0.125 1 calc GR . . B -1
N2 N 0.0531(12) 0.6483(8) 0.4887(3) 0.0949(3) Uani 0.125 1 d D U . B -1
H2C H 0.016246 0.727291 0.500688 0.114 Uiso 0.125 1 calc R . . B -1
H2D H 0.120258 0.691796 0.474929 0.114 Uiso 0.125 1 calc R . . B -1
C6 C -0.0850(12) 0.572(2) 0.4724(3) 0.0931(7) Uani 0.125 1 d D U . B -1
H6A H -0.056395 0.463807 0.466690 0.140 Uiso 0.125 1 calc GR . . B -1
H6B H -0.110366 0.633159 0.454294 0.140 Uiso 0.125 1 calc GR . . B -1
H6C H -0.177762 0.569602 0.485759 0.140 Uiso 0.125 1 calc GR . . B -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br2 2.9566(6) 19_655 ?
Pb1 Br2 2.9566(6) 13_455 ?
Pb1 Br2 2.9566(6) . ?
Pb1 Br2 2.9566(6) 31_655 ?
Pb1 Br1 2.803(3) 2_665 ?
Pb1 Br1 2.803(3) . ?
Pb1 Br3 3.1930(11) . ?
Br1 Br1 0.809(6) 2_665 ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 C2 1.487(11) . ?
C1 N1 1.497(12) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 C3 1.490(11) . ?
C3 H3 0.9900 . ?
C3 C5 1.504(12) . ?
C3 C4 1.505(13) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 H5C 0.9700 . ?
N1 H1C 0.9000 . ?
N1 H1D 0.9000 . ?
N1 H1E 0.9000 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 H4C 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 H7C 0.9700 . ?
C7 N2 1.501(13) . ?
N2 H2C 0.9000 . ?
N2 H2D 0.9000 . ?
N2 C6 1.497(14) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 H6C 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br2 Pb1 Br2 89.60(2) 19_655 . ?
Br2 Pb1 Br2 89.60(2) 31_655 13_455 ?
Br2 Pb1 Br2 90.13(2) 19_655 13_455 ?
Br2 Pb1 Br2 174.45(11) 19_655 31_655 ?
Br2 Pb1 Br2 90.13(2) . 31_655 ?
Br2 Pb1 Br2 174.45(11) . 13_455 ?
Br2 Pb1 Br3 92.77(5) 19_655 . ?
Br2 Pb1 Br3 92.77(5) 13_455 . ?
Br2 Pb1 Br3 92.77(5) . . ?
Br2 Pb1 Br3 92.77(5) 31_655 . ?
Br1 Pb1 Br2 81.37(7) 2_665 13_455 ?
Br1 Pb1 Br2 81.37(7) 2_665 31_655 ?
Br1 Pb1 Br2 81.37(7) . 19_655 ?
Br1 Pb1 Br2 93.11(7) . 13_455 ?
Br1 Pb1 Br2 93.11(7) 2_665 19_655 ?
Br1 Pb1 Br2 93.11(7) 2_665 . ?
Br1 Pb1 Br2 81.37(7) . . ?
Br1 Pb1 Br2 93.11(7) . 31_655 ?
Br1 Pb1 Br1 16.60(12) 2_665 . ?
Br1 Pb1 Br3 171.70(6) . . ?
Br1 Pb1 Br3 171.70(6) 2_665 . ?
Pb1 Br2 Pb1 174.46(11) 13_545 . ?
Br1 Br1 Pb1 81.70(6) 2_665 . ?
Pb1 Br3 Pb1 180.0 . 17_666 ?
H1A C1 H1B 107.8 . . ?
C2 C1 H1A 109.0 . . ?
C2 C1 H1B 109.0 . . ?
C2 C1 N1 113.1(9) . . ?
N1 C1 H1A 109.0 . . ?
N1 C1 H1B 109.0 . . ?
C1 C2 H2A 107.8 . . ?
C1 C2 H2B 107.8 . . ?
C1 C2 C3 117.8(8) . . ?
H2A C2 H2B 107.2 . . ?
C3 C2 H2A 107.8 . . ?
C3 C2 H2B 107.8 . . ?
C2 C3 H3 108.9 . . ?
C2 C3 C5 115.8(10) . . ?
C2 C3 C4 104.2(9) . . ?
C5 C3 H3 108.9 . . ?
C5 C3 C4 110.0(9) . . ?
C4 C3 H3 108.9 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C1 N1 H1C 109.5 . . ?
C1 N1 H1D 109.5 . . ?
C1 N1 H1E 109.5 . . ?
H1C N1 H1D 109.5 . . ?
H1C N1 H1E 109.5 . . ?
H1D N1 H1E 109.5 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N2 C7 H7A 109.5 . . ?
N2 C7 H7B 109.5 . . ?
N2 C7 H7C 109.5 . . ?
C7 N2 H2C 109.3 . . ?
C7 N2 H2D 109.3 . . ?
H2C N2 H2D 108.0 . . ?
C6 N2 C7 111.5(10) . . ?
C6 N2 H2C 109.3 . . ?
C6 N2 H2D 109.3 . . ?
N2 C6 H6A 109.5 . . ?
N2 C6 H6B 109.5 . . ?
N2 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C5 -78.3(15) . . . . ?
C1 C2 C3 C4 160.9(13) . . . . ?
N1 C1 C2 C3 56.4(17) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
