# Electronic Supplementary Material (ESI) for Nanoscale.
# This journal is © The Royal Society of Chemistry 2015

 
data_36
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C6 H24 I8 N2 O2 Pb3 S2'
_chemical_formula_weight          1857.16
 
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'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'S'  'S'   0.1246   0.1234
 '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            'Orthorhombic'
_symmetry_space_group_name_H-M    'Cmc2(1) '
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y, z+1/2'
 'x, -y, z+1/2'
 '-x, y, z'
 'x+1/2, y+1/2, z'
 '-x+1/2, -y+1/2, z+1/2'
 'x+1/2, -y+1/2, z+1/2'
 '-x+1/2, y+1/2, z'
 
_cell_length_a                    4.6212(13)
_cell_length_b                    27.484(8)
_cell_length_c                    26.923(7)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 90.00
_cell_volume                      3419.5(16)
_cell_formula_units_Z             4
_cell_measurement_temperature     296(2)
_cell_measurement_reflns_used     1331
_cell_measurement_theta_min        2.71
_cell_measurement_theta_max       23.16
 
_exptl_crystal_description        'needle'
_exptl_crystal_colour             'Translucent light yellow'
_exptl_crystal_size_max           0.40
_exptl_crystal_size_mid           0.02
_exptl_crystal_size_min           0.02
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     3.607
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              3168
_exptl_absorpt_coefficient_mu     22.084
_exptl_absorpt_correction_type    psi-scan
_exptl_absorpt_correction_T_min   0.6129
_exptl_absorpt_correction_T_max   0.8401
_exptl_absorpt_process_details    '(North et al., 1968)'
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       296(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   'CCD area detector'
_diffrn_measurement_method        'phi and omega scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             9176
_diffrn_reflns_av_R_equivalents   0.0841
_diffrn_reflns_av_sigmaI/netI     0.1352
_diffrn_reflns_limit_h_min        -4
_diffrn_reflns_limit_h_max        6
_diffrn_reflns_limit_k_min        -37
_diffrn_reflns_limit_k_max        34
_diffrn_reflns_limit_l_min        -36
_diffrn_reflns_limit_l_max        32
_diffrn_reflns_theta_min          1.48
_diffrn_reflns_theta_max          29.34
_reflns_number_total              4384
_reflns_number_gt                 2186
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection      'Bruker SMART'
_computing_cell_refinement      'Bruker SMART'
_computing_data_reduction       'Bruker SAINT'
_computing_structure_solution   'Bruker SHELXTL'
_computing_structure_refinement 'Bruker SHELXTL'
_computing_molecular_graphics   'Diamond 3'
_computing_publication_material 'Bruker SHELXTL'
 
_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)+(0.0461P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    none
_refine_ls_hydrogen_treatment     none
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        0.000049(12)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_abs_structure_details
 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack    0.421(12)
_refine_ls_number_reflns          4384
_refine_ls_number_parameters      123
_refine_ls_number_restraints      1
_refine_ls_R_factor_all           0.1237
_refine_ls_R_factor_gt            0.0538
_refine_ls_wR_factor_ref          0.1217
_refine_ls_wR_factor_gt           0.1053
_refine_ls_goodness_of_fit_ref    0.836
_refine_ls_restrained_S_all       0.836
_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
N1 N 0.5000 0.3623(14) 0.8214(14) 0.072(10) Uiso 1 2 d S . .
C1 C 0.5000 0.3692(19) 0.7622(18) 0.096(17) Uiso 1 2 d S . .
N2 N 0.5000 0.8658(16) 0.2797(16) 0.105(14) Uiso 1 2 d S . .
C2 C 0.5000 0.8818(17) 0.2276(16) 0.063(11) Uiso 1 2 d S . .
S1 S 0.144(3) 0.4466(6) 0.8936(6) 0.058(4) Uani 0.50 1 d P . .
O1 O 0.0000 0.4045(10) 0.8576(11) 0.066(8) Uani 1 2 d S . .
C3 C 0.0000 0.5032(13) 0.8794(13) 0.046(9) Uiso 1 2 d S . .
C4 C 0.0000 0.4332(18) 0.9550(16) 0.073(14) Uiso 1 2 d S . .
S2 S 0.866(3) 0.8018(5) 0.1512(5) 0.050(4) Uani 0.50 1 d P . .
O2 O 1.0000 0.8402(10) 0.1882(8) 0.058(8) Uani 1 2 d S . .
C5 C 1.0000 0.8136(15) 0.0942(14) 0.050(10) Uiso 1 2 d S . .
C6 C 1.0000 0.7491(18) 0.1654(18) 0.087(16) Uiso 1 2 d S . .
Pb1 Pb 0.5000 0.12169(6) 0.03065(6) 0.0388(3) Uani 1 2 d S . .
Pb2 Pb 0.0000 0.01055(6) 0.13482(5) 0.0444(4) Uani 1 2 d S . .
Pb3 Pb 0.0000 0.23496(6) -0.07450(5) 0.0455(4) Uani 1 2 d S . .
I1 I 0.0000 0.04303(10) 0.00964(9) 0.0427(6) Uani 1 2 d S . .
I2 I 0.0000 0.20177(9) 0.04978(9) 0.0436(7) Uani 1 2 d S . .
I3 I 0.5000 0.09665(10) 0.14830(8) 0.0443(6) Uani 1 2 d S . .
I4 I 0.5000 0.14923(10) -0.08443(9) 0.0468(7) Uani 1 2 d S . .
I5 I -0.5000 -0.06277(10) 0.10461(10) 0.0477(7) Uani 1 2 d S . .
I6 I -0.5000 0.31134(10) -0.05121(10) 0.0491(7) Uani 1 2 d S . .
I7 I 0.0000 -0.01417(11) 0.24436(10) 0.0589(8) Uani 1 2 d S . .
I8 I 0.0000 0.25415(12) -0.18449(10) 0.0601(8) Uani 1 2 d S . .
 
loop_
 _atom_site_aniso_label
 _atom_site_aniso_U_11
 _atom_site_aniso_U_22
 _atom_site_aniso_U_33
 _atom_site_aniso_U_23
 _atom_site_aniso_U_13
 _atom_site_aniso_U_12
S1 0.047(8) 0.066(11) 0.062(9) -0.019(8) 0.010(7) -0.004(7)
O1 0.07(2) 0.030(17) 0.09(2) 0.008(15) 0.000 0.000
S2 0.043(8) 0.052(9) 0.056(9) -0.016(7) -0.002(6) -0.006(6)
O2 0.063(18) 0.09(2) 0.023(12) -0.024(13) 0.000 0.000
Pb1 0.0332(6) 0.0437(8) 0.0395(7) 0.0030(6) 0.000 0.000
Pb2 0.0353(8) 0.0475(10) 0.0503(9) 0.0064(8) 0.000 0.000
Pb3 0.0430(9) 0.0496(10) 0.0439(9) 0.0069(7) 0.000 0.000
I1 0.0373(14) 0.0411(17) 0.0497(15) -0.0032(11) 0.000 0.000
I2 0.0430(16) 0.0434(17) 0.0444(15) -0.0059(11) 0.000 0.000
I3 0.0436(15) 0.0508(17) 0.0386(15) -0.0010(12) 0.000 0.000
I4 0.0589(16) 0.0473(17) 0.0341(14) 0.0025(12) 0.000 0.000
I5 0.0419(15) 0.0467(17) 0.0547(16) -0.0009(13) 0.000 0.000
I6 0.0476(16) 0.0474(17) 0.0522(15) 0.0008(12) 0.000 0.000
I7 0.0680(19) 0.062(2) 0.0472(16) -0.0007(15) 0.000 0.000
I8 0.078(2) 0.059(2) 0.0439(15) 0.0043(14) 0.000 0.000
 
_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
N1 C1 1.60(6) . ?
N2 C2 1.47(6) . ?
S1 S1 1.33(3) 4 ?
S1 O1 1.65(3) . ?
S1 C3 1.73(4) . ?
S1 C4 1.82(4) . ?
O1 S1 1.65(3) 4 ?
C3 S1 1.73(4) 4 ?
C4 S1 1.82(4) 4 ?
S2 S2 1.24(3) 4_755 ?
S2 O2 1.58(2) . ?
S2 C6 1.62(5) . ?
S2 C5 1.69(4) . ?
O2 S2 1.58(2) 4_755 ?
C5 S2 1.69(4) 4_755 ?
C6 S2 1.62(5) 4_755 ?
Pb1 I4 3.189(3) . ?
Pb1 I1 3.214(2) . ?
Pb1 I1 3.214(2) 1_655 ?
Pb1 I2 3.232(2) 1_655 ?
Pb1 I2 3.232(2) . ?
Pb1 I3 3.241(3) . ?
Pb2 I7 3.027(3) . ?
Pb2 I5 3.172(2) . ?
Pb2 I5 3.172(2) 1_655 ?
Pb2 I3 3.327(2) . ?
Pb2 I3 3.327(2) 1_455 ?
Pb3 I8 3.008(3) . ?
Pb3 I6 3.184(2) 1_655 ?
Pb3 I6 3.184(2) . ?
Pb3 I4 3.311(2) 1_455 ?
Pb3 I4 3.311(2) . ?
I1 Pb1 3.214(2) 1_455 ?
I2 Pb1 3.232(2) 1_455 ?
I3 Pb2 3.327(2) 1_655 ?
I4 Pb3 3.311(2) 1_655 ?
I5 Pb2 3.172(2) 1_455 ?
I6 Pb3 3.184(2) 1_455 ?
 
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
S1 S1 O1 66.1(7) 4 . ?
S1 S1 C3 67.4(7) 4 . ?
O1 S1 C3 110.1(15) . . ?
S1 S1 C4 68.5(7) 4 . ?
O1 S1 C4 104.1(17) . . ?
C3 S1 C4 103.9(18) . . ?
S1 O1 S1 47.7(13) . 4 ?
S1 C3 S1 45.2(14) . 4 ?
S1 C4 S1 43.0(15) 4 . ?
S2 S2 O2 66.8(6) 4_755 . ?
S2 S2 C6 67.5(8) 4_755 . ?
O2 S2 C6 107.4(19) . . ?
S2 S2 C5 68.4(7) 4_755 . ?
O2 S2 C5 107.5(16) . . ?
C6 S2 C5 104(2) . . ?
S2 O2 S2 46.3(12) . 4_755 ?
S2 C5 S2 43.2(14) 4_755 . ?
S2 C6 S2 45.0(17) 4_755 . ?
I4 Pb1 I1 89.35(6) . . ?
I4 Pb1 I1 89.35(6) . 1_655 ?
I1 Pb1 I1 91.91(8) . 1_655 ?
I4 Pb1 I2 89.61(6) . 1_655 ?
I1 Pb1 I2 178.90(9) . 1_655 ?
I1 Pb1 I2 88.40(4) 1_655 1_655 ?
I4 Pb1 I2 89.61(6) . . ?
I1 Pb1 I2 88.40(4) . . ?
I1 Pb1 I2 178.90(9) 1_655 . ?
I2 Pb1 I2 91.26(8) 1_655 . ?
I4 Pb1 I3 178.53(10) . . ?
I1 Pb1 I3 91.67(7) . . ?
I1 Pb1 I3 91.67(7) 1_655 . ?
I2 Pb1 I3 89.36(6) 1_655 . ?
I2 Pb1 I3 89.36(6) . . ?
I7 Pb2 I5 96.16(7) . . ?
I7 Pb2 I5 96.16(7) . 1_655 ?
I5 Pb2 I5 93.51(8) . 1_655 ?
I7 Pb2 I3 93.06(6) . . ?
I5 Pb2 I3 170.30(8) . . ?
I5 Pb2 I3 88.51(5) 1_655 . ?
I7 Pb2 I3 93.06(6) . 1_455 ?
I5 Pb2 I3 88.51(5) . 1_455 ?
I5 Pb2 I3 170.30(8) 1_655 1_455 ?
I3 Pb2 I3 87.97(8) . 1_455 ?
I8 Pb3 I6 94.48(8) . 1_655 ?
I8 Pb3 I6 94.48(8) . . ?
I6 Pb3 I6 93.05(9) 1_655 . ?
I8 Pb3 I4 92.60(7) . 1_455 ?
I6 Pb3 I4 172.53(8) 1_655 1_455 ?
I6 Pb3 I4 88.78(5) . 1_455 ?
I8 Pb3 I4 92.60(7) . . ?
I6 Pb3 I4 88.78(5) 1_655 . ?
I6 Pb3 I4 172.53(8) . . ?
I4 Pb3 I4 88.52(8) 1_455 . ?
Pb1 I1 Pb1 91.91(8) . 1_455 ?
Pb1 I2 Pb1 91.26(8) 1_455 . ?
Pb1 I3 Pb2 92.54(6) . . ?
Pb1 I3 Pb2 92.54(6) . 1_655 ?
Pb2 I3 Pb2 87.97(8) . 1_655 ?
Pb1 I4 Pb3 95.19(6) . 1_655 ?
Pb1 I4 Pb3 95.19(6) . . ?
Pb3 I4 Pb3 88.52(8) 1_655 . ?
Pb2 I5 Pb2 93.51(8) . 1_455 ?
Pb3 I6 Pb3 93.05(9) 1_455 . ?
 
_diffrn_measured_fraction_theta_max    0.925
_diffrn_reflns_theta_full              25.00
_diffrn_measured_fraction_theta_full   0.997
_refine_diff_density_max    1.395
_refine_diff_density_min   -1.390
_refine_diff_density_rms    0.290
