# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_x
_audit_block_doi                 10.5517/ccdc.csd.cc218mvt
_database_code_depnum_ccdc_archive 'CCDC 1885136'
loop_
_audit_author_name
_audit_author_address
'liaokuo gong'
;Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences
China
;
_audit_update_record             
;
2018-12-14 deposited with the CCDC.	2019-06-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            none
_chemical_melting_point          'not measured'
_chemical_formula_moiety         '(Br12 Pb3),6(C9 H14 N)'
_chemical_formula_sum            'C54 H84 Br12 N6 Pb3'
_chemical_formula_weight         2397.76

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

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 3'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   17.1167(6)
_cell_length_b                   17.1167(6)
_cell_length_c                   21.9553(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     5570.7(5)
_cell_formula_units_Z            3
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3398
_cell_measurement_theta_min      3.9510
_cell_measurement_theta_max      28.5700

_exptl_crystal_description       bulk
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.144
_exptl_crystal_F_000             3348
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_exptl_absorpt_coefficient_mu    13.274
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.52715
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6049
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_av_R_equivalents  0.0194
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         3.663
_diffrn_reflns_theta_max         28.867
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.819
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.819
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.819
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             2672
_reflns_number_gt                2448
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0204P)²+7.5000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2672
_refine_ls_number_parameters     115
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0219
_refine_ls_R_factor_gt           0.0184
_refine_ls_wR_factor_ref         0.0418
_refine_ls_wR_factor_gt          0.0405
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_restrained_S_all      1.001
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.333333 0.666667 0.166667 0.01377(7) Uani 1 6 d S T P . .
Pb2 Pb 0.333333 0.666667 -0.01525(2) 0.01314(6) Uani 1 3 d S T P . .
Br1 Br 0.45854(2) 0.64354(2) 0.08186(2) 0.01744(7) Uani 1 1 d . . . . .
Br2 Br 0.31977(2) 0.51360(2) -0.08036(2) 0.02568(8) Uani 1 1 d . . . . .
N1 N 0.74000(16) 0.66168(16) -0.11112(11) 0.0182(5) Uani 1 1 d . . . . .
C1 C 0.7166(2) 0.7229(2) -0.12632(13) 0.0238(7) Uani 1 1 d . . . . .
H1 H 0.750378 0.767219 -0.156221 0.029 Uiso 1 1 calc R U . . .
C2 C 0.6439(2) 0.7221(2) -0.09896(14) 0.0254(7) Uani 1 1 d . . . . .
H2 H 0.627646 0.765775 -0.109769 0.031 Uiso 1 1 calc R U . . .
C3 C 0.5951(2) 0.6578(2) -0.05600(14) 0.0254(7) Uani 1 1 d . . . . .
H3 H 0.543959 0.655780 -0.037466 0.030 Uiso 1 1 calc R U . . .
C4 C 0.6209(2) 0.5964(2) -0.04003(15) 0.0305(8) Uani 1 1 d . . . . .
H4 H 0.588933 0.552669 -0.009396 0.037 Uiso 1 1 calc R U . . .
C5 C 0.6931(2) 0.5988(2) -0.06869(15) 0.0259(7) Uani 1 1 d . . . . .
H5 H 0.710233 0.555575 -0.058463 0.031 Uiso 1 1 calc R U . . .
C6 C 0.8185(2) 0.6625(2) -0.14072(14) 0.0258(7) Uani 1 1 d . . . . .
H6A H 0.832653 0.696879 -0.179291 0.031 Uiso 1 1 calc R U . . .
H6B H 0.802711 0.599842 -0.150672 0.031 Uiso 1 1 calc R U . . .
C7 C 0.9016(2) 0.7050(2) -0.09940(16) 0.0325(8) Uani 1 1 d . . . . .
H7A H 0.883102 0.681102 -0.057602 0.039 Uiso 1 1 calc R U . . .
H7B H 0.944905 0.686723 -0.113939 0.039 Uiso 1 1 calc R U . . .
C8 C 0.9483(3) 0.8061(3) -0.09727(19) 0.0454(10) Uani 1 1 d . . . . .
H8A H 0.906568 0.825317 -0.081083 0.055 Uiso 1 1 calc R U . . .
H8B H 0.966506 0.830911 -0.138877 0.055 Uiso 1 1 calc R U . . .
C9 C 1.0324(3) 0.8423(4) -0.0560(3) 0.0725(16) Uani 1 1 d . . . . .
H9A H 1.013632 0.821290 -0.014184 0.109 Uiso 1 1 calc R U . . .
H9B H 1.065111 0.908417 -0.056782 0.109 Uiso 1 1 calc R U . . .
H9C H 1.071859 0.820248 -0.070883 0.109 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br1 3.0108(3) 14_455 ?
Pb1 Br1 3.0108(3) 15 ?
Pb1 Br1 3.0109(3) . ?
Pb1 Br1 3.0109(3) 2_665 ?
Pb1 Br1 3.0109(3) 3_565 ?
Pb1 Br1 3.0110(3) 13_565 ?
Pb2 Br2 2.8903(3) 2_665 ?
Pb2 Br2 2.8903(3) . ?
Pb2 Br2 2.8903(3) 3_565 ?
Pb2 Br1 3.1848(3) . ?
Pb2 Br1 3.1849(3) 2_665 ?
Pb2 Br1 3.1849(3) 3_565 ?
N1 C1 1.338(4) . ?
N1 C5 1.344(4) . ?
N1 C6 1.486(4) . ?
C1 C2 1.375(4) . ?
C1 H1 0.9500 . ?
C2 C3 1.370(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.374(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.369(5) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C6 C7 1.531(5) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.500(5) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.545(6) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?

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 85.773(8) 14_455 15 ?
Br1 Pb1 Br1 94.230(8) 14_455 . ?
Br1 Pb1 Br1 94.230(8) 15 . ?
Br1 Pb1 Br1 180.0 14_455 2_665 ?
Br1 Pb1 Br1 94.225(8) 15 2_665 ?
Br1 Pb1 Br1 85.773(8) . 2_665 ?
Br1 Pb1 Br1 94.228(8) 14_455 3_565 ?
Br1 Pb1 Br1 180.0 15 3_565 ?
Br1 Pb1 Br1 85.773(8) . 3_565 ?
Br1 Pb1 Br1 85.774(8) 2_665 3_565 ?
Br1 Pb1 Br1 85.771(8) 14_455 13_565 ?
Br1 Pb1 Br1 85.770(8) 15 13_565 ?
Br1 Pb1 Br1 180.0 . 13_565 ?
Br1 Pb1 Br1 94.226(8) 2_665 13_565 ?
Br1 Pb1 Br1 94.227(8) 3_565 13_565 ?
Br2 Pb2 Br2 97.647(9) 2_665 . ?
Br2 Pb2 Br2 97.647(9) 2_665 3_565 ?
Br2 Pb2 Br2 97.647(9) . 3_565 ?
Br2 Pb2 Br1 92.602(8) 2_665 . ?
Br2 Pb2 Br1 88.422(9) . . ?
Br2 Pb2 Br1 167.260(10) 3_565 . ?
Br2 Pb2 Br1 88.421(9) 2_665 2_665 ?
Br2 Pb2 Br1 167.260(10) . 2_665 ?
Br2 Pb2 Br1 92.603(8) 3_565 2_665 ?
Br1 Pb2 Br1 80.087(9) . 2_665 ?
Br2 Pb2 Br1 167.260(10) 2_665 3_565 ?
Br2 Pb2 Br1 92.602(8) . 3_565 ?
Br2 Pb2 Br1 88.421(8) 3_565 3_565 ?
Br1 Pb2 Br1 80.088(9) . 3_565 ?
Br1 Pb2 Br1 80.088(9) 2_665 3_565 ?
Pb1 Br1 Pb2 80.224(8) . . ?
C1 N1 C5 120.4(3) . . ?
C1 N1 C6 120.5(3) . . ?
C5 N1 C6 119.1(3) . . ?
N1 C1 C2 120.4(3) . . ?
N1 C1 H1 119.8 . . ?
C2 C1 H1 119.8 . . ?
C3 C2 C1 119.6(3) . . ?
C3 C2 H2 120.2 . . ?
C1 C2 H2 120.2 . . ?
C2 C3 C4 119.3(3) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C5 C4 C3 119.3(3) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
N1 C5 C4 120.8(3) . . ?
N1 C5 H5 119.6 . . ?
C4 C5 H5 119.6 . . ?
N1 C6 C7 111.5(3) . . ?
N1 C6 H6A 109.3 . . ?
C7 C6 H6A 109.3 . . ?
N1 C6 H6B 109.3 . . ?
C7 C6 H6B 109.3 . . ?
H6A C6 H6B 108.0 . . ?
C8 C7 C6 113.5(3) . . ?
C8 C7 H7A 108.9 . . ?
C6 C7 H7A 108.9 . . ?
C8 C7 H7B 108.9 . . ?
C6 C7 H7B 108.9 . . ?
H7A C7 H7B 107.7 . . ?
C7 C8 C9 109.5(4) . . ?
C7 C8 H8A 109.8 . . ?
C9 C8 H8A 109.8 . . ?
C7 C8 H8B 109.8 . . ?
C9 C8 H8B 109.8 . . ?
H8A C8 H8B 108.2 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 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
C5 N1 C1 C2 -0.3(4) . . . . ?
C6 N1 C1 C2 179.9(3) . . . . ?
N1 C1 C2 C3 -0.2(5) . . . . ?
C1 C2 C3 C4 1.4(5) . . . . ?
C2 C3 C4 C5 -2.0(5) . . . . ?
C1 N1 C5 C4 -0.3(5) . . . . ?
C6 N1 C5 C4 179.4(3) . . . . ?
C3 C4 C5 N1 1.5(5) . . . . ?
C1 N1 C6 C7 101.6(3) . . . . ?
C5 N1 C6 C7 -78.2(4) . . . . ?
N1 C6 C7 C8 -77.0(4) . . . . ?
C6 C7 C8 C9 -178.4(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C1 H1 Br2 0.95 2.67 3.606(3) 166.7 17_554
C2 H2 Br2 0.95 2.90 3.659(3) 137.7 2_665
C4 H4 Br2 0.95 3.06 3.671(3) 123.2 10_665
C5 H5 Br1 0.95 3.04 3.901(3) 152.1 12_655
C6 H6A Br2 0.99 3.14 4.019(3) 149.2 17_554
C6 H6B Br1 0.99 2.97 3.678(3) 129.4 8_654
C6 H6B Br1 0.99 2.95 3.695(3) 133.1 12_655

_refine_diff_density_max         0.673
_refine_diff_density_min         -0.795
_refine_diff_density_rms         0.103

