# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 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_7863
_database_code_depnum_ccdc_archive 'CCDC 2289662'
loop_
_audit_author_name
_audit_author_address
'sheng cao'
;HuBei University
China
;
_audit_update_record             
;
2023-08-20 deposited with the CCDC.	2024-05-28 downloaded from the CCDC.
;
_audit_creation_date             2022-09-19
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(Br6 Pb2), 0.5(C4 H14 N2)'
_chemical_formula_sum            'C2 H7 Br3 N Pb'
_chemical_formula_weight         492.01
_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 0.0181 0.0091 '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 -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -4.0753 8.5060 '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           55
_space_group_name_H-M_alt        'P b a m'
_space_group_name_Hall           '-P 2 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z'
'x-1/2, -y-1/2, z'
'-x-1/2, y-1/2, z'

_cell_length_a                   16.7748(2)
_cell_length_b                   8.58510(10)
_cell_length_c                   6.03300(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     868.83(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4846
_cell_measurement_temperature    298.0(1)
_cell_measurement_theta_max      75.3710
_cell_measurement_theta_min      5.2280
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    53.201
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.25710
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.761
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0652
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            6081
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.023
_diffrn_reflns_theta_min         5.274
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      298.0(1)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -35.00  -1.00   0.50    0.50    --    0.00  82.00 -60.00   68
  2  ω    -39.00 -11.00   0.50    0.50    --    0.00 -82.00  60.00   56
  3  ω    -39.00  36.00   0.50    0.50    --    0.00 -82.00 -60.00  150
  4  ω      3.00  34.00   0.50    0.50    --    0.00  82.00 -60.00   62
  5  ω     -8.00  36.00   0.50    0.50    --    0.00 -82.00  60.00   88
  6  ω    153.00 187.00   0.50    0.50    --  101.90  38.00 -60.00   68
  7  ω     77.00 106.00   0.50    0.50    --  101.90  38.00 -60.00   58
  8  ω     41.00  67.00   0.50    0.50    --  101.90 -82.00 120.00   52
  9  ω     18.00 126.00   0.50    0.50    --  101.90 -82.00 -60.00  216
 10  ω    101.00 136.00   0.50    0.50    --  101.90 -82.00 120.00   70
 11  ω     85.00 189.00   0.50    0.50    --  101.90  57.00-120.00  208
 12  ω     16.00 129.00   0.50    0.50    --  101.90 -82.00  90.00  226
 13  ω     76.00 182.00   0.50    0.50    --  101.90  38.00 150.00  212
 14  ω     82.00 190.00   0.50    0.50    --  101.90  38.00 -30.00  216
 15  ω     74.00 160.00   0.50    0.50    --  101.90  57.00-150.00  172
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0448444000
_diffrn_orient_matrix_UB_12      -0.0005935000
_diffrn_orient_matrix_UB_13      0.2228494000
_diffrn_orient_matrix_UB_21      -0.0645508000
_diffrn_orient_matrix_UB_22      -0.1061093000
_diffrn_orient_matrix_UB_23      -0.1009473000
_diffrn_orient_matrix_UB_31      0.0474845000
_diffrn_orient_matrix_UB_32      -0.1447422000
_diffrn_orient_matrix_UB_33      0.0731219000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                961
_reflns_number_total             992
_reflns_odcompleteness_completeness 99.58
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         2.953
_refine_diff_density_min         -2.822
_refine_diff_density_rms         0.667
_refine_ls_extinction_coef       0.0069(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     44
_refine_ls_number_reflns         992
_refine_ls_number_restraints     51
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_gt           0.0465
_refine_ls_restrained_S_all      1.067
_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)+(0.0839P)²+5.3324P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1195
_refine_ls_wR_factor_ref         0.1201
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,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. Shared sites
{C1, N1}
{C2, N2}
3. Restrained distances
 N2-C3 = N2-N1
 1.51 with sigma of 0.02
 C3_$1-C3
 1.55 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C3 \\sim C1 \\sim C2 \\sim N2 \\sim N1: within 1.7A with sigma of 0.02 and
sigma for terminal atoms of 0.04 within 1.7A
Uanis(C1) = Uanis(N1)
Uanis(C2) = Uanis(N2)
5. Others
 Fixed Sof: C1(0.25) H1A(0.25) H1B(0.25) H1C(0.25) C2(0.25) H2A(0.25)
 H2B(0.25) H3AA(0.25) H3AB(0.25) H3BC(0.25) H3BD(0.25) N1(0.25) H1D(0.25)
 H1E(0.25) H1F(0.25) N2(0.25) H2C(0.25) H2D(0.25)
6.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3AA,H3AB), C3(H3BC,H3BD), N2(H2C,H2D)
6.b Me refined with riding coordinates:
 C1(H1A,H1B,H1C), N1(H1D,H1E,H1F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.62924(2) 0.44581(5) 1.000000 0.0223(3) Uani 1 2 d S T P . .
Br1 Br 0.52612(9) 0.73121(16) 1.000000 0.0398(4) Uani 1 2 d S T P . .
Br2 Br 0.77512(14) 0.6482(3) 1.000000 0.0802(7) Uani 1 2 d S T P . .
Br3 Br 0.62818(11) 0.4483(2) 0.500000 0.0530(6) Uani 1 2 d S T P . .
C1 C 0.6693(17) 0.880(4) 0.500000 0.123(8) Uani 0.5 2 d S TU P A 1
H1A H 0.692837 0.778482 0.500000 0.185 Uiso 0.5 2 calc R U P A 1
H1B H 0.686018 0.936059 0.370075 0.185 Uiso 0.25 1 calc R U P A 1
H1C H 0.686018 0.936059 0.629925 0.185 Uiso 0.25 1 calc R U P A 1
C2 C 0.5806(16) 0.866(3) 0.500000 0.116(6) Uani 0.5 2 d S TU P A 1
H2A H 0.563409 0.808605 0.369738 0.140 Uiso 0.25 1 calc R U P A 1
H2B H 0.563409 0.808605 0.630262 0.140 Uiso 0.25 1 calc R U P A 1
C3 C 0.5441(6) 1.023(2) 0.500000 0.108(7) Uani 1 2 d DS TU P . .
H3AA H 0.558359 1.081870 0.368624 0.130 Uiso 0.25 1 calc R U P A 1
H3AB H 0.558359 1.081871 0.631376 0.130 Uiso 0.25 1 calc R U P A 1
H3BC H 0.558359 1.081870 0.368624 0.130 Uiso 0.25 1 calc R U P A 2
H3BD H 0.558359 1.081871 0.631376 0.130 Uiso 0.25 1 calc R U P A 2
N1 N 0.6693(17) 0.880(4) 0.500000 0.123(8) Uani 0.5 2 d DS TU P A 2
H1D H 0.691120 0.785913 0.500000 0.148 Uiso 0.5 2 calc R U P A 2
H1E H 0.684797 0.932000 0.379549 0.148 Uiso 0.25 1 calc R U P A 2
H1F H 0.684797 0.932000 0.620451 0.148 Uiso 0.25 1 calc R U P A 2
N2 N 0.5806(16) 0.866(3) 0.500000 0.116(6) Uani 0.5 2 d DS TU P A 2
H2C H 0.564824 0.813317 0.380481 0.140 Uiso 0.25 1 calc R U P A 2
H2D H 0.564824 0.813317 0.619519 0.140 Uiso 0.25 1 calc R U 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 2.9993(14) . ?
Pb1 Br1 3.0170(15) 5_667 ?
Pb1 Br2 3.0168(18) 3_647 ?
Pb1 Br2 3.0013(19) . ?
Pb1 Br3 3.01663(6) 1_556 ?
Pb1 Br3 3.01663(6) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C1 C2 1.494(19) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C3 1.482(18) . ?
C3 C3 1.53(2) 2_675 ?
C3 H3AA 0.9700 . ?
C3 H3AB 0.9700 . ?
C3 H3BC 0.9700 . ?
C3 H3BD 0.9700 . ?
C3 N2 1.482(18) . ?
N1 H1D 0.8900 . ?
N1 H1E 0.8900 . ?
N1 H1F 0.8900 . ?
N1 N2 1.494(19) . ?
N2 H2C 0.8900 . ?
N2 H2D 0.8900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br1 Pb1 Br1 85.03(4) . 5_667 ?
Br1 Pb1 Br2 176.91(6) . 3_647 ?
Br1 Pb1 Br2 89.84(6) . . ?
Br1 Pb1 Br3 89.47(3) . 1_556 ?
Br1 Pb1 Br3 89.47(3) . . ?
Br2 Pb1 Br1 91.88(6) 3_647 5_667 ?
Br2 Pb1 Br1 174.87(6) . 5_667 ?
Br2 Pb1 Br2 93.251(17) . 3_647 ?
Br2 Pb1 Br3 90.04(3) . 1_556 ?
Br2 Pb1 Br3 90.04(3) . . ?
Br3 Pb1 Br1 89.91(3) 1_556 5_667 ?
Br3 Pb1 Br1 89.91(3) . 5_667 ?
Br3 Pb1 Br2 90.52(3) . 3_647 ?
Br3 Pb1 Br2 90.52(3) 1_556 3_647 ?
Br3 Pb1 Br3 178.94(7) 1_556 . ?
Pb1 Br1 Pb1 94.97(4) . 5_667 ?
Pb1 Br2 Pb1 157.51(11) . 3_657 ?
Pb1 Br3 Pb1 178.94(7) . 1_554 ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
C1 C2 H2A 109.8 . . ?
C1 C2 H2B 109.8 . . ?
H2A C2 H2B 108.2 . . ?
C3 C2 C1 110(2) . . ?
C3 C2 H2A 109.8 . . ?
C3 C2 H2B 109.8 . . ?
C2 C3 C3 99(2) . 2_675 ?
C2 C3 H3AA 111.9 . . ?
C2 C3 H3AB 111.9 . . ?
C3 C3 H3AA 111.9 2_675 . ?
C3 C3 H3AB 111.9 2_675 . ?
C3 C3 H3BC 111.9 2_675 . ?
C3 C3 H3BD 111.9 2_675 . ?
H3AA C3 H3AB 109.6 . . ?
H3BC C3 H3BD 109.6 . . ?
N2 C3 H3BC 111.9 . . ?
N2 C3 H3BD 111.9 . . ?
H1D N1 H1E 109.5 . . ?
H1D N1 H1F 109.5 . . ?
H1E N1 H1F 109.5 . . ?
N2 N1 H1D 109.5 . . ?
N2 N1 H1E 109.5 . . ?
N2 N1 H1F 109.5 . . ?
C3 N2 N1 110(2) . . ?
C3 N2 H2C 109.8 . . ?
C3 N2 H2D 109.8 . . ?
N1 N2 H2C 109.8 . . ?
N1 N2 H2D 109.8 . . ?
H2C N2 H2D 108.2 . . ?

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 C3 180.0 . . . 2_675 ?
C3 C3 N2 N1 180.0 2_675 . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.279
_oxdiff_exptl_absorpt_empirical_full_min 0.520
