# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A.
# 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_ggc
_database_code_depnum_ccdc_archive 'CCDC 1506170'
_audit_update_record             
;
2016-09-24 deposited with the CCDC.
2017-04-21 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         '2(C18 H6.50 O Pb3 S6), 6(H2 O)'
_chemical_formula_sum            'C36 H25 O8 Pb6 S12'
_chemical_formula_weight         2213.48

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -4.0753 8.5060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           205
_space_group_name_H-M_alt        'P a -3'
_space_group_name_Hall           '-P 2ac 2ab 3'

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

_cell_length_a                   19.88410(10)
_cell_length_b                   19.88410(10)
_cell_length_c                   19.88410(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7861.72(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8768
_cell_measurement_theta_min      3.1180
_cell_measurement_theta_max      73.7360
_cell_oxdiff_length_a            19.8930(6)
_cell_oxdiff_length_b            19.8552(7)
_cell_oxdiff_length_c            19.9042(6)
_cell_oxdiff_angle_alpha         89.998(3)
_cell_oxdiff_angle_beta          89.964(2)
_cell_oxdiff_angle_gamma         90.054(3)
_cell_oxdiff_volume              7861.7(4)
_cell_oxdiff_measurement_reflns_used 8768

_exptl_crystal_description       octahedron
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.870
_exptl_crystal_F_000             3956
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.235
_exptl_crystal_size_mid          0.162
_exptl_crystal_size_min          0.157
_exptl_absorpt_coefficient_mu    27.685
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.21263
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5148
_diffrn_detector_type            Atlas
_diffrn_reflns_number            21276
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_av_R_equivalents  0.0879
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.850
_diffrn_reflns_theta_max         73.715
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2650
_reflns_number_gt                2235
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .
_diffrn_orient_matrix_UB_11      -0.0040270000
_diffrn_orient_matrix_UB_12      -0.0735413000
_diffrn_orient_matrix_UB_13      -0.0243508000
_diffrn_orient_matrix_UB_21      -0.0412012000
_diffrn_orient_matrix_UB_22      -0.0186893000
_diffrn_orient_matrix_UB_23      0.0628666000
_diffrn_orient_matrix_UB_31      -0.0654492000
_diffrn_orient_matrix_UB_32      0.0162041000
_diffrn_orient_matrix_UB_33      -0.0380189000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -74.00   35.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.3249   77.0000  -90.0000 109

#__ type_ start__ end____ width___ exp.time_
  2 omega  -74.00   35.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.3249   77.0000  120.0000 109

#__ type_ start__ end____ width___ exp.time_
  3 omega   88.00  144.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -      106.3615   77.0000  150.0000 56

#__ type_ start__ end____ width___ exp.time_
  4 omega   86.00  165.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -      106.3615   77.0000   60.0000 79

#__ type_ start__ end____ width___ exp.time_
  5 omega   85.00  178.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -      106.3615   77.0000 -180.0000 93

#__ type_ start__ end____ width___ exp.time_
  6 omega  117.00  162.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -      106.3615   77.0000   30.0000 45

;


_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_computing_structure_refinement  
;  
SHELXL-2014/7 (Sheldrick, 2014), 
SHELXLE Rev714 (Hübschle et al., 2011)
;
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
An oxygen atom (O1) is located in hydrogen bonding distance to its 
symmetry equivalent counterpart across an inversion center. It was 
refined as being protonated half the time. 

A difference electron density peak located in the void space atop of 
the plane of the aromatic moieties was tentatively refined as a water 
molecule. Partial occupancy of this site with sodium cannot be 
categorically excluded. The water molecule is in hydrogen bonding 
distance to two copies of itself across a threefold axis. H atoms 
were added and restrained with O-H distances of 0.84(2) Angstrom and 
H...H distances within each molecule of 1.36(2) Angstrom. The distance 
of one of the two H atoms to the neighboring symmetry created oxygen 
atom was restrained to 1.95(2) Angstrom. 
 

Two carbon atoms, C1 and C2, were restrained to be close to isotropic. 
  
The structure contains additional solvent accessible voids of 3674 Ang3 
combined. No substantial electron density peaks were found in 
the solvent accessible voids (less than 2.5 electron per cubic Angstrom) and 
the residual electron density peaks are not arranged in an interpretable 
pattern. The hkl file was instead corrected using reverse Fourier 
transform methods using the SQUEEZE routine (P. van der Sluis & A.L. Spek 
(1990). Acta Cryst. A46, 194-201) as implemented in the program Platon. 
The resultant files were used in the further
refinement. (The FAB file with details of the Squeeze results is appended 
to this cif file). The Squeeze procedure corrected for 1040 electrons within 
the solvent accessible voids.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0655P)²+251.8441P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2650
_refine_ls_number_parameters     100
_refine_ls_number_restraints     16
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0574
_refine_ls_wR_factor_ref         0.1535
_refine_ls_wR_factor_gt          0.1424
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_restrained_S_all      1.085
_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
C1 C 0.2426(6) 0.4888(6) 0.4638(6) 0.027(3) Uani 1 1 d . U . . .
O1 O 0.0386(4) 0.4614(4) 0.5386(4) 0.020(3) Uani 1 3 d S T P . .
H1 H 0.0101 0.4899 0.5101 0.023 Uiso 0.1667 1 calc R U P A -1
C2 C 0.2529(5) 0.4358(5) 0.5143(6) 0.019(2) Uani 1 1 d . U . . .
C3 C 0.3054(5) 0.3891(5) 0.5066(6) 0.019(2) Uani 1 1 d . . . . .
H3 H 0.3098 0.3546 0.5379 0.022 Uiso 1 1 calc R U . . .
C4 C 0.3510(6) 0.3932(6) 0.4534(6) 0.021(2) Uani 1 1 d . . . . .
C5 C 0.3444(6) 0.4465(6) 0.4044(6) 0.022(2) Uani 1 1 d . . . . .
C6 C 0.2899(5) 0.4901(6) 0.4129(6) 0.021(2) Uani 1 1 d . . . . .
H6 H 0.2850 0.5237 0.3807 0.025 Uiso 1 1 calc R U . . .
S1 S 0.17717(15) 0.54536(16) 0.46836(17) 0.0316(7) Uani 1 1 d . . . . .
S2 S 0.20008(14) 0.42427(15) 0.58459(15) 0.0244(6) Uani 1 1 d . . . . .
Pb1 Pb 0.11701(2) 0.52937(2) 0.58982(2) 0.02477(19) Uani 1 1 d . . . . .
O2 O 0.2428(9) 0.2994(8) 0.3468(8) 0.087(5) Uani 1 1 d D . . . .
H2B H 0.215(10) 0.268(8) 0.344(14) 0.131 Uiso 1 1 d D U . . .
H2A H 0.235(5) 0.326(9) 0.314(7) 0.131 Uiso 1 1 d D 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
C1 C6 1.381(16) . ?
C1 C2 1.471(16) . ?
C1 S1 1.722(13) . ?
O1 Pb1 2.301(4) . ?
O1 Pb1 2.301(4) 6_456 ?
O1 Pb1 2.301(4) 12_565 ?
O1 H1 0.9800 . ?
C2 C3 1.404(15) . ?
C2 S2 1.763(11) . ?
C3 C4 1.396(15) . ?
C3 H3 0.9300 . ?
C4 C5 1.445(15) 5 ?
C4 C5 1.445(15) . ?
C5 C6 1.399(15) . ?
C5 C4 1.445(15) 9 ?
C6 H6 0.9300 . ?
S1 Pb1 2.714(3) . ?
S2 Pb1 2.666(3) . ?
O2 H2B 0.85(2) . ?
O2 H2A 0.85(2) . ?

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
C6 C1 C2 114.7(11) . . ?
C6 C1 S1 122.8(10) . . ?
C2 C1 S1 122.5(9) . . ?
Pb1 O1 Pb1 111.0(3) . 6_456 ?
Pb1 O1 Pb1 111.0(3) . 12_565 ?
Pb1 O1 Pb1 111.0(3) 6_456 12_565 ?
Pb1 O1 H1 107.9 . . ?
Pb1 O1 H1 107.9 6_456 . ?
Pb1 O1 H1 107.9 12_565 . ?
C3 C2 C1 120.2(10) . . ?
C3 C2 S2 116.3(8) . . ?
C1 C2 S2 123.5(9) . . ?
C4 C3 C2 121.8(10) . . ?
C4 C3 H3 119.1 . . ?
C2 C3 H3 119.1 . . ?
C3 C4 C5 120.8(10) . 5 ?
C3 C4 C5 119.7(10) . . ?
C5 C4 C5 119.5(11) 5 . ?
C6 C5 C4 123.3(10) . 9 ?
C6 C5 C4 116.3(10) . . ?
C4 C5 C4 120.4(11) 9 . ?
C1 C6 C5 127.2(11) . . ?
C1 C6 H6 116.4 . . ?
C5 C6 H6 116.4 . . ?
C1 S1 Pb1 107.7(4) . . ?
C2 S2 Pb1 107.4(4) . . ?
O1 Pb1 S2 86.7(3) . . ?
O1 Pb1 S1 88.48(13) . . ?
S2 Pb1 S1 77.53(9) . . ?
H2B O2 H2A 107(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
C6 C1 C2 C3 -3.5(16) . . . . ?
S1 C1 C2 C3 177.2(9) . . . . ?
C6 C1 C2 S2 179.3(9) . . . . ?
S1 C1 C2 S2 -0.1(15) . . . . ?
C1 C2 C3 C4 3.2(17) . . . . ?
S2 C2 C3 C4 -179.4(9) . . . . ?
C2 C3 C4 C5 -179.8(11) . . . 5 ?
C2 C3 C4 C5 -0.3(18) . . . . ?
C3 C4 C5 C6 -2.1(17) . . . . ?
C5 C4 C5 C6 177.5(8) 5 . . . ?
C3 C4 C5 C4 176.9(8) . . . 9 ?
C5 C4 C5 C4 -4(2) 5 . . 9 ?
C2 C1 C6 C5 1.1(18) . . . . ?
S1 C1 C6 C5 -179.6(10) . . . . ?
C4 C5 C6 C1 -177.3(12) 9 . . . ?
C4 C5 C6 C1 1.6(19) . . . . ?
C6 C1 S1 Pb1 -170.2(9) . . . . ?
C2 C1 S1 Pb1 9.1(11) . . . . ?
C3 C2 S2 Pb1 173.5(8) . . . . ?
C1 C2 S2 Pb1 -9.1(10) . . . . ?

_refine_diff_density_max         2.603
_refine_diff_density_min         -1.609
_refine_diff_density_rms         0.294




