# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 2060102'
loop_
_audit_author_name
_audit_author_address
'Xiao-Wu Iei'
;JiNing University
China
;
_audit_update_record             
;
2021-02-01 deposited with the CCDC.	2021-09-24 downloaded from the CCDC.
;
_audit_creation_date             2020-07-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br10 Pb3, 2(C7 H20 N2)'
_chemical_formula_sum            'C14 H40 Br10 N4 Pb3'
_chemical_formula_weight         1685.17
_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      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                   11.6976(19)
_cell_length_b                   15.7370(15)
_cell_length_c                   11.890(2)
_cell_angle_alpha                90
_cell_angle_beta                 118.68(2)
_cell_angle_gamma                90
_cell_volume                     1920.2(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    10790
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.8040
_cell_measurement_theta_min      1.9280
_shelx_estimated_absorpt_T_max   0.101
_shelx_estimated_absorpt_T_min   0.089
_exptl_absorpt_coefficient_mu    23.535
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.02995
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017)
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    2.915
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0759
_diffrn_reflns_av_unetI/netI     0.0470
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            21921
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.811
_diffrn_reflns_theta_min         1.984
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      2.26 188.26   0.50    5.00    --   28.00  73.75 -25.74  372
  2  ω      2.26 188.26   0.50    5.00    --   28.00  73.75 154.26  372
  3  ω      2.26 188.26   0.50    5.00    --   28.00  73.75  64.26  372
  4  ω      2.26 188.26   0.50    5.00    --   28.00  73.75-115.74  372
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0062825000
_diffrn_orient_matrix_UB_12      0.0403333000
_diffrn_orient_matrix_UB_13      -0.0232647000
_diffrn_orient_matrix_UB_21      -0.0683597000
_diffrn_orient_matrix_UB_22      0.0056144000
_diffrn_orient_matrix_UB_23      -0.0295654000
_diffrn_orient_matrix_UB_31      0.0066965000
_diffrn_orient_matrix_UB_32      0.0195228000
_diffrn_orient_matrix_UB_33      0.0565289000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3287
_reflns_number_total             4701
_reflns_odcompleteness_completeness 93.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.75
_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 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         1.137
_refine_diff_density_min         -1.874
_refine_diff_density_rms         0.247
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         4701
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.0813
_refine_ls_R_factor_gt           0.0518
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0619P)²+8.9187P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1193
_refine_ls_wR_factor_ref         0.1335
_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) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1-C3A = N1-C3
 1.4 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(N1) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(H6BC)=Sof(H6BD)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=1-FVAR(1)
 Sof(H6AA)=Sof(H6AB)=Sof(C3)=Sof(H3A)=Sof(H3B)=FVAR(1)
 Sof(C2A)=Sof(H2AA)=Sof(H2AB)=1-FVAR(2)
 Sof(C2)=Sof(H2A)=Sof(H2B)=FVAR(2)
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=
 1-FVAR(3)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=FVAR(3)
5.a Ternary CH refined with riding coordinates:
 N2(H2), N1(H1)
5.b Secondary CH2 refined with riding coordinates:
 C6(H6AA,H6AB), C6(H6BC,H6BD), C3(H3A,H3B), C2(H2A,H2B), C3A(H3AA,H3AB),
 C2A(H2AA,H2AB)
5.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C4(H4A,H4B,H4C), C1(H1A,H1B,H1C), C7(H7A,H7B,H7C), C1A(H1AA,
 H1AB,H1AC), C7A(H7AA,H7AB,H7AC)
;
_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 0.29634(4) 0.49119(2) 0.35863(3) 0.04499(14) Uani 1 1 d . . . . .
Pb2 Pb 0.0000 0.5000 0.0000 0.04927(17) Uani 1 2 d S T P . .
Br5 Br 0.46989(13) 0.63109(7) 0.53707(13) 0.0622(3) Uani 1 1 d . . . . .
Br4 Br 0.28416(12) 0.53862(8) 0.07675(12) 0.0606(3) Uani 1 1 d . . . . .
Br3 Br 0.24968(15) 0.45140(8) 0.56432(12) 0.0712(4) Uani 1 1 d . . . . .
Br2 Br 0.11611(14) 0.35434(8) 0.18878(11) 0.0692(4) Uani 1 1 d . . . . .
Br1 Br 0.06061(15) 0.60438(9) 0.23826(14) 0.0800(4) Uani 1 1 d . . . . .
N2 N 0.8108(10) 0.3502(6) 0.3657(9) 0.063(3) Uani 1 1 d . . . . .
H2 H 0.7848 0.3987 0.3998 0.076 Uiso 1 1 calc R . . A 1
N1 N 0.3627(11) 0.3453(8) 0.0072(11) 0.080(3) Uani 1 1 d D U . . .
H1 H 0.3419 0.3987 0.0356 0.096 Uiso 1 1 calc R . . B 1
C6 C 0.5887(13) 0.3506(11) 0.1805(12) 0.080(4) Uani 1 1 d . . . . .
H6AA H 0.6099 0.3661 0.1136 0.096 Uiso 0.56(3) 1 calc R . . C 1
H6AB H 0.5781 0.4029 0.2176 0.096 Uiso 0.56(3) 1 calc R . . C 1
H6BC H 0.5667 0.2978 0.2077 0.096 Uiso 0.44(3) 1 calc R . . C 2
H6BD H 0.5687 0.3957 0.2239 0.096 Uiso 0.44(3) 1 calc R . . C 2
C5 C 0.267(2) 0.2848(13) -0.003(2) 0.140(7) Uani 1 1 d . U . . .
H5A H 0.3029 0.2285 0.0079 0.210 Uiso 1 1 calc GR . . . .
H5B H 0.1918 0.2894 -0.0857 0.210 Uiso 1 1 calc GR . . . .
H5C H 0.2434 0.2957 0.0625 0.210 Uiso 1 1 calc GR . . . .
C3 C 0.459(2) 0.3040(12) 0.1187(16) 0.067(8) Uani 0.56(3) 1 d D . . C 1
H3A H 0.4725 0.2470 0.0961 0.081 Uiso 0.56(3) 1 calc R . . C 1
H3B H 0.4278 0.2991 0.1806 0.081 Uiso 0.56(3) 1 calc R . . C 1
C2 C 0.698(2) 0.3048(16) 0.278(2) 0.056(8) Uani 0.53(4) 1 d . . . C 1
H2A H 0.6662 0.2737 0.3285 0.068 Uiso 0.53(4) 1 calc R . . C 1
H2B H 0.7246 0.2631 0.2358 0.068 Uiso 0.53(4) 1 calc R . . C 1
C4 C 0.347(2) 0.3607(14) -0.120(2) 0.140(8) Uani 1 1 d . U . . .
H4A H 0.3759 0.3119 -0.1479 0.210 Uiso 1 1 calc GR . . . .
H4B H 0.3971 0.4094 -0.1180 0.210 Uiso 1 1 calc GR . . . .
H4C H 0.2563 0.3709 -0.1791 0.210 Uiso 1 1 calc GR . . . .
C1 C 0.912(3) 0.3018(19) 0.473(2) 0.084(11) Uani 0.53(2) 1 d . . . C 1
H1A H 0.8794 0.2836 0.5289 0.125 Uiso 0.53(2) 1 calc GR . . C 1
H1B H 0.9872 0.3371 0.5189 0.125 Uiso 0.53(2) 1 calc GR . . C 1
H1C H 0.9357 0.2530 0.4397 0.125 Uiso 0.53(2) 1 calc GR . . C 1
C7 C 0.880(3) 0.384(2) 0.285(3) 0.105(13) Uani 0.53(2) 1 d . . . C 1
H7A H 0.9397 0.3423 0.2864 0.158 Uiso 0.53(2) 1 calc GR . . C 1
H7B H 0.9260 0.4359 0.3234 0.158 Uiso 0.53(2) 1 calc GR . . C 1
H7C H 0.8146 0.3951 0.1985 0.158 Uiso 0.53(2) 1 calc GR . . C 1
C3A C 0.4970(15) 0.3594(18) 0.048(3) 0.062(9) Uani 0.44(3) 1 d D . . C 2
H3AA H 0.5056 0.4165 0.0222 0.075 Uiso 0.44(3) 1 calc R . . C 2
H3AB H 0.5226 0.3205 0.0007 0.075 Uiso 0.44(3) 1 calc R . . C 2
C2A C 0.729(3) 0.350(2) 0.236(3) 0.070(10) Uani 0.47(4) 1 d . . . C 2
H2AA H 0.7515 0.3010 0.2013 0.084 Uiso 0.47(4) 1 calc R . . C 2
H2AB H 0.7518 0.3999 0.2017 0.084 Uiso 0.47(4) 1 calc R . . C 2
C1A C 0.794(3) 0.2636(17) 0.425(3) 0.081(10) Uani 0.47(2) 1 d . . . C 2
H1AA H 0.7106 0.2635 0.4235 0.121 Uiso 0.47(2) 1 calc GR . . C 2
H1AB H 0.8619 0.2585 0.5124 0.121 Uiso 0.47(2) 1 calc GR . . C 2
H1AC H 0.7978 0.2165 0.3761 0.121 Uiso 0.47(2) 1 calc GR . . C 2
C7A C 0.949(3) 0.368(2) 0.421(3) 0.086(11) Uani 0.47(2) 1 d . . . C 2
H7AA H 0.9941 0.3177 0.4172 0.129 Uiso 0.47(2) 1 calc GR . . C 2
H7AB H 0.9833 0.3852 0.5086 0.129 Uiso 0.47(2) 1 calc GR . . C 2
H7AC H 0.9626 0.4127 0.3733 0.129 Uiso 0.47(2) 1 calc GR . . C 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 Br5 3.0555(13) . ?
Pb1 Br5 3.0761(14) 3_666 ?
Pb1 Br3 2.8201(13) . ?
Pb1 Br2 3.0123(13) . ?
Pb1 Br1 3.0061(15) . ?
Pb2 Br4 3.0560(14) . ?
Pb2 Br4 3.0559(14) 3_565 ?
Pb2 Br2 3.0349(13) . ?
Pb2 Br2 3.0349(13) 3_565 ?
Pb2 Br1 3.0493(15) 3_565 ?
Pb2 Br1 3.0493(15) . ?
Br5 Pb1 3.0761(14) 3_666 ?
N2 C2 1.42(2) . ?
N2 C1 1.47(2) . ?
N2 C7 1.61(3) . ?
N2 C2A 1.37(3) . ?
N2 C1A 1.59(3) . ?
N2 C7A 1.46(3) . ?
N1 C5 1.43(2) . ?
N1 C3 1.421(9) . ?
N1 C4 1.46(2) . ?
N1 C3A 1.422(10) . ?
C6 C3 1.52(3) . ?
C6 C2 1.44(3) . ?
C6 C3A 1.42(3) . ?
C6 C2A 1.45(4) . ?

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
Br5 Pb1 Br5 90.29(4) . 3_666 ?
Br3 Pb1 Br5 90.92(4) . 3_666 ?
Br3 Pb1 Br5 84.17(4) . . ?
Br3 Pb1 Br2 93.34(4) . . ?
Br3 Pb1 Br1 91.68(5) . . ?
Br2 Pb1 Br5 91.36(4) . 3_666 ?
Br2 Pb1 Br5 177.03(4) . . ?
Br1 Pb1 Br5 93.18(4) . . ?
Br1 Pb1 Br5 175.86(4) . 3_666 ?
Br1 Pb1 Br2 85.27(5) . . ?
Br4 Pb2 Br4 180.0 3_565 . ?
Br2 Pb2 Br4 96.15(4) . 3_565 ?
Br2 Pb2 Br4 83.85(4) . . ?
Br2 Pb2 Br4 83.84(4) 3_565 3_565 ?
Br2 Pb2 Br4 96.15(4) 3_565 . ?
Br2 Pb2 Br2 180.0 3_565 . ?
Br2 Pb2 Br1 84.13(4) . . ?
Br2 Pb2 Br1 84.13(4) 3_565 3_565 ?
Br2 Pb2 Br1 95.87(4) 3_565 . ?
Br2 Pb2 Br1 95.87(4) . 3_565 ?
Br1 Pb2 Br4 96.84(4) . 3_565 ?
Br1 Pb2 Br4 96.84(4) 3_565 . ?
Br1 Pb2 Br4 83.16(4) 3_565 3_565 ?
Br1 Pb2 Br4 83.16(4) . . ?
Br1 Pb2 Br1 180.0 3_565 . ?
Pb1 Br5 Pb1 89.71(4) . 3_666 ?
Pb1 Br2 Pb2 82.92(4) . . ?
Pb1 Br1 Pb2 82.78(4) . . ?
C2 N2 C1 117.0(19) . . ?
C2 N2 C7 106.9(18) . . ?
C1 N2 C7 105.1(19) . . ?
C2A N2 C1A 110(2) . . ?
C2A N2 C7A 122(2) . . ?
C7A N2 C1A 108(2) . . ?
C5 N1 C4 108.6(14) . . ?
C3 N1 C5 90.7(16) . . ?
C3 N1 C4 134.1(16) . . ?
C3A N1 C5 145.5(17) . . ?
C3A N1 C4 84.2(16) . . ?
C2 C6 C3 116.1(17) . . ?
C3A C6 C2A 126.1(18) . . ?
N1 C3 C6 113.1(16) . . ?
N2 C2 C6 119(2) . . ?
N1 C3A C6 119.0(19) . . ?
N2 C2A C6 122(3) . . ?

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 7.921
_oxdiff_exptl_absorpt_empirical_full_min 0.275
