# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_a
_database_code_depnum_ccdc_archive 'CCDC 1507207'
_audit_update_record             
;
2017-08-24 deposited with the CCDC.
2017-10-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C48 H32 Cu2 I10 N8 Pb3'
_chemical_formula_sum            'C48 H32 Cu2 I10 N8 Pb3'
_chemical_formula_weight         2738.47

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'
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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21/n
_symmetry_space_group_name_Hall  '-P 2yn'

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

_cell_length_a                   13.0188(6)
_cell_length_b                   15.3408(6)
_cell_length_c                   16.2776(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 112.263(5)
_cell_angle_gamma                90.00
_cell_volume                     3008.6(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4995
_cell_measurement_theta_min      3.1380
_cell_measurement_theta_max      28.6510

_exptl_crystal_description       Prism
_exptl_crystal_colour            Black
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.023
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2420
_exptl_absorpt_coefficient_mu    14.232
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.47599
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   'CrystalClear (Rigaku,2007)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Sealed Tube'
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_measurement_device_type  'Rigaku Mercury CCD diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            20210
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_sigmaI/netI    0.0418
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.70
_diffrn_reflns_theta_max         29.21
_reflns_number_total             7123
_reflns_number_gt                5640
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku, 2007)'
_computing_cell_refinement       'CrystalClear (Rigaku, 2007)'
_computing_data_reduction        'CrystalClear (Rigaku, 2007)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'XP (Sheldrick, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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)+(0.0273P)²+3.7078P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7123
_refine_ls_number_parameters     322
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0377
_refine_ls_wR_factor_ref         0.0778
_refine_ls_wR_factor_gt          0.0716
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.063
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.67408(2) 0.972557(18) 0.484662(17) 0.04080(8) Uani 1 1 d . . .
Pb2 Pb 1.0000 1.0000 0.5000 0.04232(11) Uani 1 2 d S . .
Cu1 Cu 0.68693(7) 0.67777(6) 0.45132(5) 0.0396(2) Uani 1 1 d . . .
I1 I 0.53785(4) 0.79966(3) 0.39598(3) 0.04703(13) Uani 1 1 d . . .
I2 I 0.43639(4) 1.05652(4) 0.36546(3) 0.05386(14) Uani 1 1 d . . .
I3 I 0.78019(4) 0.94922(4) 0.33718(3) 0.04910(14) Uani 1 1 d . . .
I4 I 0.83448(5) 1.14190(3) 0.54262(3) 0.06406(17) Uani 1 1 d . . .
I5 I 0.89734(4) 0.87405(3) 0.61102(3) 0.04969(13) Uani 1 1 d . . .
N1 N 0.7423(5) 0.6893(3) 0.3533(4) 0.0387(13) Uani 1 1 d . . .
N2 N 0.8542(4) 0.6467(4) 0.5227(4) 0.0393(13) Uani 1 1 d . . .
N3 N 0.6321(4) 0.5448(4) 0.4196(3) 0.0351(12) Uani 1 1 d . . .
N4 N 0.6561(5) 0.6470(4) 0.5589(3) 0.0383(13) Uani 1 1 d . . .
C1 C 0.6837(7) 0.7091(5) 0.2690(5) 0.054(2) Uani 1 1 d . . .
H1A H 0.6094 0.7246 0.2518 0.065 Uiso 1 1 calc R . .
C2 C 0.7327(8) 0.7068(5) 0.2057(5) 0.056(2) Uani 1 1 d . . .
H2A H 0.6910 0.7218 0.1471 0.067 Uiso 1 1 calc R . .
C3 C 0.8395(8) 0.6832(5) 0.2290(6) 0.061(2) Uani 1 1 d . . .
H3A H 0.8709 0.6809 0.1864 0.073 Uiso 1 1 calc R . .
C4 C 0.9032(7) 0.6622(5) 0.3169(5) 0.0489(19) Uani 1 1 d . . .
C5 C 0.8494(6) 0.6651(4) 0.3772(5) 0.0392(16) Uani 1 1 d . . .
C6 C 1.0159(8) 0.6367(6) 0.3476(7) 0.070(3) Uani 1 1 d . . .
H6A H 1.0524 0.6342 0.3084 0.084 Uiso 1 1 calc R . .
C7 C 1.0698(7) 0.6161(6) 0.4329(8) 0.077(3) Uani 1 1 d . . .
H7A H 1.1436 0.5991 0.4511 0.092 Uiso 1 1 calc R . .
C8 C 1.0215(6) 0.6187(5) 0.4969(6) 0.054(2) Uani 1 1 d . . .
C9 C 0.9096(5) 0.6430(4) 0.4679(5) 0.0387(16) Uani 1 1 d . . .
C10 C 1.0735(7) 0.5975(6) 0.5878(6) 0.068(3) Uani 1 1 d . . .
H10A H 1.1474 0.5800 0.6103 0.081 Uiso 1 1 calc R . .
C11 C 1.0181(7) 0.6022(6) 0.6415(6) 0.059(2) Uani 1 1 d . . .
H11A H 1.0532 0.5892 0.7015 0.071 Uiso 1 1 calc R . .
C12 C 0.9068(6) 0.6268(5) 0.6068(5) 0.051(2) Uani 1 1 d . . .
H12A H 0.8682 0.6293 0.6446 0.062 Uiso 1 1 calc R . .
C13 C 0.6167(6) 0.4944(5) 0.3499(5) 0.0475(18) Uani 1 1 d . . .
H13A H 0.6129 0.5206 0.2973 0.057 Uiso 1 1 calc R . .
C14 C 0.6059(6) 0.4039(5) 0.3514(5) 0.0512(19) Uani 1 1 d . . .
H14A H 0.5917 0.3718 0.2998 0.061 Uiso 1 1 calc R . .
C15 C 0.6161(6) 0.3629(5) 0.4277(6) 0.052(2) Uani 1 1 d . . .
H15A H 0.6130 0.3025 0.4302 0.062 Uiso 1 1 calc R . .
C16 C 0.6316(5) 0.4146(5) 0.5035(5) 0.0394(16) Uani 1 1 d . . .
C17 C 0.6370(5) 0.5037(4) 0.4954(4) 0.0349(15) Uani 1 1 d . . .
C18 C 0.6429(6) 0.3782(5) 0.5881(6) 0.052(2) Uani 1 1 d . . .
H18A H 0.6417 0.3181 0.5947 0.063 Uiso 1 1 calc R . .
C19 C 0.6552(6) 0.4299(5) 0.6568(5) 0.054(2) Uani 1 1 d . . .
H19A H 0.6608 0.4047 0.7103 0.065 Uiso 1 1 calc R . .
C20 C 0.6601(5) 0.5233(5) 0.6512(5) 0.0432(17) Uani 1 1 d . . .
C21 C 0.6502(5) 0.5595(4) 0.5693(4) 0.0345(15) Uani 1 1 d . . .
C22 C 0.6708(7) 0.5796(6) 0.7194(5) 0.058(2) Uani 1 1 d . . .
H22A H 0.6756 0.5576 0.7740 0.070 Uiso 1 1 calc R . .
C23 C 0.6745(6) 0.6657(6) 0.7084(5) 0.055(2) Uani 1 1 d . . .
H23A H 0.6830 0.7031 0.7556 0.066 Uiso 1 1 calc R . .
C24 C 0.6654(6) 0.7003(5) 0.6255(5) 0.0489(18) Uani 1 1 d . . .
H24A H 0.6659 0.7603 0.6177 0.059 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 I3 3.2114(6) . ?
Pb1 I1 3.2132(6) . ?
Pb1 I5 3.2300(6) . ?
Pb1 I2 3.2326(6) . ?
Pb1 I4 3.2414(6) . ?
Pb1 I2 3.2981(6) 3_676 ?
Pb2 I3 3.1739(5) 3_776 ?
Pb2 I3 3.1739(5) . ?
Pb2 I5 3.2580(5) . ?
Pb2 I5 3.2580(5) 3_776 ?
Pb2 I4 3.3161(6) . ?
Pb2 I4 3.3161(6) 3_776 ?
Cu1 N1 1.992(6) . ?
Cu1 N4 1.995(5) . ?
Cu1 N2 2.098(5) . ?
Cu1 N3 2.158(5) . ?
Cu1 I1 2.5980(9) . ?
I2 Pb1 3.2981(6) 3_676 ?
N1 C1 1.328(9) . ?
N1 C5 1.350(8) . ?
N2 C12 1.313(9) . ?
N2 C9 1.344(8) . ?
N3 C13 1.324(8) . ?
N3 C17 1.364(8) . ?
N4 C24 1.326(8) . ?
N4 C21 1.359(8) . ?
C1 C2 1.403(11) . ?
C1 H1A 0.9300 . ?
C2 C3 1.344(11) . ?
C2 H2A 0.9300 . ?
C3 C4 1.393(11) . ?
C3 H3A 0.9300 . ?
C4 C5 1.405(9) . ?
C4 C6 1.415(11) . ?
C5 C9 1.426(10) . ?
C6 C7 1.335(13) . ?
C6 H6A 0.9300 . ?
C7 C8 1.406(12) . ?
C7 H7A 0.9300 . ?
C8 C9 1.401(10) . ?
C8 C10 1.412(12) . ?
C10 C11 1.330(12) . ?
C10 H10A 0.9300 . ?
C11 C12 1.394(10) . ?
C11 H11A 0.9300 . ?
C12 H12A 0.9300 . ?
C13 C14 1.397(10) . ?
C13 H13A 0.9300 . ?
C14 C15 1.353(11) . ?
C14 H14A 0.9300 . ?
C15 C16 1.416(10) . ?
C15 H15A 0.9300 . ?
C16 C17 1.379(9) . ?
C16 C18 1.439(10) . ?
C17 C21 1.433(9) . ?
C18 C19 1.330(11) . ?
C18 H18A 0.9300 . ?
C19 C20 1.440(11) . ?
C19 H19A 0.9300 . ?
C20 C22 1.371(11) . ?
C20 C21 1.405(9) . ?
C22 C23 1.336(12) . ?
C22 H22A 0.9300 . ?
C23 C24 1.412(10) . ?
C23 H23A 0.9300 . ?
C24 H24A 0.9300 . ?

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 I1 83.837(15) . . ?
I3 Pb1 I5 83.433(15) . . ?
I1 Pb1 I5 96.330(15) . . ?
I3 Pb1 I2 100.417(15) . . ?
I1 Pb1 I2 79.592(15) . . ?
I5 Pb1 I2 173.980(17) . . ?
I3 Pb1 I4 83.959(15) . . ?
I1 Pb1 I4 167.796(17) . . ?
I5 Pb1 I4 82.215(16) . . ?
I2 Pb1 I4 102.709(18) . . ?
I3 Pb1 I2 165.820(17) . 3_676 ?
I1 Pb1 I2 84.235(16) . 3_676 ?
I5 Pb1 I2 90.293(14) . 3_676 ?
I2 Pb1 I2 84.914(14) . 3_676 ?
I4 Pb1 I2 107.847(16) . 3_676 ?
I3 Pb2 I3 180.0 3_776 . ?
I3 Pb2 I5 96.427(13) 3_776 . ?
I3 Pb2 I5 83.573(13) . . ?
I3 Pb2 I5 83.573(13) 3_776 3_776 ?
I3 Pb2 I5 96.427(12) . 3_776 ?
I5 Pb2 I5 180.000(15) . 3_776 ?
I3 Pb2 I4 96.659(14) 3_776 . ?
I3 Pb2 I4 83.341(14) . . ?
I5 Pb2 I4 80.657(14) . . ?
I5 Pb2 I4 99.343(14) 3_776 . ?
I3 Pb2 I4 83.341(14) 3_776 3_776 ?
I3 Pb2 I4 96.659(14) . 3_776 ?
I5 Pb2 I4 99.343(14) . 3_776 ?
I5 Pb2 I4 80.657(14) 3_776 3_776 ?
I4 Pb2 I4 180.0 . 3_776 ?
N1 Cu1 N4 167.9(2) . . ?
N1 Cu1 N2 81.3(2) . . ?
N4 Cu1 N2 88.4(2) . . ?
N1 Cu1 N3 94.5(2) . . ?
N4 Cu1 N3 80.1(2) . . ?
N2 Cu1 N3 95.6(2) . . ?
N1 Cu1 I1 96.21(16) . . ?
N4 Cu1 I1 95.87(17) . . ?
N2 Cu1 I1 146.90(16) . . ?
N3 Cu1 I1 117.49(14) . . ?
Cu1 I1 Pb1 103.04(2) . . ?
Pb1 I2 Pb1 95.086(14) . 3_676 ?
Pb2 I3 Pb1 81.693(12) . . ?
Pb1 I4 Pb2 79.108(13) . . ?
Pb1 I5 Pb2 80.133(12) . . ?
C1 N1 C5 119.1(6) . . ?
C1 N1 Cu1 127.4(5) . . ?
C5 N1 Cu1 113.1(4) . . ?
C12 N2 C9 118.9(6) . . ?
C12 N2 Cu1 130.6(5) . . ?
C9 N2 Cu1 110.4(4) . . ?
C13 N3 C17 116.5(6) . . ?
C13 N3 Cu1 133.3(5) . . ?
C17 N3 Cu1 108.8(4) . . ?
C24 N4 C21 119.9(6) . . ?
C24 N4 Cu1 125.9(5) . . ?
C21 N4 Cu1 112.4(4) . . ?
N1 C1 C2 120.7(8) . . ?
N1 C1 H1A 119.7 . . ?
C2 C1 H1A 119.7 . . ?
C3 C2 C1 120.6(7) . . ?
C3 C2 H2A 119.7 . . ?
C1 C2 H2A 119.7 . . ?
C2 C3 C4 120.1(7) . . ?
C2 C3 H3A 120.0 . . ?
C4 C3 H3A 120.0 . . ?
C3 C4 C5 116.7(7) . . ?
C3 C4 C6 124.1(8) . . ?
C5 C4 C6 119.1(7) . . ?
N1 C5 C4 122.8(7) . . ?
N1 C5 C9 117.8(6) . . ?
C4 C5 C9 119.5(7) . . ?
C7 C6 C4 119.9(8) . . ?
C7 C6 H6A 120.1 . . ?
C4 C6 H6A 120.1 . . ?
C6 C7 C8 123.9(8) . . ?
C6 C7 H7A 118.1 . . ?
C8 C7 H7A 118.1 . . ?
C9 C8 C7 117.3(8) . . ?
C9 C8 C10 116.0(8) . . ?
C7 C8 C10 126.7(8) . . ?
N2 C9 C8 122.6(7) . . ?
N2 C9 C5 117.0(6) . . ?
C8 C9 C5 120.4(7) . . ?
C11 C10 C8 120.8(8) . . ?
C11 C10 H10A 119.6 . . ?
C8 C10 H10A 119.6 . . ?
C10 C11 C12 119.2(8) . . ?
C10 C11 H11A 120.4 . . ?
C12 C11 H11A 120.4 . . ?
N2 C12 C11 122.4(8) . . ?
N2 C12 H12A 118.8 . . ?
C11 C12 H12A 118.8 . . ?
N3 C13 C14 123.2(7) . . ?
N3 C13 H13A 118.4 . . ?
C14 C13 H13A 118.4 . . ?
C15 C14 C13 120.2(7) . . ?
C15 C14 H14A 119.9 . . ?
C13 C14 H14A 119.9 . . ?
C14 C15 C16 118.2(7) . . ?
C14 C15 H15A 120.9 . . ?
C16 C15 H15A 120.9 . . ?
C17 C16 C15 117.8(7) . . ?
C17 C16 C18 119.1(7) . . ?
C15 C16 C18 123.1(7) . . ?
N3 C17 C16 124.0(6) . . ?
N3 C17 C21 115.6(6) . . ?
C16 C17 C21 120.4(6) . . ?
C19 C18 C16 120.6(7) . . ?
C19 C18 H18A 119.7 . . ?
C16 C18 H18A 119.7 . . ?
C18 C19 C20 122.3(7) . . ?
C18 C19 H19A 118.9 . . ?
C20 C19 H19A 118.9 . . ?
C22 C20 C21 117.7(7) . . ?
C22 C20 C19 124.7(7) . . ?
C21 C20 C19 117.6(7) . . ?
N4 C21 C20 121.3(6) . . ?
N4 C21 C17 118.7(6) . . ?
C20 C21 C17 120.0(6) . . ?
C23 C22 C20 120.8(7) . . ?
C23 C22 H22A 119.6 . . ?
C20 C22 H22A 119.6 . . ?
C22 C23 C24 120.3(8) . . ?
C22 C23 H23A 119.9 . . ?
C24 C23 H23A 119.9 . . ?
N4 C24 C23 119.9(7) . . ?
N4 C24 H24A 120.0 . . ?
C23 C24 H24A 120.0 . . ?

_diffrn_measured_fraction_theta_max 0.873
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.302
_refine_diff_density_min         -1.024
_refine_diff_density_rms         0.163
