# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1566082'
_audit_update_record             
;
2017-08-02 deposited with the CCDC.
2017-09-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H20 Cu6 I2 N4 O20 S0'
_chemical_formula_weight         1367.52

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'
N N 0.0311 0.0180 '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'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   I4/mmm

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 -0.030 -0.018 -0.018 4047.1 614.0
_platon_squeeze_details          
;
;

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

_cell_length_a                   18.5020(2)
_cell_length_b                   18.5020(2)
_cell_length_c                   20.9217(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     7162.0(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4180
_cell_measurement_theta_min      4.2040
_cell_measurement_theta_max      70.1050

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2624
_exptl_absorpt_coefficient_mu    9.133
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.65466
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7659
_diffrn_reflns_av_R_equivalents  0.0202
_diffrn_reflns_av_sigmaI/netI    0.0151
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.38
_diffrn_reflns_theta_max         70.23
_reflns_number_total             1932
_reflns_number_gt                1811
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0970P)²+12.2888P] 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         1932
_refine_ls_number_parameters     80
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0426
_refine_ls_wR_factor_ref         0.1409
_refine_ls_wR_factor_gt          0.1394
_refine_ls_goodness_of_fit_ref   1.085
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.07308(7) 0.5000 0.0000 0.0431(3) Uani 1 4 d S . .
Cu2 Cu 0.28620(3) 0.71380(3) -0.29536(3) 0.0319(2) Uani 1 2 d S . .
I1 I 0.0000 0.37830(3) 0.0063(5) 0.0438(11) Uani 0.50 2 d SP . .
C1 C 0.1622(2) 0.5621(2) -0.10570(17) 0.0412(8) Uani 1 1 d . . .
H1A H 0.1472 0.6054 -0.0875 0.049 Uiso 1 1 calc R . .
C2 C 0.2064(2) 0.5648(2) -0.15859(18) 0.0399(8) Uani 1 1 d . . .
C3 C 0.2295(3) 0.5000 -0.1858(3) 0.0418(11) Uani 1 2 d S . .
H3A H 0.2597 0.5000 -0.2213 0.050 Uiso 1 2 calc SR . .
C4 C 0.2256(2) 0.6353(2) -0.18948(19) 0.0409(8) Uani 1 1 d . . .
N1 N 0.1398(3) 0.5000 -0.0793(2) 0.0424(10) Uani 1 2 d S . .
O1 O 0.26226(17) 0.63156(14) -0.23977(15) 0.0495(7) Uani 1 1 d . . .
O1W O 0.3488(2) 0.6512(2) -0.3611(3) 0.0870(18) Uani 1 2 d S . .
O2 O 0.20217(16) 0.69155(14) -0.16368(14) 0.0488(7) Uani 1 1 d . . .

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
Cu1 0.0571(7) 0.0353(6) 0.0369(5) 0.000 0.000 0.000
Cu2 0.0276(3) 0.0276(3) 0.0405(4) -0.00714(18) 0.00714(18) -0.0032(2)
I1 0.0550(4) 0.0294(3) 0.047(3) 0.0023(5) 0.000 0.000
C1 0.048(2) 0.0295(17) 0.0464(18) -0.0017(15) 0.0052(16) -0.0016(14)
C2 0.0387(19) 0.0332(19) 0.0480(19) 0.0016(15) 0.0019(15) -0.0029(14)
C3 0.042(3) 0.033(3) 0.050(3) 0.000 0.008(2) 0.000
C4 0.0394(19) 0.0328(18) 0.0506(19) -0.0019(16) 0.0010(16) -0.0056(14)
N1 0.057(3) 0.030(2) 0.040(2) 0.000 0.008(2) 0.000
O1 0.0581(17) 0.0323(13) 0.0582(16) 0.0012(12) 0.0187(13) -0.0012(11)
O1W 0.086(2) 0.086(2) 0.089(4) -0.036(2) 0.036(2) 0.024(3)
O2 0.0582(16) 0.0321(14) 0.0561(16) -0.0017(11) 0.0143(13) -0.0045(11)

_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
Cu1 N1 2.067(5) 18 ?
Cu1 N1 2.067(5) . ?
Cu1 I1 2.6299(10) . ?
Cu1 I1 2.6299(10) 2_565 ?
Cu1 I1 2.6299(10) 17_565 ?
Cu1 I1 2.6299(10) 18 ?
Cu1 Cu1 2.704(2) 17_565 ?
Cu2 O2 1.961(3) 25_564 ?
Cu2 O2 1.961(3) 15_454 ?
Cu2 O1 1.966(3) 23_665 ?
Cu2 O1 1.966(3) . ?
Cu2 O1W 2.138(4) . ?
Cu2 Cu2 2.6817(13) 25_564 ?
I1 I1 0.26(2) 18 ?
I1 Cu1 2.6299(10) 17_565 ?
C1 N1 1.341(4) . ?
C1 C2 1.377(5) . ?
C1 H1A 0.9300 . ?
C2 C3 1.394(5) . ?
C2 C4 1.498(5) . ?
C3 C2 1.394(5) 21_565 ?
C3 H3A 0.9300 . ?
C4 O2 1.251(5) . ?
C4 O1 1.253(5) . ?
N1 C1 1.341(4) 21_565 ?
O2 Cu2 1.961(3) 25_564 ?

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
N1 Cu1 N1 106.7(3) 18 . ?
N1 Cu1 I1 105.5(2) 18 . ?
N1 Cu1 I1 110.3(2) . . ?
N1 Cu1 I1 105.5(2) 18 2_565 ?
N1 Cu1 I1 110.3(2) . 2_565 ?
I1 Cu1 I1 117.79(6) . 2_565 ?
N1 Cu1 I1 110.3(2) 18 17_565 ?
N1 Cu1 I1 105.5(2) . 17_565 ?
I1 Cu1 I1 118.12(5) . 17_565 ?
I1 Cu1 I1 5.8(5) 2_565 17_565 ?
N1 Cu1 I1 110.3(2) 18 18 ?
N1 Cu1 I1 105.5(2) . 18 ?
I1 Cu1 I1 5.8(5) . 18 ?
I1 Cu1 I1 118.12(5) 2_565 18 ?
I1 Cu1 I1 117.79(6) 17_565 18 ?
N1 Cu1 Cu1 126.64(15) 18 17_565 ?
N1 Cu1 Cu1 126.64(15) . 17_565 ?
I1 Cu1 Cu1 59.06(3) . 17_565 ?
I1 Cu1 Cu1 59.06(3) 2_565 17_565 ?
I1 Cu1 Cu1 59.06(3) 17_565 17_565 ?
I1 Cu1 Cu1 59.06(3) 18 17_565 ?
O2 Cu2 O2 90.29(19) 25_564 15_454 ?
O2 Cu2 O1 88.42(14) 25_564 23_665 ?
O2 Cu2 O1 166.97(12) 15_454 23_665 ?
O2 Cu2 O1 166.97(12) 25_564 . ?
O2 Cu2 O1 88.42(14) 15_454 . ?
O1 Cu2 O1 89.9(2) 23_665 . ?
O2 Cu2 O1W 98.23(15) 25_564 . ?
O2 Cu2 O1W 98.23(15) 15_454 . ?
O1 Cu2 O1W 94.78(15) 23_665 . ?
O1 Cu2 O1W 94.78(15) . . ?
O2 Cu2 Cu2 85.30(8) 25_564 25_564 ?
O2 Cu2 Cu2 85.30(8) 15_454 25_564 ?
O1 Cu2 Cu2 81.68(8) 23_665 25_564 ?
O1 Cu2 Cu2 81.68(8) . 25_564 ?
O1W Cu2 Cu2 174.96(19) . 25_564 ?
I1 I1 Cu1 87.1(2) 18 . ?
I1 I1 Cu1 87.1(2) 18 17_565 ?
Cu1 I1 Cu1 61.88(5) . 17_565 ?
N1 C1 C2 123.1(4) . . ?
N1 C1 H1A 118.4 . . ?
C2 C1 H1A 118.4 . . ?
C1 C2 C3 118.6(4) . . ?
C1 C2 C4 121.3(3) . . ?
C3 C2 C4 120.0(3) . . ?
C2 C3 C2 118.7(5) . 21_565 ?
C2 C3 H3A 120.7 . . ?
C2 C3 H3A 120.7 21_565 . ?
O2 C4 O1 126.5(4) . . ?
O2 C4 C2 117.1(3) . . ?
O1 C4 C2 116.3(3) . . ?
C1 N1 C1 117.9(5) 21_565 . ?
C1 N1 Cu1 121.0(2) 21_565 . ?
C1 N1 Cu1 121.0(2) . . ?
C4 O1 Cu2 125.2(3) . . ?
C4 O2 Cu2 121.1(3) . 25_564 ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        70.23
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         1.828
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.102
