# Electronic Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2012


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#                 Cambridge Crystallographic Data Centre
#                                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 
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#  except for the purpose of generating routine backup copies 
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data_c
_database_code_depnum_ccdc_archive 'CCDC 891188'
#TrackingRef 'Shengqun_Su_1.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C12 H28 Cu3 N6 O17'
_chemical_formula_sum            'C12 H28 Cu3 N6 O17'
_chemical_formula_weight         719.02

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'
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   F-43c

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

_cell_length_a                   30.1702(11)
_cell_length_b                   30.1702(11)
_cell_length_c                   30.1702(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     27462.2(17)
_cell_formula_units_Z            32
_cell_measurement_temperature    185(2)
_cell_measurement_reflns_used    2301
_cell_measurement_theta_min      1.35
_cell_measurement_theta_max      26.11

_exptl_crystal_description       block
_exptl_crystal_colour            dark-blue
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             11680
_exptl_absorpt_coefficient_mu    1.907
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6173
_exptl_absorpt_correction_T_max  0.6791
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      185(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 9.00cm
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            35260
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_av_sigmaI/netI    0.0228
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         1.35
_diffrn_reflns_theta_max         26.11
_reflns_number_total             2301
_reflns_number_gt                2168
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXP-97
_computing_publication_material  SHELXTL

_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^)+(0.1507P)^2^+60.7942P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.05(5)
_refine_ls_number_reflns         2301
_refine_ls_number_parameters     95
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0638
_refine_ls_wR_factor_ref         0.2010
_refine_ls_wR_factor_gt          0.1940
_refine_ls_goodness_of_fit_ref   1.162
_refine_ls_restrained_S_all      1.176
_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 0.38747(3) 0.42595(3) 0.16422(3) 0.0498(4) Uani 1 1 d . . .
C1 C 0.3693(3) 0.4655(3) 0.2449(3) 0.063(2) Uani 1 1 d . . .
C2 C 0.3732(3) 0.5005(3) 0.2784(3) 0.0521(19) Uani 1 1 d . A .
C3 C 0.4025(3) 0.5357(3) 0.2780(3) 0.054(2) Uani 1 1 d . . .
H3A H 0.4244 0.5411 0.2561 0.065 Uiso 1 1 calc R A .
C4 C 0.3478(3) 0.5067(3) 0.3158(2) 0.051(2) Uani 1 1 d . . .
H4A H 0.3243 0.4878 0.3249 0.061 Uiso 1 1 calc R A .
N1 N 0.3949(2) 0.5611(2) 0.3139(2) 0.0507(18) Uani 1 1 d . A .
N2 N 0.3608(2) 0.5428(2) 0.3373(2) 0.0489(16) Uani 1 1 d . A .
O1 O 0.39452(18) 0.4708(2) 0.21011(18) 0.0572(16) Uani 1 1 d . A .
O2 O 0.3420(3) 0.4350(2) 0.2496(2) 0.086(3) Uani 1 1 d U A .
O3 O 0.3717(4) 0.3717(4) 0.1283(4) 0.042(3) Uani 0.50 3 d SP A 1
O3' O 0.3929(4) 0.3929(4) 0.1071(4) 0.042(3) Uani 0.50 3 d SP A 2
O4 O 0.2938(3) 0.3743(3) 0.2617(3) 0.085(2) 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 0.0484(5) 0.0550(6) 0.0460(5) -0.0410(4) -0.0323(4) 0.0352(4)
C1 0.088(6) 0.049(4) 0.052(5) -0.036(4) -0.022(5) 0.003(4)
C2 0.061(4) 0.044(4) 0.052(4) -0.034(4) 0.000(4) -0.007(3)
C3 0.058(4) 0.060(5) 0.044(4) -0.035(4) 0.019(3) -0.016(4)
C4 0.064(5) 0.043(4) 0.046(4) -0.024(3) 0.011(3) -0.030(4)
N1 0.058(4) 0.052(3) 0.042(3) -0.031(3) 0.024(3) -0.025(3)
N2 0.058(4) 0.043(3) 0.045(3) -0.029(3) 0.021(3) -0.033(3)
O1 0.052(3) 0.070(4) 0.049(3) -0.044(3) -0.015(2) 0.021(3)
O2 0.135(6) 0.054(4) 0.069(4) -0.036(3) 0.003(4) -0.032(4)
O3 0.042(3) 0.042(3) 0.042(3) -0.034(4) -0.034(4) 0.034(4)
O3' 0.042(3) 0.042(3) 0.042(3) -0.034(4) -0.034(4) 0.034(4)
O4 0.077(5) 0.076(5) 0.101(6) 0.014(4) 0.006(4) -0.009(4)

_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 1.930(6) 88_545 ?
Cu1 N2 1.936(6) 94_455 ?
Cu1 O1 1.947(5) . ?
Cu1 O3' 1.998(6) . ?
Cu1 O3 2.019(6) . ?
C1 O2 1.242(12) . ?
C1 O1 1.308(12) . ?
C1 C2 1.468(9) . ?
C2 C4 1.375(11) . ?
C2 C3 1.382(12) . ?
C3 N1 1.345(9) . ?
C4 N2 1.329(8) . ?
N1 N2 1.363(8) . ?
N1 Cu1 1.930(6) 87_455 ?
N2 Cu1 1.936(6) 48_554 ?
O3 Cu1 2.019(6) 56 ?
O3 Cu1 2.019(6) 35 ?
O3' Cu1 1.998(6) 56 ?
O3' Cu1 1.998(6) 35 ?

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 N2 177.0(3) 88_545 94_455 ?
N1 Cu1 O1 90.3(2) 88_545 . ?
N2 Cu1 O1 91.4(2) 94_455 . ?
N1 Cu1 O3' 89.24(16) 88_545 . ?
N2 Cu1 O3' 88.31(17) 94_455 . ?
O1 Cu1 O3' 162.0(6) . . ?
N1 Cu1 O3 88.82(18) 88_545 . ?
N2 Cu1 O3 90.04(17) 94_455 . ?
O1 Cu1 O3 166.0(6) . . ?
O3' Cu1 O3 32.0(7) . . ?
O2 C1 O1 124.6(7) . . ?
O2 C1 C2 120.6(9) . . ?
O1 C1 C2 114.7(8) . . ?
C4 C2 C3 105.1(6) . . ?
C4 C2 C1 128.0(8) . . ?
C3 C2 C1 126.9(8) . . ?
N1 C3 C2 108.7(7) . . ?
N2 C4 C2 110.2(6) . . ?
C3 N1 N2 108.4(6) . . ?
C3 N1 Cu1 130.5(5) . 87_455 ?
N2 N1 Cu1 120.9(4) . 87_455 ?
C4 N2 N1 107.6(5) . . ?
C4 N2 Cu1 131.8(5) . 48_554 ?
N1 N2 Cu1 120.2(4) . 48_554 ?
C1 O1 Cu1 115.0(5) . . ?
Cu1 O3 Cu1 111.8(5) 56 . ?
Cu1 O3 Cu1 111.8(5) 56 35 ?
Cu1 O3 Cu1 111.8(5) . 35 ?
Cu1 O3' Cu1 113.6(5) 56 . ?
Cu1 O3' Cu1 113.6(5) 56 35 ?
Cu1 O3' Cu1 113.6(5) . 35 ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        26.11
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.204
_refine_diff_density_min         -0.643
_refine_diff_density_rms         0.234