# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_exp_11839
_database_code_depnum_ccdc_archive 'CCDC 2264136'
loop_
_audit_author_name
_audit_author_address
'xiao-fan jiang'
;Peking university
China
;
_audit_update_record             
;
2023-07-10 deposited with the CCDC.	2023-07-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H42 Br12 Cl6 N6 Pb3'
_chemical_formula_weight         2351.95

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'
Cl Cl 0.1484 0.1585 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   16.6366(7)
_cell_length_b                   8.0081(4)
_cell_length_c                   23.0142(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.410(4)
_cell_angle_gamma                90.00
_cell_volume                     2955.9(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    102(2)
_cell_measurement_reflns_used    4892
_cell_measurement_theta_min      3.4790
_cell_measurement_theta_max      29.4450

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.643
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2136
_exptl_absorpt_coefficient_mu    16.937
_exptl_absorpt_correction_T_min  0.08097
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      102(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14358
_diffrn_reflns_av_R_equivalents  0.0715
_diffrn_reflns_av_sigmaI/netI    0.0809
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3.51
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5187
_reflns_number_gt                4042
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0725P)²+5.4853P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5187
_refine_ls_number_parameters     253
_refine_ls_number_restraints     151
_refine_ls_R_factor_all          0.0738
_refine_ls_R_factor_gt           0.0565
_refine_ls_wR_factor_ref         0.1510
_refine_ls_wR_factor_gt          0.1366
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.566
_refine_ls_shift/su_max          0.000
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.5000 0.5000 0.5000 0.0053(3) Uani 1 2 d S . .
Pb2 Pb 0.45979(4) 0.00379(8) 0.30068(3) 0.0054(2) Uani 1 1 d . . .
Br3 Br 0.38439(9) 0.2532(2) 0.20780(7) 0.0079(4) Uani 1 1 d . . .
Br4 Br 0.38025(9) -0.2813(2) 0.22485(7) 0.0073(4) Uani 1 1 d . . .
Br6 Br 0.29913(9) 0.0420(2) 0.32850(8) 0.0116(4) Uani 1 1 d . . .
Br7 Br 0.50974(11) 0.2697(3) 0.40204(9) 0.0227(5) Uani 1 1 d . . .
Br8 Br 0.49542(14) 0.7828(3) 0.41685(10) 0.0304(6) Uani 1 1 d U . .
Br9 Br 0.31310(13) 0.5025(4) 0.45969(10) 0.0440(7) Uani 1 1 d U . .
Cl16 Cl -0.0485(3) 0.0757(8) 0.1010(2) 0.0264(12) Uani 1 1 d . . .
Cl24 Cl -0.0420(3) 0.6136(7) 0.1867(2) 0.0258(12) Uani 1 1 d . . .
Cl32 Cl 0.0639(3) 0.8954(8) 0.5694(2) 0.0316(14) Uani 1 1 d . . .
N19 N 0.3099(8) 0.4582(19) 0.3150(7) 0.012(3) Uani 1 1 d U . .
H19A H 0.3443 0.5045 0.2947 0.019 Uiso 1 1 calc R . .
H19B H 0.3170 0.3454 0.3167 0.019 Uiso 1 1 calc R . .
H19C H 0.3222 0.5003 0.3531 0.019 Uiso 1 1 calc R . .
N17 N 0.3064(9) -0.0195(18) 0.1041(7) 0.013(3) Uani 1 1 d U . .
H17A H 0.3112 -0.0153 0.0656 0.015 Uiso 1 1 calc R . .
H17B H 0.3232 -0.1216 0.1202 0.015 Uiso 1 1 calc R . .
H17C H 0.3390 0.0611 0.1266 0.015 Uiso 1 1 calc R . .
N18 N 0.3609(11) 1.002(2) 0.4785(8) 0.025(4) Uani 1 1 d U . .
H18A H 0.3921 1.0906 0.4963 0.038 Uiso 1 1 calc R . .
H18B H 0.3448 1.0176 0.4379 0.038 Uiso 1 1 calc R . .
H18C H 0.3917 0.9070 0.4871 0.038 Uiso 1 1 calc R . .
C15 C 0.1110(6) -0.0080(16) 0.1536(4) 0.014(4) Uani 1 1 d GDU . .
H15 H 0.0923 -0.0364 0.1879 0.017 Uiso 1 1 calc R . .
C14 C 0.1938(6) -0.0339(15) 0.1541(4) 0.019(4) Uani 1 1 d GDU . .
H14 H 0.2317 -0.0799 0.1888 0.023 Uiso 1 1 calc R . .
C13 C 0.2211(5) 0.0076(15) 0.1039(5) 0.010(4) Uani 1 1 d GDU . .
C12 C 0.1657(6) 0.0749(16) 0.0532(4) 0.015(4) Uani 1 1 d GDU . .
H12 H 0.1843 0.1033 0.0189 0.018 Uiso 1 1 calc R . .
C11 C 0.0829(6) 0.1008(16) 0.0527(4) 0.016(4) Uani 1 1 d GDU . .
H11 H 0.0449 0.1468 0.0180 0.019 Uiso 1 1 calc R . .
C10 C 0.0555(5) 0.0593(16) 0.1029(5) 0.008(4) Uani 1 1 d GDU . .
C22 C 0.1866(6) 0.6407(13) 0.2983(5) 0.016(4) Uani 1 1 d GDU . .
H22 H 0.2171 0.7146 0.3284 0.019 Uiso 1 1 calc R . .
C23 C 0.1044(6) 0.6767(12) 0.2681(5) 0.016(4) Uani 1 1 d GDU . .
H23 H 0.0787 0.7751 0.2777 0.019 Uiso 1 1 calc R . .
C18 C 0.0597(5) 0.5687(15) 0.2239(5) 0.017(4) Uani 1 1 d GDU . .
C19 C 0.0974(6) 0.4247(14) 0.2099(5) 0.017(4) Uani 1 1 d GDU . .
H19 H 0.0669 0.3509 0.1797 0.021 Uiso 1 1 calc R . .
C20 C 0.1796(6) 0.3888(12) 0.2401(5) 0.012(4) Uani 1 1 d GDU . .
H20 H 0.2053 0.2904 0.2305 0.015 Uiso 1 1 calc R . .
C21 C 0.2242(5) 0.4968(14) 0.2842(5) 0.013(4) Uani 1 1 d GD . .
C30 C 0.2957(5) 0.9914(16) 0.5623(5) 0.025(5) Uani 1 1 d GU . .
H30 H 0.3484 1.0121 0.5899 0.030 Uiso 1 1 calc R . .
C29 C 0.2885(6) 0.9878(16) 0.5008(5) 0.016(4) Uani 1 1 d GU . .
C28 C 0.2115(7) 0.9575(18) 0.4603(4) 0.023(5) Uani 1 1 d G . .
H28 H 0.2066 0.9550 0.4183 0.028 Uiso 1 1 calc R . .
C27 C 0.1417(5) 0.9308(19) 0.4815(5) 0.028(5) Uani 1 1 d GU . .
H27 H 0.0890 0.9101 0.4539 0.033 Uiso 1 1 calc R . .
C26 C 0.1489(6) 0.9345(18) 0.5431(5) 0.018(4) Uani 1 1 d G . .
C31 C 0.2259(7) 0.9648(17) 0.5835(4) 0.020(4) Uani 1 1 d GU . .
H31 H 0.2308 0.9673 0.6255 0.024 Uiso 1 1 calc R . .


_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 Br7 2.9502(18) 3_666 ?
Pb1 Br7 2.9502(18) . ?
Pb1 Br8 2.953(2) 3_666 ?
Pb1 Br8 2.953(2) . ?
Pb1 Br9 2.999(2) . ?
Pb1 Br9 2.999(2) 3_666 ?
Pb2 Br6 2.9251(16) . ?
Pb2 Br3 2.9510(18) . ?
Pb2 Br4 2.9633(18) . ?
Pb2 Br7 3.104(2) . ?
Pb2 Br8 3.129(2) 1_545 ?
Br8 Pb2 3.129(2) 1_565 ?
Cl16 C10 1.725(8) . ?
Cl24 C18 1.719(8) . ?
Cl32 C26 1.709(9) . ?
N19 C21 1.446(15) . ?
N19 H19A 0.9100 . ?
N19 H19B 0.9100 . ?
N19 H19C 0.9100 . ?
N17 C13 1.434(15) . ?
N17 H17A 0.9100 . ?
N17 H17B 0.9100 . ?
N17 H17C 0.9100 . ?
N18 C29 1.433(18) . ?
N18 H18A 0.9100 . ?
N18 H18B 0.9100 . ?
N18 H18C 0.9100 . ?
C15 C14 1.3900 . ?
C15 C10 1.3900 . ?
C15 H15 0.9500 . ?
C14 C13 1.3900 . ?
C14 H14 0.9500 . ?
C13 C12 1.3900 . ?
C12 C11 1.3900 . ?
C12 H12 0.9500 . ?
C11 C10 1.3900 . ?
C11 H11 0.9500 . ?
C22 C23 1.3900 . ?
C22 C21 1.3900 . ?
C22 H22 0.9500 . ?
C23 C18 1.3900 . ?
C23 H23 0.9500 . ?
C18 C19 1.3900 . ?
C19 C20 1.3900 . ?
C19 H19 0.9500 . ?
C20 C21 1.3900 . ?
C20 H20 0.9500 . ?
C30 C29 1.3900 . ?
C30 C31 1.3900 . ?
C30 H30 0.9500 . ?
C29 C28 1.3900 . ?
C28 C27 1.3900 . ?
C28 H28 0.9500 . ?
C27 C26 1.3900 . ?
C27 H27 0.9500 . ?
C26 C31 1.3900 . ?
C31 H31 0.9500 . ?

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
Br7 Pb1 Br7 180.0 3_666 . ?
Br7 Pb1 Br8 88.93(6) 3_666 3_666 ?
Br7 Pb1 Br8 91.07(6) . 3_666 ?
Br7 Pb1 Br8 91.07(6) 3_666 . ?
Br7 Pb1 Br8 88.93(6) . . ?
Br8 Pb1 Br8 180.00(7) 3_666 . ?
Br7 Pb1 Br9 88.24(6) 3_666 . ?
Br7 Pb1 Br9 91.76(6) . . ?
Br8 Pb1 Br9 92.97(7) 3_666 . ?
Br8 Pb1 Br9 87.03(7) . . ?
Br7 Pb1 Br9 91.76(6) 3_666 3_666 ?
Br7 Pb1 Br9 88.24(6) . 3_666 ?
Br8 Pb1 Br9 87.03(7) 3_666 3_666 ?
Br8 Pb1 Br9 92.97(7) . 3_666 ?
Br9 Pb1 Br9 180.0 . 3_666 ?
Br6 Pb2 Br3 81.40(5) . . ?
Br6 Pb2 Br4 85.33(5) . . ?
Br3 Pb2 Br4 93.30(5) . . ?
Br6 Pb2 Br7 80.88(5) . . ?
Br3 Pb2 Br7 93.29(6) . . ?
Br4 Pb2 Br7 163.64(5) . . ?
Br6 Pb2 Br8 81.31(5) . 1_545 ?
Br3 Pb2 Br8 161.70(5) . 1_545 ?
Br4 Pb2 Br8 91.20(6) . 1_545 ?
Br7 Pb2 Br8 78.10(6) . 1_545 ?
Pb1 Br7 Pb2 160.90(6) . . ?
Pb1 Br8 Pb2 162.56(9) . 1_565 ?
C21 N19 H19A 109.5 . . ?
C21 N19 H19B 109.5 . . ?
H19A N19 H19B 109.5 . . ?
C21 N19 H19C 109.5 . . ?
H19A N19 H19C 109.5 . . ?
H19B N19 H19C 109.5 . . ?
C13 N17 H17A 109.5 . . ?
C13 N17 H17B 109.5 . . ?
H17A N17 H17B 109.5 . . ?
C13 N17 H17C 109.5 . . ?
H17A N17 H17C 109.5 . . ?
H17B N17 H17C 109.5 . . ?
C29 N18 H18A 109.5 . . ?
C29 N18 H18B 109.5 . . ?
H18A N18 H18B 109.5 . . ?
C29 N18 H18C 109.5 . . ?
H18A N18 H18C 109.5 . . ?
H18B N18 H18C 109.5 . . ?
C14 C15 C10 120.0 . . ?
C14 C15 H15 120.0 . . ?
C10 C15 H15 120.0 . . ?
C15 C14 C13 120.0 . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C12 C13 C14 120.0 . . ?
C12 C13 N17 119.8(9) . . ?
C14 C13 N17 120.2(9) . . ?
C13 C12 C11 120.0 . . ?
C13 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
C10 C11 C12 120.0 . . ?
C10 C11 H11 120.0 . . ?
C12 C11 H11 120.0 . . ?
C11 C10 C15 120.0 . . ?
C11 C10 Cl16 120.6(6) . . ?
C15 C10 Cl16 119.2(6) . . ?
C23 C22 C21 120.0 . . ?
C23 C22 H22 120.0 . . ?
C21 C22 H22 120.0 . . ?
C18 C23 C22 120.0 . . ?
C18 C23 H23 120.0 . . ?
C22 C23 H23 120.0 . . ?
C19 C18 C23 120.0 . . ?
C19 C18 Cl24 120.1(7) . . ?
C23 C18 Cl24 119.9(7) . . ?
C20 C19 C18 120.0 . . ?
C20 C19 H19 120.0 . . ?
C18 C19 H19 120.0 . . ?
C19 C20 C21 120.0 . . ?
C19 C20 H20 120.0 . . ?
C21 C20 H20 120.0 . . ?
C20 C21 C22 120.0 . . ?
C20 C21 N19 119.4(9) . . ?
C22 C21 N19 120.6(9) . . ?
C29 C30 C31 120.0 . . ?
C29 C30 H30 120.0 . . ?
C31 C30 H30 120.0 . . ?
C28 C29 C30 120.0 . . ?
C28 C29 N18 119.2(11) . . ?
C30 C29 N18 120.7(11) . . ?
C29 C28 C27 120.0 . . ?
C29 C28 H28 120.0 . . ?
C27 C28 H28 120.0 . . ?
C26 C27 C28 120.0 . . ?
C26 C27 H27 120.0 . . ?
C28 C27 H27 120.0 . . ?
C27 C26 C31 120.0 . . ?
C27 C26 Cl32 120.2(7) . . ?
C31 C26 Cl32 119.8(7) . . ?
C26 C31 C30 120.0 . . ?
C26 C31 H31 120.0 . . ?
C30 C31 H31 120.0 . . ?

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
Br7 Pb1 Br7 Pb2 -97(17) 3_666 . . . ?
Br8 Pb1 Br7 Pb2 72.0(3) 3_666 . . . ?
Br8 Pb1 Br7 Pb2 -108.0(3) . . . . ?
Br9 Pb1 Br7 Pb2 -21.0(3) . . . . ?
Br9 Pb1 Br7 Pb2 159.0(3) 3_666 . . . ?
Br6 Pb2 Br7 Pb1 5.2(3) . . . . ?
Br3 Pb2 Br7 Pb1 86.0(3) . . . . ?
Br4 Pb2 Br7 Pb1 -27.6(4) . . . . ?
Br8 Pb2 Br7 Pb1 -77.7(3) 1_545 . . . ?
Br7 Pb1 Br8 Pb2 -144.9(3) 3_666 . . 1_565 ?
Br7 Pb1 Br8 Pb2 35.1(3) . . . 1_565 ?
Br8 Pb1 Br8 Pb2 35(18) 3_666 . . 1_565 ?
Br9 Pb1 Br8 Pb2 -56.7(2) . . . 1_565 ?
Br9 Pb1 Br8 Pb2 123.3(2) 3_666 . . 1_565 ?
C10 C15 C14 C13 0.0 . . . . ?
C15 C14 C13 C12 0.0 . . . . ?
C15 C14 C13 N17 -179.7(12) . . . . ?
C14 C13 C12 C11 0.0 . . . . ?
N17 C13 C12 C11 179.7(12) . . . . ?
C13 C12 C11 C10 0.0 . . . . ?
C12 C11 C10 C15 0.0 . . . . ?
C12 C11 C10 Cl16 -175.1(10) . . . . ?
C14 C15 C10 C11 0.0 . . . . ?
C14 C15 C10 Cl16 175.1(10) . . . . ?
C21 C22 C23 C18 0.0 . . . . ?
C22 C23 C18 C19 0.0 . . . . ?
C22 C23 C18 Cl24 -180.0(9) . . . . ?
C23 C18 C19 C20 0.0 . . . . ?
Cl24 C18 C19 C20 180.0(9) . . . . ?
C18 C19 C20 C21 0.0 . . . . ?
C19 C20 C21 C22 0.0 . . . . ?
C19 C20 C21 N19 -179.7(12) . . . . ?
C23 C22 C21 C20 0.0 . . . . ?
C23 C22 C21 N19 179.7(12) . . . . ?
C31 C30 C29 C28 0.0 . . . . ?
C31 C30 C29 N18 -175.1(13) . . . . ?
C30 C29 C28 C27 0.0 . . . . ?
N18 C29 C28 C27 175.2(13) . . . . ?
C29 C28 C27 C26 0.0 . . . . ?
C28 C27 C26 C31 0.0 . . . . ?
C28 C27 C26 Cl32 -178.0(11) . . . . ?
C27 C26 C31 C30 0.0 . . . . ?
Cl32 C26 C31 C30 178.0(11) . . . . ?
C29 C30 C31 C26 0.0 . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         6.709
_refine_diff_density_min         -4.728
_refine_diff_density_rms         0.394
