# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1880856'
loop_
_audit_author_name
_audit_author_address
'Mingjun Xia'
;Technical Institute of Physics and Chemistry
China
;
_audit_update_record             
;
2019-05-14 deposited with the CCDC.	2019-05-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 Cl54 K12 N60 Pb51'
_chemical_formula_weight         14151.09

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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'
C C 0.0033 0.0016 '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'

_space_group_crystal_system      trigonal
_space_group_IT_number           166
_space_group_name_H-M_alt        'R -3 m :H'
_space_group_name_Hall           '-R 3 2"'

_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'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -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'
'y+2/3, x+1/3, -z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+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'
'y+1/3, x+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, 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'
'-y+2/3, -x+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'x+2/3, x-y+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'
'-y+1/3, -x+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'

_cell_length_a                   10.3072(4)
_cell_length_b                   10.3072(4)
_cell_length_c                   45.528(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4188.8(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    4992
_cell_measurement_theta_min      3.2300
_cell_measurement_theta_max      31.1690

_exptl_crystal_description       Prism
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    5.610
_exptl_crystal_F_000             5928
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_exptl_absorpt_coefficient_mu    52.226
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.42321
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  Rigaku
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            37495
_diffrn_reflns_av_unetI/netI     0.0133
_diffrn_reflns_av_R_equivalents  0.0603
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_theta_min         2.900
_diffrn_reflns_theta_max         26.359
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             1122
_reflns_number_gt                1109
_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-2017/1 (Sheldrick, 2017)'
_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)+(0.0269P)²+150.9609P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1122
_refine_ls_number_parameters     78
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0221
_refine_ls_R_factor_gt           0.0217
_refine_ls_wR_factor_ref         0.0530
_refine_ls_wR_factor_gt          0.0527
_refine_ls_goodness_of_fit_ref   1.162
_refine_ls_restrained_S_all      1.162
_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 0.13212(2) 0.86788(2) 0.20176(2) 0.00803(11) Uani 1 2 d S T P . .
Pb2 Pb 0.54138(2) 0.08275(4) 0.28049(2) 0.01203(11) Uani 1 2 d S T P . .
Pb3 Pb 0.000000 0.000000 0.12979(2) 0.00848(13) Uani 1 6 d S T P . .
Pb4 Pb 0.000000 0.000000 0.27164(2) 0.01042(14) Uani 1 6 d S T P . .
Pb5 Pb 0.166667 0.833333 0.333333 0.0086(2) Uani 0.33 4 d S T P . .
K5 K 0.166667 0.833333 0.333333 0.0086(2) Uani 0.67 4 d S T P . .
K1 K 0.333333 0.666667 0.23257(6) 0.0036(5) Uani 1 6 d S T P . .
Cl1 Cl 0.19359(13) 0.80641(13) 0.26972(5) 0.0172(5) Uani 1 2 d S T P . .
Cl2 Cl 0.48777(14) 0.51223(14) 0.20335(5) 0.0209(5) Uani 1 2 d S T P . .
Cl3 Cl -0.14678(15) 0.7064(3) 0.31714(5) 0.0199(5) Uani 1 2 d S T P . .
C1 C -0.166667 0.666667 0.166667 0.006(2) Uani 1 4 d S T P . .
C2 C 0.8363(5) 0.1637(5) 0.24342(16) 0.0076(16) Uani 1 2 d S T P . .
C3 C 0.666667 0.333333 0.333333 0.012(4) Uani 1 12 d S T P . .
N1 N 0.7697(4) 0.2303(4) 0.25105(15) 0.0084(14) Uani 1 2 d S T P . .
N2 N -0.0988(4) 0.8024(8) 0.17183(14) 0.0056(13) Uani 1 2 d S T P . .
N3 N -0.0984(4) 0.8033(8) 0.23505(15) 0.0090(14) Uani 1 2 d S T P . .
N4 N 0.666667 0.333333 0.3064(3) 0.007(2) Uani 1 6 d S T P . .


_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 N2 2.524(4) 2_675 ?
Pb1 N2 2.524(4) . ?
Pb1 N3 2.608(4) 2_675 ?
Pb1 N3 2.608(4) . ?
Pb1 K1 3.8563(11) . ?
Pb2 N1 2.463(4) . ?
Pb2 N1 2.464(4) 3_665 ?
Pb2 N4 2.529(5) . ?
Pb2 K5 4.1695(3) 3 ?
Pb2 K5 4.1696(3) 1_545 ?
Pb2 K1 4.3076(15) 1_545 ?
Pb3 N2 2.603(7) 2_665 ?
Pb3 N2 2.603(6) 3_455 ?
Pb3 N2 2.603(6) 1_545 ?
Pb4 N3 2.420(7) 1_545 ?
Pb4 N3 2.420(7) 3_455 ?
Pb4 N3 2.420(7) 2_665 ?
Pb4 K5 4.0919(4) 1_545 ?
Pb4 K5 4.0920(4) 2_665 ?
Pb4 K5 4.0920(4) 3_455 ?
Pb5 Cl3 2.9097(12) 2_675 ?
Pb5 Cl3 2.9098(12) . ?
Pb5 Cl3 2.9098(12) 31_565 ?
Pb5 Cl3 2.9098(12) 32_445 ?
Pb5 Cl1 2.936(2) . ?
Pb5 Cl1 2.936(2) 31_565 ?
K1 Cl1 3.014(3) 3_565 ?
K1 Cl1 3.014(3) 2_665 ?
K1 Cl1 3.014(3) . ?
K1 Cl2 3.061(3) 3_565 ?
K1 Cl2 3.061(3) 2_665 ?
K1 Cl2 3.061(3) . ?
C1 N2 1.234(7) 25_465 ?
C1 N2 1.234(7) . ?
C2 N3 1.228(11) 3 ?
C2 N1 1.238(11) . ?
C3 N4 1.227(12) . ?
C3 N4 1.227(12) 31_655 ?

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
N2 Pb1 N2 74.5(3) 2_675 . ?
N2 Pb1 N3 68.20(18) 2_675 2_675 ?
N2 Pb1 N3 109.5(2) . 2_675 ?
N2 Pb1 N3 109.5(2) 2_675 . ?
N2 Pb1 N3 68.21(18) . . ?
N3 Pb1 N3 71.3(3) 2_675 . ?
N2 Pb1 K1 137.84(15) 2_675 . ?
N2 Pb1 K1 137.84(15) . . ?
N3 Pb1 K1 108.51(13) 2_675 . ?
N3 Pb1 K1 108.51(13) . . ?
N1 Pb2 N1 80.5(3) . 3_665 ?
N1 Pb2 N4 77.3(2) . . ?
N1 Pb2 N4 77.3(2) 3_665 . ?
N1 Pb2 K5 101.54(16) . 3 ?
N1 Pb2 K5 177.51(15) 3_665 3 ?
N4 Pb2 K5 101.73(18) . 3 ?
N1 Pb2 K5 177.51(15) . 1_545 ?
N1 Pb2 K5 101.54(16) 3_665 1_545 ?
N4 Pb2 K5 101.73(18) . 1_545 ?
K5 Pb2 K5 76.341(6) 3 1_545 ?
N1 Pb2 K1 100.69(13) . 1_545 ?
N1 Pb2 K1 100.69(14) 3_665 1_545 ?
N4 Pb2 K1 177.4(2) . 1_545 ?
K5 Pb2 K1 80.32(3) 3 1_545 ?
K5 Pb2 K1 80.32(3) 1_545 1_545 ?
N2 Pb3 N2 71.9(2) 2_665 3_455 ?
N2 Pb3 N2 71.9(2) 2_665 1_545 ?
N2 Pb3 N2 71.9(2) 3_455 1_545 ?
N3 Pb4 N3 77.9(3) 1_545 3_455 ?
N3 Pb4 N3 77.9(3) 1_545 2_665 ?
N3 Pb4 N3 77.9(3) 3_455 2_665 ?
N3 Pb4 K5 102.04(13) 1_545 1_545 ?
N3 Pb4 K5 179.87(18) 3_455 1_545 ?
N3 Pb4 K5 102.04(13) 2_665 1_545 ?
N3 Pb4 K5 179.87(16) 1_545 2_665 ?
N3 Pb4 K5 102.04(13) 3_455 2_665 ?
N3 Pb4 K5 102.04(13) 2_665 2_665 ?
K5 Pb4 K5 78.059(9) 1_545 2_665 ?
N3 Pb4 K5 102.04(13) 1_545 3_455 ?
N3 Pb4 K5 102.04(13) 3_455 3_455 ?
N3 Pb4 K5 179.87(16) 2_665 3_455 ?
K5 Pb4 K5 78.059(9) 1_545 3_455 ?
K5 Pb4 K5 78.058(9) 2_665 3_455 ?
Cl3 Pb5 Cl3 102.51(10) 2_675 . ?
Cl3 Pb5 Cl3 77.49(10) 2_675 31_565 ?
Cl3 Pb5 Cl3 180.00(3) . 31_565 ?
Cl3 Pb5 Cl3 180.0 2_675 32_445 ?
Cl3 Pb5 Cl3 77.50(10) . 32_445 ?
Cl3 Pb5 Cl3 102.50(10) 31_565 32_445 ?
Cl3 Pb5 Cl1 81.01(5) 2_675 . ?
Cl3 Pb5 Cl1 81.01(5) . . ?
Cl3 Pb5 Cl1 98.99(5) 31_565 . ?
Cl3 Pb5 Cl1 98.99(5) 32_445 . ?
Cl3 Pb5 Cl1 98.99(5) 2_675 31_565 ?
Cl3 Pb5 Cl1 98.99(5) . 31_565 ?
Cl3 Pb5 Cl1 81.01(5) 31_565 31_565 ?
Cl3 Pb5 Cl1 81.01(5) 32_445 31_565 ?
Cl1 Pb5 Cl1 180.00(5) . 31_565 ?
Cl1 K1 Cl1 91.58(9) 3_565 2_665 ?
Cl1 K1 Cl1 91.58(9) 3_565 . ?
Cl1 K1 Cl1 91.58(9) 2_665 . ?
Cl1 K1 Cl2 171.61(12) 3_565 3_565 ?
Cl1 K1 Cl2 82.59(4) 2_665 3_565 ?
Cl1 K1 Cl2 82.59(4) . 3_565 ?
Cl1 K1 Cl2 82.59(4) 3_565 2_665 ?
Cl1 K1 Cl2 171.61(12) 2_665 2_665 ?
Cl1 K1 Cl2 82.59(4) . 2_665 ?
Cl2 K1 Cl2 102.52(8) 3_565 2_665 ?
Cl1 K1 Cl2 82.60(4) 3_565 . ?
Cl1 K1 Cl2 82.60(4) 2_665 . ?
Cl1 K1 Cl2 171.61(12) . . ?
Cl2 K1 Cl2 102.52(8) 3_565 . ?
Cl2 K1 Cl2 102.52(8) 2_665 . ?
Cl1 K1 Pb1 126.128(17) 3_565 . ?
Cl1 K1 Pb1 126.128(17) 2_665 . ?
Cl1 K1 Pb1 55.47(4) . . ?
Cl2 K1 Pb1 54.72(2) 3_565 . ?
Cl2 K1 Pb1 54.72(2) 2_665 . ?
Cl2 K1 Pb1 132.92(10) . . ?
Cl1 K1 Pb1 126.130(17) 3_565 2_665 ?
Cl1 K1 Pb1 55.47(5) 2_665 2_665 ?
Cl1 K1 Pb1 126.130(17) . 2_665 ?
Cl2 K1 Pb1 54.72(2) 3_565 2_665 ?
Cl2 K1 Pb1 132.92(10) 2_665 2_665 ?
Cl2 K1 Pb1 54.72(2) . 2_665 ?
Pb1 K1 Pb1 107.55(4) . 2_665 ?
Cl1 K1 Pb1 55.47(5) 3_565 3_565 ?
Cl1 K1 Pb1 126.131(17) 2_665 3_565 ?
Cl1 K1 Pb1 126.130(17) . 3_565 ?
Cl2 K1 Pb1 132.92(10) 3_565 3_565 ?
Cl2 K1 Pb1 54.72(2) 2_665 3_565 ?
Cl2 K1 Pb1 54.72(2) . 3_565 ?
Pb1 K1 Pb1 107.55(4) . 3_565 ?
Pb1 K1 Pb1 107.55(4) 2_665 3_565 ?
Cl1 K1 Pb2 50.13(2) 3_565 3_665 ?
Cl1 K1 Pb2 50.13(2) 2_665 3_665 ?
Cl1 K1 Pb2 115.43(9) . 3_665 ?
Cl2 K1 Pb2 127.47(2) 3_565 3_665 ?
Cl2 K1 Pb2 127.47(2) 2_665 3_665 ?
Cl2 K1 Pb2 56.18(5) . 3_665 ?
Pb1 K1 Pb2 170.90(7) . 3_665 ?
Pb1 K1 Pb2 77.445(8) 2_665 3_665 ?
Pb1 K1 Pb2 77.445(8) 3_565 3_665 ?
Cl1 K1 Pb2 50.13(2) 3_565 1_565 ?
Cl1 K1 Pb2 115.43(9) 2_665 1_565 ?
Cl1 K1 Pb2 50.13(2) . 1_565 ?
Cl2 K1 Pb2 127.47(2) 3_565 1_565 ?
Cl2 K1 Pb2 56.18(5) 2_665 1_565 ?
Cl2 K1 Pb2 127.47(2) . 1_565 ?
Pb1 K1 Pb2 77.444(8) . 1_565 ?
Pb1 K1 Pb2 170.90(7) 2_665 1_565 ?
Pb1 K1 Pb2 77.445(8) 3_565 1_565 ?
Pb2 K1 Pb2 96.62(4) 3_665 1_565 ?
Cl1 K1 Pb2 115.43(9) 3_565 2 ?
Cl1 K1 Pb2 50.13(2) 2_665 2 ?
Cl1 K1 Pb2 50.13(2) . 2 ?
Cl2 K1 Pb2 56.18(5) 3_565 2 ?
Cl2 K1 Pb2 127.47(2) 2_665 2 ?
Cl2 K1 Pb2 127.47(2) . 2 ?
Pb1 K1 Pb2 77.444(8) . 2 ?
Pb1 K1 Pb2 77.445(8) 2_665 2 ?
Pb1 K1 Pb2 170.90(7) 3_565 2 ?
Pb2 K1 Pb2 96.62(4) 3_665 2 ?
Pb2 K1 Pb2 96.62(4) 1_565 2 ?
Pb5 Cl1 K1 133.56(10) . . ?
Pb5 Cl3 Pb5 124.64(9) . 3_465 ?
N2 C1 N2 180.0 25_465 . ?
N3 C2 N1 178.2(8) 3 . ?
N4 C3 N4 180.0 . 31_655 ?
C2 N1 Pb2 115.7(3) . 2_655 ?
C2 N1 Pb2 115.7(3) . . ?
Pb2 N1 Pb2 103.7(3) 2_655 . ?
C1 N2 Pb1 109.3(2) . 3_465 ?
C1 N2 Pb1 109.3(2) . . ?
Pb1 N2 Pb1 108.0(2) 3_465 . ?
C1 N2 Pb3 121.7(4) . 1_565 ?
Pb1 N2 Pb3 103.88(18) 3_465 1_565 ?
Pb1 N2 Pb3 103.88(18) . 1_565 ?
C2 N3 Pb4 118.4(5) 2 1_565 ?
C2 N3 Pb1 113.0(3) 2 . ?
Pb4 N3 Pb1 103.9(2) 1_565 . ?
C2 N3 Pb1 113.0(3) 2 3_465 ?
Pb4 N3 Pb1 103.9(2) 1_565 3_465 ?
Pb1 N3 Pb1 103.1(2) . 3_465 ?
C3 N4 Pb2 117.8(2) . . ?
C3 N4 Pb2 117.8(2) . 2_655 ?
Pb2 N4 Pb2 100.0(3) . 2_655 ?
C3 N4 Pb2 117.8(2) . 3_665 ?
Pb2 N4 Pb2 100.0(3) . 3_665 ?
Pb2 N4 Pb2 100.0(3) 2_655 3_665 ?

_refine_diff_density_max         1.675
_refine_diff_density_min         -2.245
_refine_diff_density_rms         0.336

