# Supplementary Information (SI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2025

####################################################################### 
# 
# 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_33
_database_code_depnum_ccdc_archive 'CCDC 2421051'
loop_
_audit_author_name
_audit_author_address
'Dingxian Jia'
;Soochow University
China
;
_audit_update_record             
;
2025-02-03 deposited with the CCDC.	2025-05-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 H24 Cu I5 Mn N6 Pb'
_chemical_formula_weight         1140.48

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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'

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

_cell_length_a                   9.2493(5)
_cell_length_b                   23.7341(13)
_cell_length_c                   10.6004(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2327.0(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2783
_cell_measurement_theta_min      3.8970
_cell_measurement_theta_max      25.35

_exptl_crystal_description       prism
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.255
_exptl_crystal_F_000             2012
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    15.290
_shelx_estimated_absorpt_T_min   0.039
_shelx_estimated_absorpt_T_max   0.515
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0393
_exptl_absorpt_correction_T_max  0.5151
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 14.63
_diffrn_reflns_number            8552
_diffrn_reflns_av_unetI/netI     0.0627
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.792
_diffrn_reflns_theta_max         25.347
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4050
_reflns_number_gt                3330
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.890
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    0.999

_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-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0170P)²] 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     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00110(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.192(10)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4050
_refine_ls_number_parameters     183
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0366
_refine_ls_wR_factor_ref         0.0709
_refine_ls_wR_factor_gt          0.0645
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_restrained_S_all      0.956
_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_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 0.51024(5) 0.24482(3) 0.30532(9) 0.0348(2) Uani 1 1 d . . . . .
Cu1 Cu 0.2689(3) 0.38412(14) 0.4336(3) 0.0618(8) Uani 1 1 d . . . . .
I1 I 0.52389(11) 0.37781(5) 0.32441(15) 0.0424(3) Uani 1 1 d . . . . .
I2 I 0.75036(14) 0.23282(6) 0.52696(11) 0.0398(3) Uani 1 1 d . . . . .
I3 I 0.54377(12) 0.10966(6) 0.28569(15) 0.0437(3) Uani 1 1 d . . . . .
I4 I 0.75494(14) 0.25223(5) 0.09823(12) 0.0388(4) Uani 1 1 d . . . . .
I5 I 0.25282(12) 0.46026(6) 0.61076(14) 0.0414(3) Uani 1 1 d . . . . .
Mn1 Mn 0.2496(2) 0.09819(12) 0.7694(2) 0.0288(6) Uani 1 1 d . . . . .
N1 N 0.1581(16) 0.0120(6) 0.7268(14) 0.048(4) Uani 1 1 d . . . . .
H1A H 0.2051 -0.0141 0.7710 0.057 Uiso 1 1 calc R U . . .
H1B H 0.0651 0.0108 0.7482 0.057 Uiso 1 1 calc R U . . .
N2 N 0.3215(15) 0.0846(8) 0.5674(14) 0.049(4) Uani 1 1 d . . . . .
H2A H 0.2644 0.1036 0.5148 0.059 Uiso 1 1 calc R U . . .
H2B H 0.4119 0.0966 0.5571 0.059 Uiso 1 1 calc R U . . .
N3 N 0.0490(13) 0.1478(6) 0.7131(13) 0.029(3) Uani 1 1 d . . . . .
H3A H 0.0741 0.1769 0.6649 0.035 Uiso 1 1 calc R U . . .
H3B H -0.0106 0.1259 0.6691 0.035 Uiso 1 1 calc R U . . .
N4 N 0.1240(14) 0.1048(7) 0.9538(12) 0.043(4) Uani 1 1 d . . . . .
H4A H 0.1233 0.0716 0.9928 0.052 Uiso 1 1 calc R U . . .
H4B H 0.1659 0.1299 1.0044 0.052 Uiso 1 1 calc R U . . .
N5 N 0.3893(12) 0.1771(6) 0.7943(16) 0.042(3) Uani 1 1 d . . . . .
H5A H 0.3890 0.1974 0.7238 0.051 Uiso 1 1 calc R U . . .
H5B H 0.3548 0.1982 0.8568 0.051 Uiso 1 1 calc R U . . .
N6 N 0.4491(14) 0.0635(7) 0.8645(15) 0.050(5) Uani 1 1 d . . . . .
H6A H 0.4235 0.0407 0.9273 0.060 Uiso 1 1 calc R U . . .
H6B H 0.5007 0.0437 0.8093 0.060 Uiso 1 1 calc R U . . .
C1 C 0.1742(19) 0.0010(10) 0.592(2) 0.063(6) Uani 1 1 d . . . . .
H1C H 0.0941 0.0181 0.5471 0.075 Uiso 1 1 calc R U . . .
H1D H 0.1707 -0.0393 0.5775 0.075 Uiso 1 1 calc R U . . .
C2 C 0.312(2) 0.0238(10) 0.542(2) 0.060(6) Uani 1 1 d . . . . .
H2C H 0.3929 0.0046 0.5817 0.072 Uiso 1 1 calc R U . . .
H2D H 0.3175 0.0171 0.4519 0.072 Uiso 1 1 calc R U . . .
C3 C -0.0245(18) 0.1683(8) 0.828(2) 0.046(6) Uani 1 1 d . . . . .
H3C H -0.1232 0.1788 0.8080 0.055 Uiso 1 1 calc R U . . .
H3D H 0.0251 0.2012 0.8603 0.055 Uiso 1 1 calc R U . . .
C4 C -0.0239(18) 0.1223(9) 0.9253(19) 0.047(5) Uani 1 1 d . . . . .
H4C H -0.0701 0.1358 1.0017 0.056 Uiso 1 1 calc R U . . .
H4D H -0.0785 0.0903 0.8944 0.056 Uiso 1 1 calc R U . . .
C5 C 0.5374(17) 0.1583(9) 0.8239(19) 0.047(5) Uani 1 1 d . . . . .
H5C H 0.5914 0.1895 0.8593 0.056 Uiso 1 1 calc R U . . .
H5D H 0.5852 0.1467 0.7467 0.056 Uiso 1 1 calc R U . . .
C6 C 0.538(2) 0.1107(10) 0.915(2) 0.061(7) Uani 1 1 d . . . . .
H6C H 0.4986 0.1231 0.9949 0.073 Uiso 1 1 calc R U . . .
H6D H 0.6360 0.0980 0.9284 0.073 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 I4 3.1579(15) . ?
Pb1 I1 3.1654(15) . ?
Pb1 I4 3.2249(15) 3_455 ?
Pb1 I3 3.2296(16) . ?
Pb1 I2 3.2456(14) . ?
Pb1 I2 3.4029(15) 3_455 ?
Cu1 I5 2.610(3) . ?
Cu1 I3 2.611(3) 3_455 ?
Cu1 I1 2.632(3) . ?
Cu1 I2 2.952(4) 3_455 ?
I2 Cu1 2.952(4) 3 ?
I2 Pb1 3.4029(15) 3 ?
I3 Cu1 2.611(3) 3 ?
I4 Pb1 3.2249(15) 3 ?
Mn1 N6 2.258(14) . ?
Mn1 N1 2.259(15) . ?
Mn1 N2 2.265(14) . ?
Mn1 N3 2.277(13) . ?
Mn1 N4 2.279(13) . ?
Mn1 N5 2.290(13) . ?
N1 C1 1.46(2) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N2 C2 1.47(2) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N3 C3 1.48(2) . ?
N3 H3A 0.8900 . ?
N3 H3B 0.8900 . ?
N4 C4 1.46(2) . ?
N4 H4A 0.8900 . ?
N4 H4B 0.8900 . ?
N5 C5 1.47(2) . ?
N5 H5A 0.8900 . ?
N5 H5B 0.8900 . ?
N6 C6 1.49(3) . ?
N6 H6A 0.8900 . ?
N6 H6B 0.8900 . ?
C1 C2 1.48(2) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
C3 C4 1.50(2) . ?
C3 H3C 0.9700 . ?
C3 H3D 0.9700 . ?
C4 H4C 0.9700 . ?
C4 H4D 0.9700 . ?
C5 C6 1.48(3) . ?
C5 H5C 0.9700 . ?
C5 H5D 0.9700 . ?
C6 H6C 0.9700 . ?
C6 H6D 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
I4 Pb1 I1 87.73(4) . . ?
I4 Pb1 I4 92.89(4) . 3_455 ?
I1 Pb1 I4 92.93(4) . 3_455 ?
I4 Pb1 I3 86.66(4) . . ?
I1 Pb1 I3 172.20(3) . . ?
I4 Pb1 I3 92.75(4) 3_455 . ?
I4 Pb1 I2 91.01(3) . . ?
I1 Pb1 I2 90.80(4) . . ?
I4 Pb1 I2 174.70(4) 3_455 . ?
I3 Pb1 I2 83.90(4) . . ?
I4 Pb1 I2 167.83(4) . 3_455 ?
I1 Pb1 I2 80.13(4) . 3_455 ?
I4 Pb1 I2 87.10(3) 3_455 3_455 ?
I3 Pb1 I2 105.50(4) . 3_455 ?
I2 Pb1 I2 89.84(4) . 3_455 ?
I5 Cu1 I3 110.34(11) . 3_455 ?
I5 Cu1 I1 114.01(11) . . ?
I3 Cu1 I1 116.99(12) 3_455 . ?
I5 Cu1 I2 113.98(11) . 3_455 ?
I3 Cu1 I2 102.01(10) 3_455 3_455 ?
I1 Cu1 I2 98.40(10) . 3_455 ?
Cu1 I1 Pb1 92.82(8) . . ?
Cu1 I2 Pb1 83.08(6) 3 . ?
Cu1 I2 Pb1 82.77(6) 3 3 ?
Pb1 I2 Pb1 88.27(4) . 3 ?
Cu1 I3 Pb1 88.96(8) 3 . ?
Pb1 I4 Pb1 93.02(4) . 3 ?
N6 Mn1 N1 93.8(6) . . ?
N6 Mn1 N2 97.5(6) . . ?
N1 Mn1 N2 78.0(6) . . ?
N6 Mn1 N3 166.2(6) . . ?
N1 Mn1 N3 96.4(5) . . ?
N2 Mn1 N3 93.7(5) . . ?
N6 Mn1 N4 93.4(5) . . ?
N1 Mn1 N4 92.5(5) . . ?
N2 Mn1 N4 166.0(5) . . ?
N3 Mn1 N4 76.9(5) . . ?
N6 Mn1 N5 77.6(5) . . ?
N1 Mn1 N5 167.1(5) . . ?
N2 Mn1 N5 93.4(6) . . ?
N3 Mn1 N5 93.8(5) . . ?
N4 Mn1 N5 97.6(6) . . ?
C1 N1 Mn1 108.6(12) . . ?
C1 N1 H1A 110.0 . . ?
Mn1 N1 H1A 110.0 . . ?
C1 N1 H1B 110.0 . . ?
Mn1 N1 H1B 110.0 . . ?
H1A N1 H1B 108.3 . . ?
C2 N2 Mn1 107.2(12) . . ?
C2 N2 H2A 110.3 . . ?
Mn1 N2 H2A 110.3 . . ?
C2 N2 H2B 110.3 . . ?
Mn1 N2 H2B 110.3 . . ?
H2A N2 H2B 108.5 . . ?
C3 N3 Mn1 109.2(10) . . ?
C3 N3 H3A 109.8 . . ?
Mn1 N3 H3A 109.8 . . ?
C3 N3 H3B 109.8 . . ?
Mn1 N3 H3B 109.8 . . ?
H3A N3 H3B 108.3 . . ?
C4 N4 Mn1 108.6(10) . . ?
C4 N4 H4A 110.0 . . ?
Mn1 N4 H4A 110.0 . . ?
C4 N4 H4B 110.0 . . ?
Mn1 N4 H4B 110.0 . . ?
H4A N4 H4B 108.3 . . ?
C5 N5 Mn1 107.6(10) . . ?
C5 N5 H5A 110.2 . . ?
Mn1 N5 H5A 110.2 . . ?
C5 N5 H5B 110.2 . . ?
Mn1 N5 H5B 110.2 . . ?
H5A N5 H5B 108.5 . . ?
C6 N6 Mn1 109.6(12) . . ?
C6 N6 H6A 109.7 . . ?
Mn1 N6 H6A 109.7 . . ?
C6 N6 H6B 109.7 . . ?
Mn1 N6 H6B 109.7 . . ?
H6A N6 H6B 108.2 . . ?
N1 C1 C2 111.9(16) . . ?
N1 C1 H1C 109.2 . . ?
C2 C1 H1C 109.2 . . ?
N1 C1 H1D 109.2 . . ?
C2 C1 H1D 109.2 . . ?
H1C C1 H1D 107.9 . . ?
N2 C2 C1 109.9(17) . . ?
N2 C2 H2C 109.7 . . ?
C1 C2 H2C 109.7 . . ?
N2 C2 H2D 109.7 . . ?
C1 C2 H2D 109.7 . . ?
H2C C2 H2D 108.2 . . ?
N3 C3 C4 109.1(14) . . ?
N3 C3 H3C 109.9 . . ?
C4 C3 H3C 109.9 . . ?
N3 C3 H3D 109.9 . . ?
C4 C3 H3D 109.9 . . ?
H3C C3 H3D 108.3 . . ?
N4 C4 C3 110.6(14) . . ?
N4 C4 H4C 109.5 . . ?
C3 C4 H4C 109.5 . . ?
N4 C4 H4D 109.5 . . ?
C3 C4 H4D 109.5 . . ?
H4C C4 H4D 108.1 . . ?
N5 C5 C6 111.7(15) . . ?
N5 C5 H5C 109.3 . . ?
C6 C5 H5C 109.3 . . ?
N5 C5 H5D 109.3 . . ?
C6 C5 H5D 109.3 . . ?
H5C C5 H5D 107.9 . . ?
C5 C6 N6 109.9(15) . . ?
C5 C6 H6C 109.7 . . ?
N6 C6 H6C 109.7 . . ?
C5 C6 H6D 109.7 . . ?
N6 C6 H6D 109.7 . . ?
H6C C6 H6D 108.2 . . ?

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
Mn1 N1 C1 C2 37(2) . . . . ?
Mn1 N2 C2 C1 44.6(19) . . . . ?
N1 C1 C2 N2 -57(2) . . . . ?
Mn1 N3 C3 C4 -41.7(18) . . . . ?
Mn1 N4 C4 C3 -42.8(19) . . . . ?
N3 C3 C4 N4 58(2) . . . . ?
Mn1 N5 C5 C6 -42.0(19) . . . . ?
N5 C5 C6 N6 56(2) . . . . ?
Mn1 N6 C6 C5 -40(2) . . . . ?

_refine_diff_density_max         1.583
_refine_diff_density_min         -1.155
_refine_diff_density_rms         0.199



####################################################################### 
# 
# 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_33o
_database_code_depnum_ccdc_archive 'CCDC 2421053'
loop_
_audit_author_name
_audit_author_address
'Dingxian Jia'
;Soochow University
China
;
_audit_update_record             
;
2025-02-03 deposited with the CCDC.	2025-05-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 H24 Cu Fe I5 N6 Pb'
_chemical_formula_weight         1141.39

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'

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

_cell_length_a                   9.2145(18)
_cell_length_b                   23.643(5)
_cell_length_c                   10.589(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2307.0(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    8694
_cell_measurement_theta_min      3.0770
_cell_measurement_theta_max      25.35

_exptl_crystal_description       Block
_exptl_crystal_colour            Orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.286
_exptl_crystal_F_000             2016
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    15.505
_shelx_estimated_absorpt_T_min   0.074
_shelx_estimated_absorpt_T_max   0.147
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0740
_exptl_absorpt_correction_T_max  0.1468
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      223(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 14.63
_diffrn_reflns_number            20911
_diffrn_reflns_av_unetI/netI     0.0576
_diffrn_reflns_av_R_equivalents  0.0643
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.055
_diffrn_reflns_theta_max         25.194
_diffrn_reflns_theta_full        25.194
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             3978
_reflns_number_gt                3530
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.890
_reflns_Friedel_fraction_max     0.994
_reflns_Friedel_fraction_full    0.994

_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-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0137P)²] 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     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00156(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.990(10)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3978
_refine_ls_number_parameters     183
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0385
_refine_ls_wR_factor_ref         0.0693
_refine_ls_wR_factor_gt          0.0668
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_restrained_S_all      1.116
_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 1.01434(6) 0.25433(3) 0.23674(9) 0.03104(19) Uani 1 1 d . . . . .
Cu1 Cu 0.7746(3) 0.11625(12) 0.3658(3) 0.0547(7) Uani 1 1 d . . . . .
I1 I 0.76035(14) 0.25036(5) 0.02687(13) 0.0350(3) Uani 1 1 d . . . . .
I2 I 1.04465(13) 0.39109(5) 0.21927(13) 0.0368(3) Uani 1 1 d . . . . .
I3 I 1.25638(14) 0.26773(5) 0.46012(11) 0.0348(3) Uani 1 1 d . . . . .
I4 I 1.03326(12) 0.11945(5) 0.25729(13) 0.0368(3) Uani 1 1 d . . . . .
I5 I 0.75411(12) 0.03973(5) 0.54640(13) 0.0352(3) Uani 1 1 d . . . . .
Fe1 Fe 0.7473(2) 0.90310(8) 0.20212(19) 0.0147(5) Uani 1 1 d D . . . .
N1 N 0.5551(14) 0.9396(6) 0.2870(13) 0.040(4) Uani 1 1 d D . . . .
H1A H 0.5800 0.9639 0.3476 0.049 Uiso 1 1 calc R U . . .
H1B H 0.5037 0.9581 0.2291 0.049 Uiso 1 1 calc R U . . .
N2 N 0.6242(13) 0.8275(5) 0.2280(15) 0.032(3) Uani 1 1 d . . . . .
H2A H 0.6292 0.8060 0.1590 0.038 Uiso 1 1 calc R U . . .
H2B H 0.6592 0.8078 0.2928 0.038 Uiso 1 1 calc R U . . .
N3 N 0.8565(14) 0.8965(5) 0.3797(12) 0.031(3) Uani 1 1 d . . . . .
H3A H 0.8540 0.9296 0.4197 0.037 Uiso 1 1 calc R U . . .
H3B H 0.8127 0.8709 0.4280 0.037 Uiso 1 1 calc R U . . .
N4 N 0.9367(15) 0.8583(6) 0.1402(13) 0.032(4) Uani 1 1 d . . . . .
H4A H 0.9114 0.8302 0.0888 0.039 Uiso 1 1 calc R U . . .
H4B H 0.9955 0.8815 0.0983 0.039 Uiso 1 1 calc R U . . .
N5 N 0.6734(15) 0.9149(5) 0.0155(13) 0.037(4) Uani 1 1 d . . . . .
H5A H 0.7255 0.8937 -0.0371 0.045 Uiso 1 1 calc R U . . .
H5B H 0.5810 0.9042 0.0096 0.045 Uiso 1 1 calc R U . . .
N6 N 0.8429(15) 0.9847(5) 0.1660(13) 0.040(4) Uani 1 1 d D . . . .
H6A H 0.8011 1.0108 0.2141 0.048 Uiso 1 1 calc R U . . .
H6B H 0.9373 0.9839 0.1839 0.048 Uiso 1 1 calc R U . . .
C1 C 0.467(2) 0.8920(7) 0.3416(19) 0.045(5) Uani 1 1 d . . . . .
H1C H 0.5052 0.8810 0.4233 0.055 Uiso 1 1 calc R U . . .
H1D H 0.3667 0.9038 0.3526 0.055 Uiso 1 1 calc R U . . .
C2 C 0.4746(18) 0.8436(7) 0.2523(19) 0.042(5) Uani 1 1 d . . . . .
H2C H 0.4226 0.8115 0.2875 0.050 Uiso 1 1 calc R U . . .
H2D H 0.4281 0.8539 0.1734 0.050 Uiso 1 1 calc R U . . .
C3 C 1.0088(19) 0.8796(8) 0.3561(17) 0.037(5) Uani 1 1 d . . . . .
H3C H 1.0513 0.8646 0.4329 0.044 Uiso 1 1 calc R U . . .
H3D H 1.0651 0.9122 0.3301 0.044 Uiso 1 1 calc R U . . .
C4 C 1.0119(18) 0.8354(7) 0.2542(19) 0.041(5) Uani 1 1 d . . . . .
H4C H 1.1115 0.8258 0.2336 0.050 Uiso 1 1 calc R U . . .
H4D H 0.9634 0.8013 0.2831 0.050 Uiso 1 1 calc R U . . .
C5 C 0.688(2) 0.9764(7) -0.0208(16) 0.038(4) Uani 1 1 d . . . . .
H5C H 0.6878 0.9801 -0.1120 0.045 Uiso 1 1 calc R U . . .
H5D H 0.6059 0.9977 0.0122 0.045 Uiso 1 1 calc R U . . .
C6 C 0.821(2) 0.9984(7) 0.0305(17) 0.038(4) Uani 1 1 d . . . . .
H6C H 0.8220 1.0392 0.0204 0.045 Uiso 1 1 calc R U . . .
H6D H 0.9018 0.9832 -0.0177 0.045 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 I1 3.1764(15) 3 ?
Pb1 I4 3.2010(15) . ?
Pb1 I1 3.2288(15) . ?
Pb1 I2 3.2508(15) . ?
Pb1 I3 3.2665(15) . ?
Pb1 I3 3.3938(16) 3_455 ?
Cu1 I2 2.632(3) 3_455 ?
Cu1 I5 2.639(3) . ?
Cu1 I4 2.647(3) . ?
Cu1 I3 2.924(3) 3_455 ?
I1 Pb1 3.1764(15) 3_455 ?
I2 Cu1 2.632(3) 3 ?
I3 Cu1 2.924(3) 3 ?
I3 Pb1 3.3938(16) 3 ?
Fe1 N5 2.109(13) . ?
Fe1 N2 2.135(11) . ?
Fe1 N3 2.139(12) . ?
Fe1 N4 2.144(13) . ?
Fe1 N6 2.154(12) . ?
Fe1 N1 2.166(12) . ?
N1 C1 1.51(2) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N2 C2 1.453(19) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N3 C3 1.48(2) . ?
N3 H3A 0.8900 . ?
N3 H3B 0.8900 . ?
N4 C4 1.49(2) . ?
N4 H4A 0.8900 . ?
N4 H4B 0.8900 . ?
N5 C5 1.51(2) . ?
N5 H5A 0.8900 . ?
N5 H5B 0.8900 . ?
N6 C6 1.48(2) . ?
N6 H6A 0.8900 . ?
N6 H6B 0.8900 . ?
C1 C2 1.49(2) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
C3 C4 1.50(2) . ?
C3 H3C 0.9700 . ?
C3 H3D 0.9700 . ?
C4 H4C 0.9700 . ?
C4 H4D 0.9700 . ?
C5 C6 1.44(2) . ?
C5 H5C 0.9700 . ?
C5 H5D 0.9700 . ?
C6 H6C 0.9700 . ?
C6 H6D 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
I1 Pb1 I4 88.51(3) 3 . ?
I1 Pb1 I1 91.99(4) 3 . ?
I4 Pb1 I1 93.29(4) . . ?
I1 Pb1 I2 86.19(4) 3 . ?
I4 Pb1 I2 171.93(3) . . ?
I1 Pb1 I2 92.98(3) . . ?
I1 Pb1 I3 91.31(3) 3 . ?
I4 Pb1 I3 90.58(4) . . ?
I1 Pb1 I3 174.98(4) . . ?
I2 Pb1 I3 83.46(4) . . ?
I1 Pb1 I3 169.16(4) 3 3_455 ?
I4 Pb1 I3 80.66(4) . 3_455 ?
I1 Pb1 I3 88.14(3) . 3_455 ?
I2 Pb1 I3 104.63(4) . 3_455 ?
I3 Pb1 I3 89.33(4) . 3_455 ?
I2 Cu1 I5 108.93(10) 3_455 . ?
I2 Cu1 I4 118.09(12) 3_455 . ?
I5 Cu1 I4 113.49(10) . . ?
I2 Cu1 I3 102.54(9) 3_455 3_455 ?
I5 Cu1 I3 113.04(10) . 3_455 ?
I4 Cu1 I3 99.97(9) . 3_455 ?
Pb1 I1 Pb1 92.10(4) 3_455 . ?
Cu1 I2 Pb1 88.28(7) 3 . ?
Cu1 I3 Pb1 83.27(6) 3 . ?
Cu1 I3 Pb1 82.29(6) 3 3 ?
Pb1 I3 Pb1 87.62(4) . 3 ?
Cu1 I4 Pb1 90.51(7) . . ?
N5 Fe1 N2 93.4(6) . . ?
N5 Fe1 N3 170.3(6) . . ?
N2 Fe1 N3 94.4(5) . . ?
N5 Fe1 N4 92.4(5) . . ?
N2 Fe1 N4 93.3(5) . . ?
N3 Fe1 N4 81.4(5) . . ?
N5 Fe1 N6 81.2(5) . . ?
N2 Fe1 N6 171.8(5) . . ?
N3 Fe1 N6 91.7(5) . . ?
N4 Fe1 N6 93.1(5) . . ?
N5 Fe1 N1 94.1(5) . . ?
N2 Fe1 N1 81.2(5) . . ?
N3 Fe1 N1 92.8(5) . . ?
N4 Fe1 N1 171.7(5) . . ?
N6 Fe1 N1 93.0(5) . . ?
C1 N1 Fe1 107.6(10) . . ?
C1 N1 H1A 110.2 . . ?
Fe1 N1 H1A 110.2 . . ?
C1 N1 H1B 110.2 . . ?
Fe1 N1 H1B 110.2 . . ?
H1A N1 H1B 108.5 . . ?
C2 N2 Fe1 107.9(9) . . ?
C2 N2 H2A 110.1 . . ?
Fe1 N2 H2A 110.1 . . ?
C2 N2 H2B 110.1 . . ?
Fe1 N2 H2B 110.1 . . ?
H2A N2 H2B 108.4 . . ?
C3 N3 Fe1 108.5(10) . . ?
C3 N3 H3A 110.0 . . ?
Fe1 N3 H3A 110.0 . . ?
C3 N3 H3B 110.0 . . ?
Fe1 N3 H3B 110.0 . . ?
H3A N3 H3B 108.4 . . ?
C4 N4 Fe1 108.1(10) . . ?
C4 N4 H4A 110.1 . . ?
Fe1 N4 H4A 110.1 . . ?
C4 N4 H4B 110.1 . . ?
Fe1 N4 H4B 110.1 . . ?
H4A N4 H4B 108.4 . . ?
C5 N5 Fe1 109.7(10) . . ?
C5 N5 H5A 109.7 . . ?
Fe1 N5 H5A 109.7 . . ?
C5 N5 H5B 109.7 . . ?
Fe1 N5 H5B 109.7 . . ?
H5A N5 H5B 108.2 . . ?
C6 N6 Fe1 108.2(10) . . ?
C6 N6 H6A 110.1 . . ?
Fe1 N6 H6A 110.1 . . ?
C6 N6 H6B 110.1 . . ?
Fe1 N6 H6B 110.1 . . ?
H6A N6 H6B 108.4 . . ?
C2 C1 N1 107.8(14) . . ?
C2 C1 H1C 110.1 . . ?
N1 C1 H1C 110.1 . . ?
C2 C1 H1D 110.1 . . ?
N1 C1 H1D 110.1 . . ?
H1C C1 H1D 108.5 . . ?
N2 C2 C1 111.1(14) . . ?
N2 C2 H2C 109.4 . . ?
C1 C2 H2C 109.4 . . ?
N2 C2 H2D 109.4 . . ?
C1 C2 H2D 109.4 . . ?
H2C C2 H2D 108.0 . . ?
N3 C3 C4 109.1(14) . . ?
N3 C3 H3C 109.9 . . ?
C4 C3 H3C 109.9 . . ?
N3 C3 H3D 109.9 . . ?
C4 C3 H3D 109.9 . . ?
H3C C3 H3D 108.3 . . ?
N4 C4 C3 108.6(13) . . ?
N4 C4 H4C 110.0 . . ?
C3 C4 H4C 110.0 . . ?
N4 C4 H4D 110.0 . . ?
C3 C4 H4D 110.0 . . ?
H4C C4 H4D 108.4 . . ?
C6 C5 N5 109.0(14) . . ?
C6 C5 H5C 109.9 . . ?
N5 C5 H5C 109.9 . . ?
C6 C5 H5D 109.9 . . ?
N5 C5 H5D 109.9 . . ?
H5C C5 H5D 108.3 . . ?
C5 C6 N6 113.6(14) . . ?
C5 C6 H6C 108.8 . . ?
N6 C6 H6C 108.8 . . ?
C5 C6 H6D 108.8 . . ?
N6 C6 H6D 108.8 . . ?
H6C C6 H6D 107.7 . . ?

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
Fe1 N1 C1 C2 -39.2(18) . . . . ?
Fe1 N2 C2 C1 -43.1(18) . . . . ?
N1 C1 C2 N2 56(2) . . . . ?
Fe1 N3 C3 C4 -41.1(15) . . . . ?
Fe1 N4 C4 C3 -41.2(15) . . . . ?
N3 C3 C4 N4 55.6(18) . . . . ?
Fe1 N5 C5 C6 39.1(16) . . . . ?
N5 C5 C6 N6 -48.4(19) . . . . ?
Fe1 N6 C6 C5 33.1(17) . . . . ?

_refine_diff_density_max         1.077
_refine_diff_density_min         -1.035
_refine_diff_density_rms         0.195



####################################################################### 
# 
# 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_33_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2421052'
loop_
_audit_author_name
_audit_author_address
'Dingxian Jia'
;Soochow University
China
;
_audit_update_record             
;
2025-02-03 deposited with the CCDC.	2025-05-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 H24 Cu I5 N6 Ni Pb'
_chemical_formula_weight         1144.25

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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'

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

_cell_length_a                   9.1008(18)
_cell_length_b                   23.247(5)
_cell_length_c                   10.511(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2223.7(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4623
_cell_measurement_theta_min      3.0515
_cell_measurement_theta_max      25.35

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.418
_exptl_crystal_F_000             2024
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    16.279
_shelx_estimated_absorpt_T_min   0.059
_shelx_estimated_absorpt_T_max   0.139
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0591
_exptl_absorpt_correction_T_max  0.1392
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 14.63
_diffrn_reflns_number            8562
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.843
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3329
_reflns_number_gt                3127
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.891
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    0.999

_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-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0284P)²+3.7344P] 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     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00063(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.555(7)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3329
_refine_ls_number_parameters     183
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0256
_refine_ls_wR_factor_ref         0.0594
_refine_ls_wR_factor_gt          0.0581
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.040
_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 0.48639(4) 0.74559(2) 0.74518(6) 0.02088(13) Uani 1 1 d . . . . .
Cu1 Cu 0.22565(17) 0.61644(9) 0.87428(19) 0.0360(4) Uani 1 1 d . . . . .
I1 I 0.24395(9) 0.73171(4) 0.96804(8) 0.0219(2) Uani 1 1 d . . . . .
I2 I 0.45513(9) 0.60831(4) 0.72695(10) 0.0260(2) Uani 1 1 d . . . . .
I3 I 0.74027(9) 0.74973(4) 0.53472(10) 0.0236(2) Uani 1 1 d . . . . .
I4 I 0.46548(8) 0.88082(4) 0.76521(10) 0.0260(2) Uani 1 1 d . . . . .
I5 I 0.24604(7) 0.53969(4) 1.05507(9) 0.0224(2) Uani 1 1 d . . . . .
Ni1 Ni 0.25257(13) 0.40314(7) 0.71023(15) 0.0144(3) Uani 1 1 d . . . . .
N1 N 0.0636(10) 0.3578(5) 0.6474(10) 0.024(2) Uani 1 1 d . . . . .
H1A H 0.0043 0.3813 0.6047 0.028 Uiso 1 1 calc R U . . .
H1B H 0.0899 0.3292 0.5958 0.028 Uiso 1 1 calc R U . . .
N2 N 0.1431(11) 0.3963(4) 0.8879(10) 0.024(2) Uani 1 1 d . . . . .
H2A H 0.1863 0.3697 0.9360 0.029 Uiso 1 1 calc R U . . .
H2B H 0.1463 0.4297 0.9289 0.029 Uiso 1 1 calc R U . . .
N3 N 0.1588(11) 0.4845(5) 0.6735(10) 0.024(2) Uani 1 1 d . . . . .
H3A H 0.0640 0.4842 0.6942 0.029 Uiso 1 1 calc R U . . .
H3B H 0.2036 0.5112 0.7201 0.029 Uiso 1 1 calc R U . . .
N4 N 0.3315(10) 0.4142(4) 0.5224(9) 0.022(2) Uani 1 1 d . . . . .
H4A H 0.4249 0.4031 0.5177 0.027 Uiso 1 1 calc R U . . .
H4B H 0.2791 0.3928 0.4688 0.027 Uiso 1 1 calc R U . . .
N5 N 0.4423(10) 0.4400(5) 0.7930(10) 0.025(2) Uani 1 1 d . . . . .
H5A H 0.4943 0.4584 0.7340 0.030 Uiso 1 1 calc R U . . .
H5B H 0.4166 0.4652 0.8527 0.030 Uiso 1 1 calc R U . . .
N6 N 0.3769(9) 0.3262(4) 0.7356(11) 0.022(2) Uani 1 1 d . . . . .
H6A H 0.3405 0.3058 0.8000 0.027 Uiso 1 1 calc R U . . .
H6B H 0.3729 0.3048 0.6655 0.027 Uiso 1 1 calc R U . . .
C1 C -0.0123(13) 0.3348(6) 0.7580(15) 0.030(3) Uani 1 1 d . . . . .
H1C H 0.0366 0.3002 0.7874 0.036 Uiso 1 1 calc R U . . .
H1D H -0.1127 0.3250 0.7359 0.036 Uiso 1 1 calc R U . . .
C2 C -0.0111(13) 0.3799(7) 0.8621(13) 0.027(3) Uani 1 1 d . . . . .
H2C H -0.0667 0.4134 0.8353 0.032 Uiso 1 1 calc R U . . .
H2D H -0.0560 0.3646 0.9386 0.032 Uiso 1 1 calc R U . . .
C3 C 0.1757(14) 0.4981(6) 0.5356(14) 0.029(3) Uani 1 1 d . . . . .
H3C H 0.0963 0.4804 0.4881 0.035 Uiso 1 1 calc R U . . .
H3D H 0.1698 0.5394 0.5233 0.035 Uiso 1 1 calc R U . . .
C4 C 0.3190(14) 0.4767(6) 0.4865(13) 0.029(3) Uani 1 1 d . . . . .
H4C H 0.3992 0.4984 0.5237 0.035 Uiso 1 1 calc R U . . .
H4D H 0.3233 0.4809 0.3948 0.035 Uiso 1 1 calc R U . . .
C5 C 0.5315(14) 0.3935(6) 0.8498(14) 0.029(3) Uani 1 1 d . . . . .
H5C H 0.4910 0.3827 0.9317 0.034 Uiso 1 1 calc R U . . .
H5D H 0.6314 0.4067 0.8628 0.034 Uiso 1 1 calc R U . . .
C6 C 0.5313(13) 0.3427(6) 0.7628(16) 0.031(3) Uani 1 1 d . . . . .
H6C H 0.5816 0.3522 0.6842 0.038 Uiso 1 1 calc R U . . .
H6D H 0.5826 0.3108 0.8026 0.038 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 I3 3.1500(11) 3_465 ?
Pb1 I4 3.1564(12) . ?
Pb1 I3 3.2003(11) . ?
Pb1 I2 3.2096(12) . ?
Pb1 I1 3.2340(11) . ?
Pb1 I1 3.3557(11) 3_565 ?
Cu1 I2 2.607(2) . ?
Cu1 I5 2.613(2) . ?
Cu1 I4 2.6314(19) 3_465 ?
Cu1 I1 2.860(2) . ?
I1 Pb1 3.3556(11) 3_465 ?
I3 Pb1 3.1500(11) 3_565 ?
I4 Cu1 2.6314(19) 3_565 ?
Ni1 N3 2.110(10) . ?
Ni1 N5 2.115(9) . ?
Ni1 N4 2.117(10) . ?
Ni1 N2 2.123(10) . ?
Ni1 N1 2.123(9) . ?
Ni1 N6 2.134(9) . ?
N1 C1 1.454(17) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N2 C2 1.479(15) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N3 C3 1.491(17) . ?
N3 H3A 0.8900 . ?
N3 H3B 0.8900 . ?
N4 C4 1.504(16) . ?
N4 H4A 0.8900 . ?
N4 H4B 0.8900 . ?
N5 C5 1.478(16) . ?
N5 H5A 0.8900 . ?
N5 H5B 0.8900 . ?
N6 C6 1.484(15) . ?
N6 H6A 0.8900 . ?
N6 H6B 0.8900 . ?
C1 C2 1.516(19) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
C3 C4 1.488(18) . ?
C3 H3C 0.9700 . ?
C3 H3D 0.9700 . ?
C4 H4C 0.9700 . ?
C4 H4D 0.9700 . ?
C5 C6 1.49(2) . ?
C5 H5C 0.9700 . ?
C5 H5D 0.9700 . ?
C6 H6C 0.9700 . ?
C6 H6D 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
I3 Pb1 I4 88.26(3) 3_465 . ?
I3 Pb1 I3 91.54(3) 3_465 . ?
I4 Pb1 I3 93.42(3) . . ?
I3 Pb1 I2 85.95(3) 3_465 . ?
I4 Pb1 I2 171.45(2) . . ?
I3 Pb1 I2 93.01(3) . . ?
I3 Pb1 I1 91.55(3) 3_465 . ?
I4 Pb1 I1 90.57(3) . . ?
I3 Pb1 I1 175.02(3) . . ?
I2 Pb1 I1 83.31(3) . . ?
I3 Pb1 I1 168.97(3) 3_465 3_565 ?
I4 Pb1 I1 80.73(3) . 3_565 ?
I3 Pb1 I1 88.48(3) . 3_565 ?
I2 Pb1 I1 105.07(3) . 3_565 ?
I1 Pb1 I1 89.24(3) . 3_565 ?
I2 Cu1 I5 109.00(7) . . ?
I2 Cu1 I4 117.64(8) . 3_465 ?
I5 Cu1 I4 113.41(7) . 3_465 ?
I2 Cu1 I1 103.06(7) . . ?
I5 Cu1 I1 112.64(8) . . ?
I4 Cu1 I1 100.36(7) 3_465 . ?
Cu1 I1 Pb1 83.32(4) . . ?
Cu1 I1 Pb1 82.31(4) . 3_465 ?
Pb1 I1 Pb1 87.44(3) . 3_465 ?
Cu1 I2 Pb1 87.91(5) . . ?
Pb1 I3 Pb1 91.66(3) 3_565 . ?
Cu1 I4 Pb1 89.94(5) 3_565 . ?
N3 Ni1 N5 92.5(4) . . ?
N3 Ni1 N4 81.8(4) . . ?
N5 Ni1 N4 93.3(4) . . ?
N3 Ni1 N2 92.2(4) . . ?
N5 Ni1 N2 93.0(4) . . ?
N4 Ni1 N2 171.5(4) . . ?
N3 Ni1 N1 93.5(4) . . ?
N5 Ni1 N1 172.2(4) . . ?
N4 Ni1 N1 92.6(4) . . ?
N2 Ni1 N1 81.7(4) . . ?
N3 Ni1 N6 171.4(4) . . ?
N5 Ni1 N6 81.6(4) . . ?
N4 Ni1 N6 92.2(4) . . ?
N2 Ni1 N6 94.4(4) . . ?
N1 Ni1 N6 93.0(4) . . ?
C1 N1 Ni1 108.6(8) . . ?
C1 N1 H1A 110.0 . . ?
Ni1 N1 H1A 110.0 . . ?
C1 N1 H1B 110.0 . . ?
Ni1 N1 H1B 110.0 . . ?
H1A N1 H1B 108.4 . . ?
C2 N2 Ni1 107.7(8) . . ?
C2 N2 H2A 110.2 . . ?
Ni1 N2 H2A 110.2 . . ?
C2 N2 H2B 110.2 . . ?
Ni1 N2 H2B 110.2 . . ?
H2A N2 H2B 108.5 . . ?
C3 N3 Ni1 109.0(8) . . ?
C3 N3 H3A 109.9 . . ?
Ni1 N3 H3A 109.9 . . ?
C3 N3 H3B 109.9 . . ?
Ni1 N3 H3B 109.9 . . ?
H3A N3 H3B 108.3 . . ?
C4 N4 Ni1 109.0(8) . . ?
C4 N4 H4A 109.9 . . ?
Ni1 N4 H4A 109.9 . . ?
C4 N4 H4B 109.9 . . ?
Ni1 N4 H4B 109.9 . . ?
H4A N4 H4B 108.3 . . ?
C5 N5 Ni1 108.6(8) . . ?
C5 N5 H5A 110.0 . . ?
Ni1 N5 H5A 110.0 . . ?
C5 N5 H5B 110.0 . . ?
Ni1 N5 H5B 110.0 . . ?
H5A N5 H5B 108.4 . . ?
C6 N6 Ni1 108.0(7) . . ?
C6 N6 H6A 110.1 . . ?
Ni1 N6 H6A 110.1 . . ?
C6 N6 H6B 110.1 . . ?
Ni1 N6 H6B 110.1 . . ?
H6A N6 H6B 108.4 . . ?
N1 C1 C2 108.6(11) . . ?
N1 C1 H1C 110.0 . . ?
C2 C1 H1C 110.0 . . ?
N1 C1 H1D 110.0 . . ?
C2 C1 H1D 110.0 . . ?
H1C C1 H1D 108.3 . . ?
N2 C2 C1 108.5(10) . . ?
N2 C2 H2C 110.0 . . ?
C1 C2 H2C 110.0 . . ?
N2 C2 H2D 110.0 . . ?
C1 C2 H2D 110.0 . . ?
H2C C2 H2D 108.4 . . ?
C4 C3 N3 110.9(10) . . ?
C4 C3 H3C 109.5 . . ?
N3 C3 H3C 109.5 . . ?
C4 C3 H3D 109.5 . . ?
N3 C3 H3D 109.5 . . ?
H3C C3 H3D 108.1 . . ?
C3 C4 N4 107.6(10) . . ?
C3 C4 H4C 110.2 . . ?
N4 C4 H4C 110.2 . . ?
C3 C4 H4D 110.2 . . ?
N4 C4 H4D 110.2 . . ?
H4C C4 H4D 108.5 . . ?
N5 C5 C6 109.3(11) . . ?
N5 C5 H5C 109.8 . . ?
C6 C5 H5C 109.8 . . ?
N5 C5 H5D 109.8 . . ?
C6 C5 H5D 109.8 . . ?
H5C C5 H5D 108.3 . . ?
N6 C6 C5 108.8(10) . . ?
N6 C6 H6C 109.9 . . ?
C5 C6 H6C 109.9 . . ?
N6 C6 H6D 109.9 . . ?
C5 C6 H6D 109.9 . . ?
H6C C6 H6D 108.3 . . ?

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
Ni1 N1 C1 C2 41.2(12) . . . . ?
Ni1 N2 C2 C1 41.6(12) . . . . ?
N1 C1 C2 N2 -56.2(14) . . . . ?
Ni1 N3 C3 C4 -36.8(12) . . . . ?
N3 C3 C4 N4 52.0(14) . . . . ?
Ni1 N4 C4 C3 -41.2(12) . . . . ?
Ni1 N5 C5 C6 40.7(12) . . . . ?
Ni1 N6 C6 C5 40.3(14) . . . . ?
N5 C5 C6 N6 -54.7(15) . . . . ?

_refine_diff_density_max         1.502
_refine_diff_density_min         -1.374
_refine_diff_density_rms         0.181



