# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  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.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_ZJU-7

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         Cu2(C26H12O8)2H2O,2(C3H7NO),3(C2H3N),4(H2O)
_chemical_formula_sum            'C38 H47 Cu2 N5 O16'
_chemical_formula_weight         956.90

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'
Cu Cu 0.3201 1.2651 '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'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   R-3m

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'

_cell_length_a                   18.6843(7)
_cell_length_b                   18.6843(7)
_cell_length_c                   38.6052(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     11671.6(7)
_cell_formula_units_Z            9
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    39425
_cell_measurement_theta_min      1.36
_cell_measurement_theta_max      25.34

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.26
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4266
_exptl_absorpt_coefficient_mu    0.848
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.681
_exptl_absorpt_correction_T_max  0.800
_exptl_absorpt_process_details   sadabs

_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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            39425
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_av_sigmaI/netI    0.0218
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_theta_min         1.36
_diffrn_reflns_theta_max         25.34
_reflns_number_total             2626
_reflns_number_gt                2144
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_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. 
;

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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
_platon_squeeze_void_content
1 -0.045 -0.030 -0.006 6221 1476 ' '
_platon_squeeze_details          
;
around 2.0 DMF, 3.0 MeCN and 4.0 H₂O disordered lattice molecules were removed from the 
formula unit by the SQUEEZE process
;

_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)+(0.0913P)²+15.6589P] 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         2626
_refine_ls_number_parameters     118
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0466
_refine_ls_wR_factor_ref         0.1450
_refine_ls_wR_factor_gt          0.1380
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.057
_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 0.856781(13) 0.143219(13) 0.138424(11) 0.0348(2) Uani 1 2 d S . .
O1 O 0.96190(13) 0.18490(14) 0.16312(5) 0.0517(6) Uani 1 1 d . . .
O2 O 0.92264(14) 0.22492(16) 0.21064(6) 0.0564(6) Uani 1 1 d . . .
O3 O 0.89202(18) 0.10798(18) 0.09151(13) 0.120(2) Uani 1 2 d S . .
H3A H 0.8852 0.1148 0.0703 0.144 Uiso 1 2 d S . .
H3B H 0.9177 0.0823 0.0962 0.144 Uiso 1 2 d S . .
C1 C 0.9731(2) 0.2139(2) 0.19338(8) 0.0462(7) Uani 1 1 d . . .
C2 C 1.10996(15) 0.2199(3) 0.19394(11) 0.0487(10) Uani 1 2 d S . .
H2A H 1.1001 0.2001 0.1713 0.058 Uiso 1 2 calc SR . .
C3 C 1.0530(2) 0.2345(2) 0.21053(8) 0.0514(8) Uani 1 1 d . . .
C4 C 1.0680(2) 0.2645(3) 0.24441(10) 0.0724(12) Uani 1 1 d . . .
H4A H 1.0300 0.2748 0.2556 0.087 Uiso 1 1 calc R . .
C5 C 1.1395(2) 0.2790(5) 0.26151(15) 0.089(2) Uani 1 2 d S . .
C6 C 1.1535(3) 0.3071(6) 0.29884(18) 0.109(3) Uani 1 2 d S . .
C7 C 1.0974(5) 0.2521(7) 0.32573(18) 0.135(6) Uani 0.50 1 d PG . .
C8 C 1.0332(8) 0.1742(8) 0.3167(3) 0.164(16) Uani 0.25 1 d PG . .
H8A H 1.0214 0.1559 0.2929 0.196 Uiso 0.25 1 d P . .
C9 C 0.9834(9) 0.1197(7) 0.3424(4) 0.188(16) Uani 0.25 1 d PG . .
H9A H 0.9401 0.0599 0.3366 0.225 Uiso 0.50 2 d SP . .
C10 C 0.9979(11) 0.1432(8) 0.3770(4) 0.190(17) Uani 0.25 1 d PG . .
H10A H 0.9655 0.1028 0.3950 0.228 Uiso 0.25 1 d P . .
C11 C 1.0621(9) 0.2210(9) 0.38597(19) 0.128(10) Uani 0.25 1 d PG . .
H11A H 1.0721 0.2369 0.4098 0.154 Uiso 0.25 1 d P . .
C12 C 1.1119(5) 0.2755(6) 0.3603(2) 0.144(7) Uani 0.50 1 d PG . .

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 0.0450(3) 0.0450(3) 0.0270(3) -0.00101(9) 0.00101(9) 0.0320(2)
O1 0.0471(13) 0.0732(15) 0.0432(12) -0.0112(11) -0.0081(10) 0.0364(11)
O2 0.0517(13) 0.0833(17) 0.0499(12) -0.0166(12) -0.0114(11) 0.0457(13)
O3 0.136(3) 0.136(3) 0.088(3) -0.0405(16) 0.0405(16) 0.068(4)
C1 0.0482(18) 0.0558(19) 0.0454(17) -0.0031(14) -0.0038(14) 0.0340(16)
C2 0.0493(18) 0.063(3) 0.038(2) -0.007(2) -0.0033(10) 0.0315(14)
C3 0.0481(18) 0.069(2) 0.0451(17) -0.0108(15) -0.0094(14) 0.0358(17)
C4 0.062(2) 0.121(4) 0.059(2) -0.035(2) -0.0159(18) 0.065(3)
C5 0.074(2) 0.164(7) 0.058(3) -0.054(4) -0.0268(19) 0.082(3)
C6 0.082(3) 0.218(9) 0.073(4) -0.081(6) -0.040(3) 0.109(5)
C7 0.083(7) 0.256(17) 0.085(7) -0.101(9) -0.037(6) 0.100(9)
C8 0.22(4) 0.31(5) 0.051(11) -0.01(2) 0.006(17) 0.20(4)
C9 0.22(3) 0.16(3) 0.21(3) -0.15(3) -0.11(3) 0.12(3)
C10 0.18(3) 0.18(3) 0.12(2) -0.03(2) 0.06(2) 0.02(2)
C11 0.14(2) 0.16(2) 0.080(13) -0.091(15) -0.022(13) 0.072(18)
C12 0.097(8) 0.287(19) 0.084(7) -0.097(10) -0.035(6) 0.124(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 O1 1.960(2) . ?
Cu1 O1 1.960(2) 22_665 ?
Cu1 O2 1.965(2) 25_655 ?
Cu1 O2 1.965(2) 10_545 ?
Cu1 O3 2.140(4) . ?
Cu1 Cu1 2.6569(8) 25_655 ?
O1 C1 1.261(4) . ?
O2 C1 1.252(4) . ?
O2 Cu1 1.965(2) 25_655 ?
C1 C3 1.498(4) . ?
C2 C3 1.380(4) . ?
C2 C3 1.380(4) 23_755 ?
C3 C4 1.395(5) . ?
C4 C5 1.389(4) . ?
C5 C4 1.389(4) 23_755 ?
C5 C6 1.511(8) . ?
C6 C7 1.468(13) . ?
C6 C7 1.468(13) 23_755 ?
C6 C12 1.473(19) 17 ?
C6 C12 1.473(18) 31_755 ?
C7 C7 1.069(17) 23_755 ?
C7 C8 1.3900 . ?
C7 C12 1.3900 . ?
C7 C12 1.722(10) 23_755 ?
C7 C8 2.02(2) 23_755 ?
C8 C9 1.3900 . ?
C8 C8 2.01(3) 23_755 ?
C8 C7 2.021(14) 23_755 ?
C9 C10 1.3900 . ?
C9 C9 1.93(2) 22_665 ?
C10 C11 1.3900 . ?
C11 C12 1.3900 . ?
C11 C11 1.81(3) 23_755 ?
C11 C12 1.918(12) 23_755 ?
C12 C12 0.966(17) 23_755 ?
C12 C6 1.473(12) 31_755 ?
C12 C7 1.722(8) 23_755 ?
C12 C11 1.92(2) 23_755 ?

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 88.78(14) . 22_665 ?
O1 Cu1 O2 167.76(9) . 25_655 ?
O1 Cu1 O2 89.75(11) 22_665 25_655 ?
O1 Cu1 O2 89.75(11) . 10_545 ?
O1 Cu1 O2 167.76(9) 22_665 10_545 ?
O2 Cu1 O2 89.12(16) 25_655 10_545 ?
O1 Cu1 O3 97.62(14) . . ?
O1 Cu1 O3 97.62(14) 22_665 . ?
O2 Cu1 O3 94.62(14) 25_655 . ?
O2 Cu1 O3 94.63(14) 10_545 . ?
O1 Cu1 Cu1 84.26(6) . 25_655 ?
O1 Cu1 Cu1 84.26(6) 22_665 25_655 ?
O2 Cu1 Cu1 83.50(6) 25_655 25_655 ?
O2 Cu1 Cu1 83.50(6) 10_545 25_655 ?
O3 Cu1 Cu1 177.36(18) . 25_655 ?
C1 O1 Cu1 122.6(2) . . ?
C1 O2 Cu1 123.5(2) . 25_655 ?
O2 C1 O1 126.0(3) . . ?
O2 C1 C3 117.3(3) . . ?
O1 C1 C3 116.7(3) . . ?
C3 C2 C3 120.7(4) . 23_755 ?
C2 C3 C4 119.6(3) . . ?
C2 C3 C1 120.8(3) . . ?
C4 C3 C1 119.4(3) . . ?
C5 C4 C3 120.3(3) . . ?
C4 C5 C4 119.4(5) . 23_755 ?
C4 C5 C6 120.3(2) . . ?
C4 C5 C6 120.3(2) 23_755 . ?
C7 C6 C7 42.7(8) . 23_755 ?
C7 C6 C12 107.6(10) . 17 ?
C7 C6 C12 122.7(7) 23_755 17 ?
C7 C6 C12 122.7(7) . 31_755 ?
C7 C6 C12 107.6(12) 23_755 31_755 ?
C12 C6 C12 38(2) 17 31_755 ?
C7 C6 C5 119.5(8) . . ?
C7 C6 C5 119.5(8) 23_755 . ?
C12 C6 C5 117.7(10) 17 . ?
C12 C6 C5 117.7(10) 31_755 . ?
C7 C7 C8 109.9(5) 23_755 . ?
C7 C7 C12 87.9(4) 23_755 . ?
C8 C7 C12 120.0 . . ?
C7 C7 C6 68.6(4) 23_755 . ?
C8 C7 C6 119.8(7) . . ?
C12 C7 C6 120.1(7) . . ?
C7 C7 C12 53.8(4) 23_755 23_755 ?
C8 C7 C12 126.5 . 23_755 ?
C12 C7 C12 34.1(5) . 23_755 ?
C6 C7 C12 101.6(8) . 23_755 ?
C7 C7 C8 40.3(3) 23_755 23_755 ?
C8 C7 C8 69.6(5) . 23_755 ?
C12 C7 C8 107.9(2) . 23_755 ?
C6 C7 C8 88.8(9) . 23_755 ?
C12 C7 C8 79.6(4) 23_755 23_755 ?
C7 C8 C9 120.0 . . ?
C7 C8 C8 70.1 . 23_755 ?
C9 C8 C8 107.6 . 23_755 ?
C7 C8 C7 29.8(4) . 23_755 ?
C9 C8 C7 120.3(3) . 23_755 ?
C8 C8 C7 40.3(4) 23_755 23_755 ?
C8 C9 C10 120.0 . . ?
C8 C9 C9 134.5 . 22_665 ?
C10 C9 C9 104.8 . 22_665 ?
C11 C10 C9 120.0 . . ?
C10 C11 C12 120.0 . . ?
C10 C11 C11 109.9 . 23_755 ?
C12 C11 C11 72.4 . 23_755 ?
C10 C11 C12 122.2 . 23_755 ?
C12 C11 C12 28.7(4) . 23_755 ?
C11 C11 C12 43.7(3) 23_755 23_755 ?
C12 C12 C11 107.6 23_755 . ?
C12 C12 C7 92.1 23_755 . ?
C11 C12 C7 120.0 . . ?
C12 C12 C6 70.9(8) 23_755 31_755 ?
C11 C12 C6 123.1(7) . 31_755 ?
C7 C12 C6 116.9(7) . 31_755 ?
C12 C12 C7 53.8(6) 23_755 23_755 ?
C11 C12 C7 126.3(4) . 23_755 ?
C7 C12 C7 38.3(6) . 23_755 ?
C6 C12 C7 99.3(6) 31_755 23_755 ?
C12 C12 C11 43.7(6) 23_755 23_755 ?
C11 C12 C11 63.9(6) . 23_755 ?
C7 C12 C11 113.4(3) . 23_755 ?
C6 C12 C11 95.0(10) 31_755 23_755 ?
C7 C12 C11 82.6(4) 23_755 23_755 ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.34
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.897
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.075
_database_code_depnum_ccdc_archive 'CCDC 1013769'
