# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2013

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#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
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#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
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#  except for the purpose of generating routine backup copies
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#  data retrieval see:
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data_JLU-Liu2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C32 H49 Cl Cu4 N16 O24'
_chemical_formula_sum            'C32 H49 Cl Cu4 N16 O24'
_chemical_formula_weight         1331.48

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'

_symmetry_cell_setting           cubic
_symmetry_space_group_name_H-M   Pm-3m

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, -z'
'-y, -x, -z'
'y, -x, z'
'-y, x, z'
'x, z, -y'
'-x, z, y'
'-x, -z, -y'
'x, -z, y'
'z, y, -x'
'z, -y, x'
'-z, y, x'
'-z, -y, -x'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-y, -x, z'
'y, x, z'
'-y, x, -z'
'y, -x, -z'
'-x, -z, y'
'x, -z, -y'
'x, z, y'
'-x, z, -y'
'-z, -y, x'
'-z, y, -x'
'z, -y, -x'
'z, y, x'

_cell_length_a                   20.208(2)
_cell_length_b                   20.208(2)
_cell_length_c                   20.208(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     8252.0(16)
_cell_formula_units_Z            3
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1906
_cell_measurement_theta_min      3.02
_cell_measurement_theta_max      27.43

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    0.804
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2034
_exptl_absorpt_coefficient_mu    0.832
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7441
_exptl_absorpt_correction_T_max  0.7916
_exptl_absorpt_process_details   Process-auto

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       omega-scan
_diffrn_detector_area_resol_mean 10.0
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            77898
_diffrn_reflns_av_R_equivalents  0.1202
_diffrn_reflns_av_sigmaI/netI    0.0284
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.02
_diffrn_reflns_theta_max         27.43
_reflns_number_total             1906
_reflns_number_gt                1726
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       Process-auto
_computing_cell_refinement       Process-auto
_computing_data_reduction        Process-auto
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'materials studio 4.0'
_computing_publication_material  'materials studio 4.0'

_refine_special_details          
; 
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F^2^, conventional R-factors R are based 
 on F, with F set to zero for negative F^2^. The threshold expression of 
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F^2^ 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/[\s^2^(Fo^2^)+(0.1140P)^2^+22.2816P] where P=(Fo^2^+2Fc^2^)/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         1906
_refine_ls_number_parameters     70
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_gt           0.0736
_refine_ls_wR_factor_ref         0.2151
_refine_ls_wR_factor_gt          0.2069
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_restrained_S_all      1.145
_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
Cu1 Cu 0.41156(3) 0.41156(3) 0.0000 0.0126(3) Uani 1 4 d S . .
Cl1 Cl 0.5000 0.5000 0.0000 0.014(15) Uani 0.50 16 d SP . .
Cl1' Cl 0.5000 0.5000 0.019(4) 0.010(9) Uani 0.25 8 d SP . .
N1 N 0.4663(4) 0.3616(3) 0.0676(3) 0.0193(14) Uani 0.50 1 d PU . 1
N2 N 0.4451(3) 0.3211(3) 0.1131(3) 0.0280(14) Uani 0.50 1 d P A 1
C2 C 0.5000 0.2466(5) 0.1938(6) 0.032(2) Uani 0.50 2 d SP . 1
O1 O 0.4436(4) 0.3566(3) 0.0701(3) 0.0312(16) Uani 0.50 1 d PU . 2
C4 C 0.4418(4) 0.1710(6) 0.2647(6) 0.064(4) Uani 0.50 1 d P . 2
H4 H 0.4013 0.1537 0.2778 0.100 Uiso 0.50 1 calc P B 2
C5 C 0.5000 0.3379(5) 0.0903(5) 0.022(2) Uani 0.50 2 d SP . 2
C1 C 0.5000 0.2932(3) 0.1441(3) 0.0320(12) Uani 1 2 d S . .
C3 C 0.4417(3) 0.2200(4) 0.2200(4) 0.072(3) Uani 1 2 d S . .
H3 H 0.3957 0.2198 0.2198 0.100 Uiso 1 2 calc S C 1
O2 O 0.3279 0.3279 0.0000 0.050 Uani 0.80 4 d SPU . .
O2' O 0.3343 0.3101 0.0172 0.050 Uani 0.05 1 d PU . .

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 0.0146(3) 0.0146(3) 0.0085(4) 0.000 0.000 0.0035(3)
Cl1 0.015(5) 0.015(5) 0.01(4) 0.000 0.000 0.000
Cl1' 0.010(5) 0.010(5) 0.01(3) 0.000 0.000 0.000
N1 0.0192(17) 0.0192(17) 0.0195(16) 0.0030(9) -0.0011(10) 0.0002(10)
N2 0.028(3) 0.027(3) 0.029(3) 0.024(3) 0.002(3) -0.003(2)
C2 0.027(5) 0.034(6) 0.033(6) 0.027(5) 0.000 0.000
O1 0.0308(18) 0.0314(18) 0.0313(18) 0.0037(9) -0.0005(10) 0.0006(10)
C4 0.023(4) 0.078(7) 0.090(8) 0.073(7) 0.016(5) 0.008(4)
C5 0.021(5) 0.024(5) 0.021(5) 0.007(4) 0.000 0.000
C1 0.028(3) 0.038(3) 0.030(3) 0.013(2) 0.000 0.000
C3 0.026(3) 0.095(5) 0.095(5) 0.079(5) 0.015(3) 0.015(3)
O2 0.050 0.050 0.050 0.000 0.000 0.000
O2' 0.050 0.050 0.050 0.000 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
Cu1 O1 1.913(7) 26 ?
Cu1 O1 1.913(7) . ?
Cu1 O1 1.913(7) 13 ?
Cu1 O1 1.913(7) 38 ?
Cu1 N1 2.027(7) 26 ?
Cu1 N1 2.027(7) . ?
Cu1 N1 2.027(7) 38 ?
Cu1 N1 2.027(7) 13 ?
Cu1 O2 2.3909(8) . ?
Cu1 Cl1 2.5274(8) . ?
Cu1 Cl1' 2.557(13) . ?
Cu1 Cl1' 2.557(13) 25_665 ?
Cl1 Cl1' 0.39(8) 25_665 ?
Cl1 Cu1 2.5274(8) 3_655 ?
Cl1 Cu1 2.5274(8) 25_665 ?
Cl1 Cu1 2.5274(8) 27_565 ?
Cl1' Cl1' 0.77(17) 25_665 ?
Cl1' Cu1 2.557(13) 3_655 ?
Cl1' Cu1 2.557(13) 25_665 ?
Cl1' Cu1 2.557(13) 27_565 ?
N1 N2 1.304(8) . ?
N1 N1 1.362(15) 28_655 ?
N2 C1 1.393(7) . ?
C2 C1 1.377(10) . ?
C2 C3 1.399(7) 28_655 ?
C2 C3 1.399(7) . ?
C2 C2 1.510(18) 18_655 ?
O1 C5 1.268(8) . ?
C4 C3 1.339(8) . ?
C4 C1 1.419(9) 18_655 ?
C4 H4 0.9300 . ?
C5 O1 1.268(8) 28_655 ?
C5 C1 1.413(11) . ?
C1 N2 1.393(7) 28_655 ?
C1 C4 1.419(9) 18_655 ?
C1 C4 1.419(9) 43 ?
C3 C4 1.339(8) 43 ?
C3 C2 1.399(7) 18_655 ?
C3 H3 0.9300 . ?
O2 O2' 0.5161 26 ?
O2 O2' 0.5161 . ?
O2 O2' 0.5161 13 ?
O2 O2' 0.5161 38 ?
O2' O2' 0.6902 38 ?
O2' O2' 0.6946 26 ?
O2' O2' 0.9792 13 ?

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
O1 Cu1 O1 95.5(4) 26 . ?
O1 Cu1 O1 81.1(4) 26 13 ?
O1 Cu1 O1 160.3(4) . 13 ?
O1 Cu1 O1 160.3(4) 26 38 ?
O1 Cu1 O1 81.1(4) . 38 ?
O1 Cu1 O1 95.5(4) 13 38 ?
O1 Cu1 N1 13.4(2) 26 26 ?
O1 Cu1 N1 91.4(2) . 26 ?
O1 Cu1 N1 89.2(3) 13 26 ?
O1 Cu1 N1 169.9(3) 38 26 ?
O1 Cu1 N1 91.4(2) 26 . ?
O1 Cu1 N1 13.4(2) . . ?
O1 Cu1 N1 169.9(3) 13 . ?
O1 Cu1 N1 89.2(3) 38 . ?
N1 Cu1 N1 84.7(4) 26 . ?
O1 Cu1 N1 169.9(3) 26 38 ?
O1 Cu1 N1 89.2(3) . 38 ?
O1 Cu1 N1 91.4(2) 13 38 ?
O1 Cu1 N1 13.4(2) 38 38 ?
N1 Cu1 N1 176.1(4) 26 38 ?
N1 Cu1 N1 95.2(4) . 38 ?
O1 Cu1 N1 89.2(3) 26 13 ?
O1 Cu1 N1 169.9(3) . 13 ?
O1 Cu1 N1 13.4(2) 13 13 ?
O1 Cu1 N1 91.4(2) 38 13 ?
N1 Cu1 N1 95.2(4) 26 13 ?
N1 Cu1 N1 176.1(4) . 13 ?
N1 Cu1 N1 84.7(4) 38 13 ?
O1 Cu1 O2 80.2(2) 26 . ?
O1 Cu1 O2 80.2(2) . . ?
O1 Cu1 O2 80.2(2) 13 . ?
O1 Cu1 O2 80.2(2) 38 . ?
N1 Cu1 O2 91.9(2) 26 . ?
N1 Cu1 O2 91.9(2) . . ?
N1 Cu1 O2 91.9(2) 38 . ?
N1 Cu1 O2 91.9(2) 13 . ?
O1 Cu1 Cl1 99.8(2) 26 . ?
O1 Cu1 Cl1 99.8(2) . . ?
O1 Cu1 Cl1 99.8(2) 13 . ?
O1 Cu1 Cl1 99.8(2) 38 . ?
N1 Cu1 Cl1 88.1(2) 26 . ?
N1 Cu1 Cl1 88.1(2) . . ?
N1 Cu1 Cl1 88.1(2) 38 . ?
N1 Cu1 Cl1 88.1(2) 13 . ?
O2 Cu1 Cl1 180.00(4) . . ?
O1 Cu1 Cl1' 106.3(14) 26 . ?
O1 Cu1 Cl1' 93.3(14) . . ?
O1 Cu1 Cl1' 106.3(14) 13 . ?
O1 Cu1 Cl1' 93.3(14) 38 . ?
N1 Cu1 Cl1' 93.9(13) 26 . ?
N1 Cu1 Cl1' 82.2(13) . . ?
N1 Cu1 Cl1' 82.2(13) 38 . ?
N1 Cu1 Cl1' 93.9(13) 13 . ?
O2 Cu1 Cl1' 171.3(18) . . ?
Cl1 Cu1 Cl1' 8.7(18) . . ?
O1 Cu1 Cl1' 93.3(14) 26 25_665 ?
O1 Cu1 Cl1' 106.3(14) . 25_665 ?
O1 Cu1 Cl1' 93.3(14) 13 25_665 ?
O1 Cu1 Cl1' 106.3(14) 38 25_665 ?
N1 Cu1 Cl1' 82.2(13) 26 25_665 ?
N1 Cu1 Cl1' 93.9(13) . 25_665 ?
N1 Cu1 Cl1' 93.9(13) 38 25_665 ?
N1 Cu1 Cl1' 82.2(13) 13 25_665 ?
O2 Cu1 Cl1' 171.3(18) . 25_665 ?
Cl1 Cu1 Cl1' 8.7(18) . 25_665 ?
Cl1' Cu1 Cl1' 17(4) . 25_665 ?
Cl1' Cl1 Cu1 90.000(15) 25_665 3_655 ?
Cl1' Cl1 Cu1 90.000(15) 25_665 . ?
Cu1 Cl1 Cu1 90.0 3_655 . ?
Cl1' Cl1 Cu1 90.000(15) 25_665 25_665 ?
Cu1 Cl1 Cu1 90.0 3_655 25_665 ?
Cu1 Cl1 Cu1 180.000(17) . 25_665 ?
Cl1' Cl1 Cu1 90.000(15) 25_665 27_565 ?
Cu1 Cl1 Cu1 180.0 3_655 27_565 ?
Cu1 Cl1 Cu1 90.0 . 27_565 ?
Cu1 Cl1 Cu1 90.0 25_665 27_565 ?
Cl1' Cl1' Cu1 81.3(19) 25_665 . ?
Cl1' Cl1' Cu1 81.3(18) 25_665 3_655 ?
Cu1 Cl1' Cu1 88.7(6) . 3_655 ?
Cl1' Cl1' Cu1 81.3(18) 25_665 25_665 ?
Cu1 Cl1' Cu1 163(4) . 25_665 ?
Cu1 Cl1' Cu1 88.7(6) 3_655 25_665 ?
Cl1' Cl1' Cu1 81.3(19) 25_665 27_565 ?
Cu1 Cl1' Cu1 88.7(6) . 27_565 ?
Cu1 Cl1' Cu1 163(4) 3_655 27_565 ?
Cu1 Cl1' Cu1 88.7(6) 25_665 27_565 ?
N2 N1 N1 109.2(5) . 28_655 ?
N2 N1 Cu1 127.5(6) . . ?
N1 N1 Cu1 123.1(2) 28_655 . ?
N1 N2 C1 108.0(6) . . ?
C1 C2 C3 122.6(4) . 28_655 ?
C1 C2 C3 122.6(4) . . ?
C3 C2 C3 114.7(7) 28_655 . ?
C1 C2 C2 178.2(6) . 18_655 ?
C3 C2 C2 57.4(3) 28_655 18_655 ?
C3 C2 C2 57.4(4) . 18_655 ?
C5 O1 Cu1 135.7(7) . . ?
C3 C4 C1 124.0(7) . 18_655 ?
C3 C4 H4 118.0 . . ?
C1 C4 H4 118.0 18_655 . ?
O1 C5 O1 127.9(11) 28_655 . ?
O1 C5 C1 116.0(5) 28_655 . ?
O1 C5 C1 116.0(5) . . ?
C2 C1 N2 127.2(3) . 28_655 ?
C2 C1 N2 127.2(3) . . ?
N2 C1 N2 105.6(6) 28_655 . ?
C2 C1 C5 176.6(9) . . ?
N2 C1 C5 52.8(3) 28_655 . ?
N2 C1 C5 52.8(3) . . ?
C2 C1 C4 56.1(4) . 18_655 ?
N2 C1 C4 71.1(4) 28_655 18_655 ?
N2 C1 C4 175.8(7) . 18_655 ?
C5 C1 C4 123.7(4) . 18_655 ?
C2 C1 C4 56.1(4) . 43 ?
N2 C1 C4 175.8(7) 28_655 43 ?
N2 C1 C4 71.1(4) . 43 ?
C5 C1 C4 123.7(4) . 43 ?
C4 C1 C4 112.0(8) 18_655 43 ?
C4 C3 C4 174.8(16) . 43 ?
C4 C3 C2 57.3(5) . 18_655 ?
C4 C3 C2 122.5(7) 43 18_655 ?
C4 C3 C2 122.5(7) . . ?
C4 C3 C2 57.3(5) 43 . ?
C2 C3 C2 65.3(7) 18_655 . ?
C4 C3 H3 90.1 . . ?
C4 C3 H3 90.1 43 . ?
C2 C3 H3 147.4 18_655 . ?
C2 C3 H3 147.4 . . ?
O2' O2 O2' 84.6 26 . ?
O2' O2 O2' 83.9 26 13 ?
O2' O2 O2' 143.1 . 13 ?
O2' O2 O2' 143.1 26 38 ?
O2' O2 O2' 83.9 . 38 ?
O2' O2 O2' 84.6 13 38 ?
O2' O2 Cu1 108.447(1) 26 . ?
O2' O2 Cu1 108.4 . . ?
O2' O2 Cu1 108.4 13 . ?
O2' O2 Cu1 108.446(1) 38 . ?
O2 O2' O2' 48.0 . 38 ?
O2 O2' O2' 47.7 . 26 ?
O2' O2' O2' 90.0 38 26 ?
O2 O2' O2' 18.4 . 13 ?
O2' O2' O2' 45.2 38 13 ?
O2' O2' O2' 44.8 26 13 ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        27.43
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.870
_refine_diff_density_min         -3.468
_refine_diff_density_rms         0.115

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 -0.010 -0.005 -0.005 5735.0 447.7
_database_code_depnum_ccdc_archive 'CCDC 947595'