# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_ZJNU-10
_database_code_depnum_ccdc_archive 'CCDC 1954395'
loop_
_audit_author_name
_audit_author_address
'Yabing He' 'Zhejiang Normal University'
_audit_update_record             
;
2019-10-06 deposited with the CCDC.	2019-10-29 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         '[C40H26Cu4O20].4DMF.2H2O'
_chemical_formula_sum            'C52 H58 Cu4 N4 O26'
_chemical_formula_weight         1409.18

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'
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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           139
_space_group_name_H-M_alt        'I 4/m m m'
_space_group_name_Hall           '-I 4 2'

_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, -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                   19.0416(10)
_cell_length_b                   19.0416(10)
_cell_length_c                   18.6430(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6759.6(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    1655
_cell_measurement_theta_min      2.629
_cell_measurement_theta_max      26.36

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_F_000             2168
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    1.318
_shelx_estimated_absorpt_T_min   0.797
_shelx_estimated_absorpt_T_max   0.879
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.827
_exptl_absorpt_correction_T_max  0.877
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON II'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9413
_diffrn_reflns_av_unetI/netI     0.0484
_diffrn_reflns_av_R_equivalents  0.0658
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.185
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             1979
_reflns_number_gt                1333
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0810P)²+4.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1979
_refine_ls_number_parameters     86
_refine_ls_number_restraints     37
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0488
_refine_ls_wR_factor_ref         0.1553
_refine_ls_wR_factor_gt          0.1394
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.002
_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
Cu1 Cu 0.71665(2) 0.71665(2) 0.30247(3) 0.0361(3) Uani 1 2 d S T P . .
O1 O 0.76724(15) 0.86960(14) 0.25329(14) 0.0488(7) Uani 1 1 d . . . . .
O2 O 0.70917(14) 0.81317(14) 0.33987(14) 0.0475(7) Uani 1 1 d . . . . .
O3 O 0.66548(19) 0.66548(19) 0.3935(3) 0.0819(16) Uani 1 2 d S T P . .
C1 C 0.7305(2) 0.8672(2) 0.3093(2) 0.0396(9) Uani 1 1 d . . . . .
C2 C 0.7095(2) 0.9370(2) 0.34183(19) 0.0387(9) Uani 1 1 d . U . . .
C3 C 0.7339(3) 1.0000 0.3145(3) 0.0421(13) Uani 1 2 d S TU P . .
H3 H 0.7689 1.0000 0.2781 0.050 Uiso 1 2 d R U P . .
C4 C 0.65694(19) 0.9374(2) 0.39395(18) 0.0372(8) Uani 1 1 d . U . . .
H4 H 0.6392 0.8944 0.4122 0.045 Uiso 1 1 d R U . . .
C5 C 0.6298(3) 1.0000 0.4194(2) 0.0321(11) Uani 1 2 d S TU P . .
C6 C 0.5628(3) 1.0000 0.4623(2) 0.0287(10) Uani 1 2 d S TU P . .
C7 C 0.5000 1.0000 0.4251(3) 0.0267(13) Uani 1 4 d DS TU P . .
C8 C 0.5000 1.0090(14) 0.3432(4) 0.034(4) Uani 0.5 2 d DS TU P . .
H8A H 0.4526 1.0075 0.3257 0.051 Uiso 0.25 1 d R U P . .
H8B H 0.5206 1.0535 0.3315 0.051 Uiso 0.25 1 d R U P . .
H8C H 0.5267 0.9720 0.3212 0.051 Uiso 0.25 1 d R U P . .


_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 O2 1.971(3) 24 ?
Cu1 O2 1.971(3) . ?
Cu1 O1 1.968(3) 16_665 ?
Cu1 O1 1.968(3) 25_665 ?
Cu1 O3 2.186(4) . ?
Cu1 Cu1 2.6557(12) 25_665 ?
O1 C1 1.258(4) . ?
O1 Cu1 1.968(3) 25_665 ?
O2 C1 1.244(5) . ?
C1 C2 1.515(5) . ?
C2 C3 1.384(5) . ?
C2 C4 1.394(5) . ?
C3 C2 1.384(5) 21_575 ?
C3 H3 0.9499 . ?
C4 C5 1.383(4) . ?
C4 H4 0.9499 . ?
C5 C4 1.383(4) 21_575 ?
C5 C6 1.504(6) . ?
C6 C6 1.406(8) 18_556 ?
C6 C7 1.383(5) . ?
C7 C6 1.383(5) 2_675 ?
C7 C8 1.538(9) 2_675 ?
C7 C8 1.538(9) . ?
C8 C8 0.34(5) 2_675 ?
C8 H8A 0.9599 . ?
C8 H8B 0.9599 . ?
C8 H8C 0.9600 . ?

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
O2 Cu1 O2 90.56(16) 24 . ?
O2 Cu1 O1 167.55(11) 24 16_665 ?
O2 Cu1 O1 88.92(12) . 16_665 ?
O2 Cu1 O1 88.93(12) 24 25_665 ?
O2 Cu1 O1 167.55(11) . 25_665 ?
O1 Cu1 O1 88.91(17) 16_665 25_665 ?
O2 Cu1 O3 96.24(13) 24 . ?
O2 Cu1 O3 96.24(13) . . ?
O1 Cu1 O3 96.18(13) 16_665 . ?
O1 Cu1 O3 96.18(13) 25_665 . ?
O2 Cu1 Cu1 81.33(8) 24 25_665 ?
O2 Cu1 Cu1 81.33(8) . 25_665 ?
O1 Cu1 Cu1 86.30(8) 16_665 25_665 ?
O1 Cu1 Cu1 86.30(8) 25_665 25_665 ?
O3 Cu1 Cu1 176.51(16) . 25_665 ?
C1 O1 Cu1 119.6(3) . 25_665 ?
C1 O2 Cu1 125.8(2) . . ?
O2 C1 O1 126.3(4) . . ?
O2 C1 C2 117.1(3) . . ?
O1 C1 C2 116.6(3) . . ?
C3 C2 C4 119.5(4) . . ?
C3 C2 C1 121.6(3) . . ?
C4 C2 C1 118.3(3) . . ?
C2 C3 C2 120.1(5) 21_575 . ?
C2 C3 H3 119.9 21_575 . ?
C2 C3 H3 119.9 . . ?
C5 C4 C2 120.8(4) . . ?
C5 C4 H4 119.2 . . ?
C2 C4 H4 119.9 . . ?
C4 C5 C4 119.0(5) . 21_575 ?
C4 C5 C6 120.0(2) . . ?
C4 C5 C6 120.0(2) 21_575 . ?
C6 C6 C7 120.1(3) 18_556 . ?
C6 C6 C5 122.1(2) 18_556 . ?
C7 C6 C5 117.8(4) . . ?
C6 C7 C6 119.9(5) . 2_675 ?
C6 C7 C8 119.9(3) . 2_675 ?
C6 C7 C8 119.9(3) 2_675 2_675 ?
C6 C7 C8 119.9(3) . . ?
C6 C7 C8 119.9(3) 2_675 . ?
C8 C7 C8 13(2) 2_675 . ?
C8 C8 C7 83.6(10) 2_675 . ?
C8 C8 H8A 88.4 2_675 . ?
C7 C8 H8A 109.5 . . ?
C8 C8 H8B 152.1 2_675 . ?
C7 C8 H8B 108.9 . . ?
H8A C8 H8B 109.5 . . ?
C8 C8 H8C 42.9 2_675 . ?
C7 C8 H8C 110.0 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?

_refine_diff_density_max         0.861
_refine_diff_density_min         -0.631
_refine_diff_density_rms         0.082



