# Supplementary Information (SI) for ChemComm.
# This journal is © The Royal Society of Chemistry 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_(MHEA)4Pb3Br10
_database_code_depnum_ccdc_archive 'CCDC 2391828'
loop_
_audit_author_name
_audit_author_address
'Wei Wang'
;Southeast University
China
;
_audit_update_record             
;
2024-10-18 deposited with the CCDC.	2024-11-25 downloaded from the CCDC.
;
_audit_creation_date             2023-12-25
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br10 Pb3, 4(C3 H10 N O)'
_chemical_formula_sum            'C12 H40 Br10 N4 O4 Pb3'
_chemical_formula_weight         1725.15
_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'
O O 0.0106 0.0060 '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           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   23.6054(10)
_cell_length_b                   8.6447(3)
_cell_length_c                   20.0369(9)
_cell_angle_alpha                90
_cell_angle_beta                 111.785(5)
_cell_angle_gamma                90
_cell_volume                     3796.8(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9284
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.6260
_cell_measurement_theta_min      2.1910
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    23.817
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.12273
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.84a (Rigaku Oxford Diffraction, 2023)
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    3.018
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3072
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0814
_diffrn_reflns_av_unetI/netI     0.0447
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            18759
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         2.189
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -13.00  36.00   0.50    1.60    --    4.83 -99.00   0.00   98
  2  ω    -35.00   7.00   0.50    1.60    --    4.83 -77.00 150.00   84
  3  ω     -8.00  69.00   0.50    1.60    --    4.83  38.00 120.00  154
  4  ω     10.00  77.00   0.50    1.60    --    4.83  57.00 -30.00  134
  5  ω    -15.00  78.00   0.50    1.60    --    4.83  77.00-150.00  186
  6  ω     -8.00  35.00   0.50    1.60    --   -5.61  38.00-180.00   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0245537000
_diffrn_orient_matrix_UB_12      -0.0445655000
_diffrn_orient_matrix_UB_13      0.0019776000
_diffrn_orient_matrix_UB_21      0.0125899000
_diffrn_orient_matrix_UB_22      -0.0673752000
_diffrn_orient_matrix_UB_23      -0.0093053000
_diffrn_orient_matrix_UB_31      0.0168826000
_diffrn_orient_matrix_UB_32      -0.0145993000
_diffrn_orient_matrix_UB_33      0.0369073000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2811
_reflns_number_total             3338
_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 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         1.893
_refine_diff_density_min         -1.631
_refine_diff_density_rms         0.225
_refine_ls_extinction_coef       0.00034(3)
_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   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         3338
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0403
_refine_ls_restrained_S_all      1.079
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0673P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1072
_refine_ls_wR_factor_ref         0.1112
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 H1-H2C
 2.2 with sigma of 0.02
2.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), N2(H2C,H2D), C5(H5A,H5B), C6(H6A,H6B)
2.b Idealised Me refined as rotating group:
 C1(H1C,H1D,H1E), C4(H4A,H4B,H4C)
2.c Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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 -0.17865(2) 0.89630(4) 0.20902(2) 0.03645(17) Uani 1 1 d . . . . .
Pb2 Pb 0.000000 0.87986(6) 0.250000 0.04232(19) Uani 1 2 d S T P . .
Br1 Br -0.05835(6) 0.85219(16) 0.36109(6) 0.0666(4) Uani 1 1 d . . . . .
Br2 Br -0.09754(5) 1.12730(11) 0.18430(6) 0.0509(3) Uani 1 1 d . . . . .
Br3 Br -0.09988(6) 0.66220(13) 0.16480(6) 0.0582(3) Uani 1 1 d . . . . .
Br4 Br -0.26629(5) 0.92188(13) 0.06676(5) 0.0549(3) Uani 1 1 d . . . . .
Br5 Br -0.23939(5) 1.13758(12) 0.26477(6) 0.0520(3) Uani 1 1 d . . . . .
O1 O -0.1014(5) 1.1404(12) 0.4417(5) 0.094(3) Uani 1 1 d . . . . .
H1 H -0.134069 1.167827 0.411308 0.141 Uiso 1 1 calc DR U . . .
N1 N -0.2186(4) 1.0064(9) 0.4310(4) 0.050(2) Uani 1 1 d . . . . .
H1A H -0.215142 1.061924 0.395346 0.060 Uiso 1 1 calc R U . . .
H1B H -0.231233 1.069505 0.457758 0.060 Uiso 1 1 calc R U . . .
C1 C -0.2651(5) 0.8856(12) 0.4003(6) 0.059(3) Uani 1 1 d . . . . .
H1C H -0.302368 0.932611 0.369207 0.089 Uiso 1 1 calc R U . . .
H1D H -0.272095 0.831717 0.438386 0.089 Uiso 1 1 calc R U . . .
H1E H -0.250969 0.813954 0.373269 0.089 Uiso 1 1 calc R U . . .
C2 C -0.1581(5) 0.9456(13) 0.4755(6) 0.059(3) Uani 1 1 d . . . . .
H2A H -0.145607 0.869680 0.448029 0.070 Uiso 1 1 calc R U . . .
H2B H -0.160668 0.893985 0.517269 0.070 Uiso 1 1 calc R U . . .
C3 C -0.1117(7) 1.0702(17) 0.4994(7) 0.081(4) Uani 1 1 d . . . . .
H3A H -0.125157 1.148103 0.525071 0.098 Uiso 1 1 calc R U . . .
H3B H -0.073679 1.027185 0.532371 0.098 Uiso 1 1 calc R U . . .
O2 O 0.0536(5) 1.5173(13) 0.4682(5) 0.095(3) Uani 1 1 d . . . . .
H2 H 0.070685 1.568629 0.446701 0.143 Uiso 1 1 calc R U . . .
N2 N -0.0646(5) 1.4235(14) 0.3869(5) 0.084(3) Uani 1 1 d . . . . .
H2C H -0.072238 1.362233 0.418273 0.100 Uiso 1 1 calc DR U . . .
H2D H -0.054297 1.515790 0.407472 0.100 Uiso 1 1 calc R U . . .
C4 C -0.1188(6) 1.4403(17) 0.3266(8) 0.088(4) Uani 1 1 d . . . . .
H4A H -0.126029 1.348198 0.297850 0.132 Uiso 1 1 calc R U . . .
H4B H -0.115151 1.527196 0.298640 0.132 Uiso 1 1 calc R U . . .
H4C H -0.152226 1.456922 0.342071 0.132 Uiso 1 1 calc R U . . .
C5 C -0.0114(7) 1.3596(16) 0.3736(8) 0.079(4) Uani 1 1 d . . . . .
H5A H -0.019305 1.252890 0.357951 0.095 Uiso 1 1 calc R U . . .
H5B H -0.004809 1.418261 0.335812 0.095 Uiso 1 1 calc R U . . .
C6 C 0.0425(7) 1.3681(17) 0.4391(8) 0.084(4) Uani 1 1 d . . . . .
H6A H 0.037521 1.298187 0.474410 0.101 Uiso 1 1 calc R U . . .
H6B H 0.077599 1.333768 0.428991 0.101 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 Br2 2.9331(10) . ?
Pb1 Br3 3.0920(11) . ?
Pb1 Br4 2.8419(11) . ?
Pb1 Br5 2.9737(10) . ?
Pb1 Br5 3.1265(10) 4_445 ?
Pb2 Br1 3.0307(11) . ?
Pb2 Br1 3.0307(11) 2 ?
Pb2 Br2 3.0595(12) . ?
Pb2 Br2 3.0595(12) 2 ?
Pb2 Br3 3.0044(12) 2 ?
Pb2 Br3 3.0044(12) . ?
O1 H1 0.8200 . ?
O1 C3 1.405(14) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C1 1.473(13) . ?
N1 C2 1.470(13) . ?
C1 H1C 0.9600 . ?
C1 H1D 0.9600 . ?
C1 H1E 0.9600 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C3 1.484(17) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
O2 H2 0.8200 . ?
O2 C6 1.400(15) . ?
N2 H2C 0.8900 . ?
N2 H2D 0.8900 . ?
N2 C4 1.403(15) . ?
N2 C5 1.484(16) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.452(18) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?

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
Br2 Pb1 Br3 84.12(3) . . ?
Br2 Pb1 Br5 177.21(3) . 4_445 ?
Br2 Pb1 Br5 91.25(3) . . ?
Br3 Pb1 Br5 93.17(3) . 4_445 ?
Br4 Pb1 Br2 93.18(3) . . ?
Br4 Pb1 Br3 93.14(3) . . ?
Br4 Pb1 Br5 87.63(3) . 4_445 ?
Br4 Pb1 Br5 92.82(3) . . ?
Br5 Pb1 Br3 172.64(3) . . ?
Br5 Pb1 Br5 91.375(10) . 4_445 ?
Br1 Pb2 Br1 170.94(6) . 2 ?
Br1 Pb2 Br2 84.06(3) 2 2 ?
Br1 Pb2 Br2 102.35(3) . 2 ?
Br1 Pb2 Br2 102.34(3) 2 . ?
Br1 Pb2 Br2 84.07(3) . . ?
Br2 Pb2 Br2 91.28(4) . 2 ?
Br3 Pb2 Br1 83.87(3) . . ?
Br3 Pb2 Br1 83.86(3) 2 2 ?
Br3 Pb2 Br1 90.46(3) . 2 ?
Br3 Pb2 Br1 90.46(3) 2 . ?
Br3 Pb2 Br2 83.50(3) . . ?
Br3 Pb2 Br2 171.48(3) 2 . ?
Br3 Pb2 Br2 83.50(3) 2 2 ?
Br3 Pb2 Br2 171.48(3) . 2 ?
Br3 Pb2 Br3 102.45(5) . 2 ?
Pb1 Br2 Pb2 83.43(3) . . ?
Pb2 Br3 Pb1 81.71(3) . . ?
Pb1 Br5 Pb1 168.39(4) . 4_455 ?
C3 O1 H1 109.5 . . ?
H1A N1 H1B 107.7 . . ?
C1 N1 H1A 108.8 . . ?
C1 N1 H1B 108.8 . . ?
C2 N1 H1A 108.8 . . ?
C2 N1 H1B 108.8 . . ?
C2 N1 C1 113.9(9) . . ?
N1 C1 H1C 109.5 . . ?
N1 C1 H1D 109.5 . . ?
N1 C1 H1E 109.5 . . ?
H1C C1 H1D 109.5 . . ?
H1C C1 H1E 109.5 . . ?
H1D C1 H1E 109.5 . . ?
N1 C2 H2A 109.3 . . ?
N1 C2 H2B 109.3 . . ?
N1 C2 C3 111.7(10) . . ?
H2A C2 H2B 107.9 . . ?
C3 C2 H2A 109.3 . . ?
C3 C2 H2B 109.3 . . ?
O1 C3 C2 112.4(11) . . ?
O1 C3 H3A 109.1 . . ?
O1 C3 H3B 109.1 . . ?
C2 C3 H3A 109.1 . . ?
C2 C3 H3B 109.1 . . ?
H3A C3 H3B 107.9 . . ?
C6 O2 H2 109.5 . . ?
H2C N2 H2D 107.3 . . ?
C4 N2 H2C 108.2 . . ?
C4 N2 H2D 108.2 . . ?
C4 N2 C5 116.4(11) . . ?
C5 N2 H2C 108.2 . . ?
C5 N2 H2D 108.2 . . ?
N2 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
N2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C5 H5A 109.8 . . ?
N2 C5 H5B 109.8 . . ?
H5A C5 H5B 108.2 . . ?
C6 C5 N2 109.6(11) . . ?
C6 C5 H5A 109.8 . . ?
C6 C5 H5B 109.8 . . ?
O2 C6 C5 112.9(12) . . ?
O2 C6 H6A 109.0 . . ?
O2 C6 H6B 109.0 . . ?
C5 C6 H6A 109.0 . . ?
C5 C6 H6B 109.0 . . ?
H6A C6 H6B 107.8 . . ?

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
N1 C2 C3 O1 -64.6(15) . . . . ?
C1 N1 C2 C3 174.6(9) . . . . ?
N2 C5 C6 O2 -54.3(16) . . . . ?
C4 N2 C5 C6 172.8(12) . . . . ?

_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 3.214
_oxdiff_exptl_absorpt_empirical_full_min 0.318
