# Electronic Supplementary Material (ESI) for CrystEngComm.
# 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-101
_database_code_depnum_ccdc_archive 'CCDC 1895248'
loop_
_audit_author_name
_audit_author_address
'Yabing He'
;Zhejiang Normal University
China
;
_audit_update_record             
;
2019-09-16 deposited with the CCDC.	2019-09-20 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         '[C22H14Cu2O10].6DMF.H2O'
_chemical_formula_sum            'C40 H58 Cu2 N6 O17'
_chemical_formula_weight         1022.00

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

_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_H-M_alt        'C m c 21'
_space_group_name_Hall           'C 2c -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+1/2'
'x, -y, z+1/2'
'-x, y, z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z'

_cell_length_a                   24.9038(10)
_cell_length_b                   33.4493(12)
_cell_length_c                   18.3388(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     15276.5(10)
_cell_formula_units_Z            12
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    30585
_cell_measurement_theta_min      0.96
_cell_measurement_theta_max      74.0

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_F_000             6408
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.160
_exptl_absorpt_coefficient_mu    1.632
_shelx_estimated_absorpt_T_min   0.686
_shelx_estimated_absorpt_T_max   0.780
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.767
_exptl_absorpt_correction_T_max  0.818
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\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            30571
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.212
_diffrn_reflns_theta_max         66.489
_diffrn_reflns_theta_full        66.489
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measured_fraction_theta_full 0.961
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_Laue_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_point_group_measured_fraction_full 0.964
_reflns_number_total             11714
_reflns_number_gt                11082
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.940
_reflns_Friedel_fraction_max     0.968
_reflns_Friedel_fraction_full    0.968

_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          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.26(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         11714
_refine_ls_number_parameters     466
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0447
_refine_ls_wR_factor_ref         0.1285
_refine_ls_wR_factor_gt          0.1253
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_restrained_S_all      1.004
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.000
_refine_ls_platon_squeeze_details 
;
The solvent molecules were highly disordered, and thus their locations
cannot be precisely determined. To address this issue, electron density 
peaks of solvent molecules were removed by the PLATON/SQUEEZE procedure,
therefore producing a set of solvent-free diffraction intensities for 
further structural refinement.
;
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 0.20319(3) 0.73918(2) 0.62048(3) 0.03264(16) Uani 1 1 d . . . . .
Cu2 Cu 0.28150(3) 0.77407(2) 0.54545(3) 0.03229(16) Uani 1 1 d . . . . .
Cu3 Cu 0.5000 0.63985(2) 0.34453(5) 0.0362(2) Uani 1 2 d S T P . .
Cu4 Cu 0.5000 0.43890(2) 0.85355(5) 0.0344(2) Uani 1 2 d S T P . .
O1 O 0.24502(15) 0.69086(8) 0.6004(2) 0.0485(9) Uani 1 1 d . . . . .
O2 O 0.31089(15) 0.71983(8) 0.5370(2) 0.0497(9) Uani 1 1 d . . . . .
O3 O 0.44482(19) 0.63800(9) 0.4189(3) 0.0671(12) Uani 1 1 d . . . . .
O4 O 0.44329(15) 0.57163(9) 0.42660(19) 0.0452(8) Uani 1 1 d . . . . .
O5 O 0.44379(14) 0.43637(8) 0.77663(19) 0.0428(8) Uani 1 1 d . . . . .
O6 O 0.4449(2) 0.36955(10) 0.7721(3) 0.0747(14) Uani 1 1 d . . . . .
O7 O 0.32481(15) 0.29401(9) 0.6290(2) 0.0482(8) Uani 1 1 d . . . . .
O8 O 0.25815(17) 0.32295(9) 0.5668(2) 0.0538(10) Uani 1 1 d . . . . .
O9 O 0.16820(16) 0.73277(10) 0.52512(17) 0.0471(8) Uani 1 1 d . . . . .
O10 O 0.23480(17) 0.76257(10) 0.46339(18) 0.0489(9) Uani 1 1 d . . . . .
O11 O 0.24966(17) 0.74965(11) 0.20376(18) 0.0494(8) Uani 1 1 d . . . . .
O12 O 0.18305(18) 0.72098(11) 0.14073(19) 0.0542(9) Uani 1 1 d . . . . .
O1W O 0.1421(2) 0.7092(2) 0.6815(3) 0.109(2) Uani 1 1 d . . . . .
O2W O 0.3435(2) 0.80873(18) 0.4924(3) 0.102(2) Uani 1 1 d . . . . .
O3W O 0.5000 0.70383(15) 0.3334(4) 0.0885(16) Uani 1 2 d S T P . .
O4W O 0.5000 0.50239(15) 0.8646(4) 0.0885(16) Uani 1 2 d S T P . .
C1 C 0.2752(2) 0.54121(15) 0.5795(3) 0.0464(12) Uani 1 1 d . . . . .
C2 C 0.3032(2) 0.50686(12) 0.5986(3) 0.0410(11) Uani 1 1 d . . . . .
H2A H 0.3413 0.5075 0.5975 0.049 Uiso 1 1 calc R U . . .
C3 C 0.2779(2) 0.47168(13) 0.6192(3) 0.0429(11) Uani 1 1 d . . . . .
C4 C 0.2211(2) 0.47157(15) 0.6188(4) 0.0571(14) Uani 1 1 d . . . . .
H4A H 0.2022 0.4478 0.6311 0.069 Uiso 1 1 calc R U . . .
C5 C 0.1935(2) 0.50505(17) 0.6012(4) 0.0632(17) Uani 1 1 d . . . . .
H5A H 0.1554 0.5045 0.6028 0.076 Uiso 1 1 calc R U . . .
C6 C 0.2198(2) 0.54098(16) 0.5804(4) 0.0575(15) Uani 1 1 d . . . . .
H6A H 0.1998 0.5641 0.5674 0.069 Uiso 1 1 calc R U . . .
C7 C 0.3048(2) 0.57755(13) 0.5566(3) 0.0407(11) Uani 1 1 d . . . . .
C8 C 0.2852(2) 0.61558(14) 0.5729(3) 0.0448(12) Uani 1 1 d . . . . .
H8A H 0.2537 0.6182 0.6016 0.054 Uiso 1 1 calc R U . . .
C9 C 0.3110(2) 0.64960(11) 0.5479(3) 0.0376(9) Uani 1 1 d . . . . .
C10 C 0.3578(2) 0.64629(13) 0.5078(2) 0.0410(11) Uani 1 1 d . . . . .
H10A H 0.3759 0.6697 0.4916 0.049 Uiso 1 1 calc R U . . .
C11 C 0.3783(2) 0.60900(13) 0.4914(3) 0.0403(10) Uani 1 1 d . . . . .
C12 C 0.3525(2) 0.57525(13) 0.5164(3) 0.0430(11) Uani 1 1 d . . . . .
H12A H 0.3674 0.5497 0.5060 0.052 Uiso 1 1 calc R U . . .
C13 C 0.2864(2) 0.69101(13) 0.5631(2) 0.0400(11) Uani 1 1 d . . . . .
C14 C 0.4265(2) 0.60565(12) 0.4427(3) 0.0412(11) Uani 1 1 d . . . . .
C15 C 0.3078(2) 0.43558(13) 0.6378(3) 0.0426(11) Uani 1 1 d . . . . .
C16 C 0.3542(2) 0.43692(13) 0.6839(3) 0.0451(12) Uani 1 1 d . . . . .
H16A H 0.3666 0.4619 0.7018 0.054 Uiso 1 1 calc R U . . .
C17 C 0.3807(2) 0.40299(12) 0.7022(3) 0.0422(11) Uani 1 1 d . . . . .
C18 C 0.3647(2) 0.36623(12) 0.6744(3) 0.0442(11) Uani 1 1 d . . . . .
H18A H 0.3840 0.3427 0.6868 0.053 Uiso 1 1 calc R U . . .
C19 C 0.3200(2) 0.36394(13) 0.6281(3) 0.0437(11) Uani 1 1 d . . . . .
C20 C 0.2927(2) 0.39801(13) 0.6096(3) 0.0411(11) Uani 1 1 d . . . . .
H20A H 0.2630 0.3963 0.5772 0.049 Uiso 1 1 calc R U . . .
C21 C 0.4271(2) 0.40303(12) 0.7557(3) 0.0438(12) Uani 1 1 d . . . . .
C22 C 0.3005(2) 0.32330(14) 0.6055(2) 0.0413(11) Uani 1 1 d . . . . .
C23 C 0.1666(2) 0.73063(12) 0.3973(3) 0.0431(11) Uani 1 1 d . . . . .
C24 C 0.1947(2) 0.73849(13) 0.3334(3) 0.0408(11) Uani 1 1 d . . . . .
H24A H 0.2272 0.7534 0.3352 0.049 Uiso 1 1 calc R U . . .
C25 C 0.1753(2) 0.72455(13) 0.2660(3) 0.0410(11) Uani 1 1 d . . . . .
C26 C 0.1273(2) 0.70208(14) 0.2651(3) 0.0459(11) Uani 1 1 d . . . . .
H26A H 0.1135 0.6926 0.2200 0.055 Uiso 1 1 calc R U . . .
C27 C 0.1000(2) 0.69369(13) 0.3292(3) 0.0420(10) Uani 1 1 d . . . . .
C28 C 0.1194(2) 0.70847(13) 0.3947(2) 0.0425(11) Uani 1 1 d . . . . .
H28A H 0.1002 0.7034 0.4385 0.051 Uiso 1 1 calc R U . . .
C29 C 0.1913(2) 0.74284(13) 0.4684(2) 0.0411(11) Uani 1 1 d . . . . .
C30 C 0.2049(2) 0.73244(13) 0.1982(3) 0.0405(12) Uani 1 1 d . . . . .
C31 C 0.0492(2) 0.67150(14) 0.3222(3) 0.0470(12) Uani 1 1 d . . . . .
C32 C 0.0000 0.68966(19) 0.3394(3) 0.0419(15) Uani 1 2 d S T P . .
H32A H 0.0000 0.7149 0.3632 0.050 Uiso 1 2 calc R U P . .
C33 C 0.0486(3) 0.63410(19) 0.2872(3) 0.0646(16) Uani 1 1 d . . . . .
H33A H 0.0813 0.6212 0.2745 0.078 Uiso 1 1 calc R U . . .
C34 C 0.0000 0.6164(3) 0.2715(6) 0.073(3) Uani 1 2 d S T P . .
H34A H 0.0000 0.5908 0.2489 0.088 Uiso 1 2 calc 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 O1 1.958(3) . ?
Cu1 O9 1.966(3) . ?
Cu1 O11 1.963(4) 6_565 ?
Cu1 O7 1.969(3) 8 ?
Cu1 O1W 2.140(4) . ?
Cu1 Cu2 2.6570(8) . ?
Cu2 O10 1.941(4) . ?
Cu2 O8 1.950(3) 8 ?
Cu2 O12 1.965(4) 6_565 ?
Cu2 O2 1.962(3) . ?
Cu2 O2W 2.163(4) . ?
Cu3 O6 1.935(4) 3_564 ?
Cu3 O6 1.935(4) 2_664 ?
Cu3 O3 1.937(4) . ?
Cu3 O3 1.937(4) 4_655 ?
Cu3 O3W 2.150(5) . ?
Cu3 Cu4 2.6393(10) 2_664 ?
Cu4 O4 1.978(4) 2_665 ?
Cu4 O4 1.978(4) 3_565 ?
Cu4 O5 1.989(3) 4_655 ?
Cu4 O5 1.989(3) . ?
Cu4 O4W 2.133(5) . ?
Cu4 Cu3 2.6393(10) 2_665 ?
O1 C13 1.237(6) . ?
O2 C13 1.237(6) . ?
O3 C14 1.253(6) . ?
O4 C14 1.247(6) . ?
O4 Cu4 1.978(4) 2_664 ?
O5 C21 1.251(6) . ?
O6 C21 1.242(6) . ?
O6 Cu3 1.935(4) 2_665 ?
O7 C22 1.230(6) . ?
O7 Cu1 1.969(3) 8_545 ?
O8 C22 1.272(6) . ?
O8 Cu2 1.950(3) 8_545 ?
O9 C29 1.236(6) . ?
O10 C29 1.272(7) . ?
O11 C30 1.258(7) . ?
O11 Cu1 1.963(4) 6_564 ?
O12 C30 1.248(6) . ?
O12 Cu2 1.965(4) 6_564 ?
C1 C2 1.389(7) . ?
C1 C6 1.381(8) . ?
C1 C7 1.483(7) . ?
C2 C3 1.388(6) . ?
C2 H2A 0.9500 . ?
C3 C4 1.414(8) . ?
C3 C15 1.461(7) . ?
C4 C5 1.353(8) . ?
C4 H4A 0.9500 . ?
C5 C6 1.421(7) . ?
C5 H5A 0.9500 . ?
C6 H6A 0.9500 . ?
C7 C8 1.395(7) . ?
C7 C12 1.399(7) . ?
C8 C9 1.385(7) . ?
C8 H8A 0.9500 . ?
C9 C10 1.382(7) . ?
C9 C13 1.540(6) . ?
C10 C11 1.381(6) . ?
C10 H10A 0.9500 . ?
C11 C12 1.378(7) . ?
C11 C14 1.500(7) . ?
C12 H12A 0.9500 . ?
C15 C16 1.431(8) . ?
C15 C20 1.411(6) . ?
C16 C17 1.355(7) . ?
C16 H16A 0.9500 . ?
C17 C18 1.389(6) . ?
C17 C21 1.515(7) . ?
C18 C19 1.402(8) . ?
C18 H18A 0.9500 . ?
C19 C20 1.370(7) . ?
C19 C22 1.502(6) . ?
C20 H20A 0.9500 . ?
C23 C24 1.391(7) . ?
C23 C28 1.390(7) . ?
C23 C29 1.498(7) . ?
C24 C25 1.405(7) . ?
C24 H24A 0.9500 . ?
C25 C26 1.414(7) . ?
C25 C30 1.469(7) . ?
C26 C27 1.386(7) . ?
C26 H26A 0.9500 . ?
C27 C28 1.387(7) . ?
C27 C31 1.472(7) . ?
C28 H28A 0.9500 . ?
C31 C32 1.403(6) . ?
C31 C33 1.406(7) . ?
C32 C31 1.403(6) 4 ?
C32 H32A 0.9500 . ?
C33 C34 1.379(8) . ?
C33 H33A 0.9500 . ?
C34 C33 1.379(8) 4 ?
C34 H34A 0.9500 . ?

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 O9 88.76(16) . . ?
O1 Cu1 O11 89.16(17) . 6_565 ?
O9 Cu1 O11 168.08(16) . 6_565 ?
O1 Cu1 O7 166.57(15) . 8 ?
O9 Cu1 O7 90.89(16) . 8 ?
O11 Cu1 O7 88.42(16) 6_565 8 ?
O1 Cu1 O1W 95.1(2) . . ?
O9 Cu1 O1W 95.7(2) . . ?
O11 Cu1 O1W 96.2(2) 6_565 . ?
O7 Cu1 O1W 98.3(2) 8 . ?
O1 Cu1 Cu2 82.79(10) . . ?
O9 Cu1 Cu2 84.98(11) . . ?
O11 Cu1 Cu2 83.11(11) 6_565 . ?
O7 Cu1 Cu2 83.80(11) 8 . ?
O1W Cu1 Cu2 177.83(19) . . ?
O10 Cu2 O8 91.04(18) . 8 ?
O10 Cu2 O12 167.36(16) . 6_565 ?
O8 Cu2 O12 88.77(17) 8 6_565 ?
O10 Cu2 O2 88.80(17) . . ?
O8 Cu2 O2 168.52(15) 8 . ?
O12 Cu2 O2 88.89(17) 6_565 . ?
O10 Cu2 O2W 100.7(2) . . ?
O8 Cu2 O2W 90.1(2) 8 . ?
O12 Cu2 O2W 91.9(2) 6_565 . ?
O2 Cu2 O2W 101.2(2) . . ?
O10 Cu2 Cu1 82.79(11) . . ?
O8 Cu2 Cu1 83.84(11) 8 . ?
O12 Cu2 Cu1 84.62(12) 6_565 . ?
O2 Cu2 Cu1 84.75(11) . . ?
O2W Cu2 Cu1 173.1(2) . . ?
O6 Cu3 O6 90.2(4) 3_564 2_664 ?
O6 Cu3 O3 88.6(2) 3_564 . ?
O6 Cu3 O3 168.80(14) 2_664 . ?
O6 Cu3 O3 168.79(14) 3_564 4_655 ?
O6 Cu3 O3 88.6(2) 2_664 4_655 ?
O3 Cu3 O3 90.4(3) . 4_655 ?
O6 Cu3 O3W 95.54(17) 3_564 . ?
O6 Cu3 O3W 95.54(17) 2_664 . ?
O3 Cu3 O3W 95.66(16) . . ?
O3 Cu3 O3W 95.67(16) 4_655 . ?
O6 Cu3 Cu4 83.15(10) 3_564 2_664 ?
O6 Cu3 Cu4 83.15(10) 2_664 2_664 ?
O3 Cu3 Cu4 85.64(9) . 2_664 ?
O3 Cu3 Cu4 85.64(9) 4_655 2_664 ?
O3W Cu3 Cu4 178.14(19) . 2_664 ?
O4 Cu4 O4 91.1(2) 2_665 3_565 ?
O4 Cu4 O5 88.30(14) 2_665 4_655 ?
O4 Cu4 O5 167.19(12) 3_565 4_655 ?
O4 Cu4 O5 167.19(12) 2_665 . ?
O4 Cu4 O5 88.29(14) 3_565 . ?
O5 Cu4 O5 89.5(2) 4_655 . ?
O4 Cu4 O4W 96.49(17) 2_665 . ?
O4 Cu4 O4W 96.49(17) 3_565 . ?
O5 Cu4 O4W 96.29(16) 4_655 . ?
O5 Cu4 O4W 96.29(16) . . ?
O4 Cu4 Cu3 82.23(9) 2_665 2_665 ?
O4 Cu4 Cu3 82.23(9) 3_565 2_665 ?
O5 Cu4 Cu3 85.02(8) 4_655 2_665 ?
O5 Cu4 Cu3 85.02(8) . 2_665 ?
O4W Cu4 Cu3 178.2(2) . 2_665 ?
C13 O1 Cu1 123.0(3) . . ?
C13 O2 Cu2 120.4(3) . . ?
C14 O3 Cu3 122.1(3) . . ?
C14 O4 Cu4 124.2(3) . 2_664 ?
C21 O5 Cu4 119.3(3) . . ?
C21 O6 Cu3 124.5(3) . 2_665 ?
C22 O7 Cu1 122.7(3) . 8_545 ?
C22 O8 Cu2 122.7(3) . 8_545 ?
C29 O9 Cu1 120.9(4) . . ?
C29 O10 Cu2 123.9(3) . . ?
C30 O11 Cu1 123.7(3) . 6_564 ?
C30 O12 Cu2 122.0(4) . 6_564 ?
C2 C1 C6 119.6(5) . . ?
C2 C1 C7 120.0(5) . . ?
C6 C1 C7 120.4(5) . . ?
C1 C2 C3 122.8(5) . . ?
C1 C2 H2A 118.6 . . ?
C3 C2 H2A 118.6 . . ?
C2 C3 C4 117.1(4) . . ?
C2 C3 C15 122.2(5) . . ?
C4 C3 C15 120.7(4) . . ?
C5 C4 C3 120.4(5) . . ?
C5 C4 H4A 119.8 . . ?
C3 C4 H4A 119.8 . . ?
C4 C5 C6 122.0(5) . . ?
C4 C5 H5A 119.0 . . ?
C6 C5 H5A 119.0 . . ?
C1 C6 C5 117.9(5) . . ?
C1 C6 H6A 121.0 . . ?
C5 C6 H6A 121.0 . . ?
C8 C7 C12 117.4(4) . . ?
C8 C7 C1 120.8(5) . . ?
C12 C7 C1 121.7(4) . . ?
C7 C8 C9 121.0(5) . . ?
C7 C8 H8A 119.5 . . ?
C9 C8 H8A 119.5 . . ?
C10 C9 C8 120.1(4) . . ?
C10 C9 C13 120.3(4) . . ?
C8 C9 C13 119.6(4) . . ?
C9 C10 C11 120.0(4) . . ?
C9 C10 H10A 120.0 . . ?
C11 C10 H10A 120.0 . . ?
C12 C11 C10 119.6(5) . . ?
C12 C11 C14 120.7(4) . . ?
C10 C11 C14 119.6(4) . . ?
C11 C12 C7 121.8(4) . . ?
C11 C12 H12A 119.1 . . ?
C7 C12 H12A 119.1 . . ?
O2 C13 O1 128.9(4) . . ?
O2 C13 C9 115.8(4) . . ?
O1 C13 C9 115.4(4) . . ?
O3 C14 O4 125.7(5) . . ?
O3 C14 C11 115.7(4) . . ?
O4 C14 C11 118.5(4) . . ?
C16 C15 C20 117.4(4) . . ?
C16 C15 C3 121.7(4) . . ?
C20 C15 C3 120.9(5) . . ?
C17 C16 C15 120.9(4) . . ?
C17 C16 H16A 119.6 . . ?
C15 C16 H16A 119.6 . . ?
C16 C17 C18 120.7(5) . . ?
C16 C17 C21 122.1(4) . . ?
C18 C17 C21 117.2(4) . . ?
C19 C18 C17 119.9(4) . . ?
C19 C18 H18A 120.1 . . ?
C17 C18 H18A 120.1 . . ?
C20 C19 C18 119.9(4) . . ?
C20 C19 C22 121.6(5) . . ?
C18 C19 C22 118.3(4) . . ?
C19 C20 C15 121.2(5) . . ?
C19 C20 H20A 119.4 . . ?
C15 C20 H20A 119.4 . . ?
O6 C21 O5 127.6(5) . . ?
O6 C21 C17 115.4(4) . . ?
O5 C21 C17 117.0(4) . . ?
O7 C22 O8 126.7(4) . . ?
O7 C22 C19 117.7(5) . . ?
O8 C22 C19 115.5(4) . . ?
C24 C23 C28 119.8(4) . . ?
C24 C23 C29 118.4(5) . . ?
C28 C23 C29 121.4(4) . . ?
C23 C24 C25 120.4(5) . . ?
C23 C24 H24A 119.8 . . ?
C25 C24 H24A 119.8 . . ?
C24 C25 C26 118.5(4) . . ?
C24 C25 C30 120.8(5) . . ?
C26 C25 C30 120.7(4) . . ?
C27 C26 C25 120.8(4) . . ?
C27 C26 H26A 119.6 . . ?
C25 C26 H26A 119.6 . . ?
C26 C27 C28 119.4(4) . . ?
C26 C27 C31 116.7(4) . . ?
C28 C27 C31 123.7(4) . . ?
C27 C28 C23 121.0(4) . . ?
C27 C28 H28A 119.5 . . ?
C23 C28 H28A 119.5 . . ?
O9 C29 O10 126.8(5) . . ?
O9 C29 C23 117.9(5) . . ?
O10 C29 C23 115.4(4) . . ?
O11 C30 O12 126.6(5) . . ?
O11 C30 C25 117.3(4) . . ?
O12 C30 C25 116.2(5) . . ?
C32 C31 C33 118.6(5) . . ?
C32 C31 C27 120.8(4) . . ?
C33 C31 C27 119.8(5) . . ?
C31 C32 C31 121.6(6) . 4 ?
C31 C32 H32A 119.2 . . ?
C31 C32 H32A 119.2 4 . ?
C34 C33 C31 119.1(6) . . ?
C34 C33 H33A 120.4 . . ?
C31 C33 H33A 120.4 . . ?
C33 C34 C33 122.8(8) . 4 ?
C33 C34 H34A 118.6 . . ?
C33 C34 H34A 118.6 4 . ?

_refine_diff_density_max         0.974
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.066



####################################################################### 
# 
# 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-102
_database_code_depnum_ccdc_archive 'CCDC 1895249'
loop_
_audit_author_name
_audit_author_address
'Yabing He' 'Zhejiang Normal University'
_audit_update_record             
;
2019-09-18 deposited with the CCDC.	2019-09-20 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         '(C23 H16 Cu2 O11).7(C3 H7 N O)'
_chemical_formula_sum            'C44 H65 Cu2 N7 O18'
_chemical_formula_weight         1107.11

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
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'

_space_group_crystal_system      cubic
_space_group_IT_number           200
_space_group_name_H-M_alt        'P m -3'
_space_group_name_Hall           '-P 2 2 3'

_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'
'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'
'-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'

_cell_length_a                   25.3148(4)
_cell_length_b                   25.3148(4)
_cell_length_c                   25.3148(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     16222.7(8)
_cell_formula_units_Z            12
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    50295
_cell_measurement_theta_min      2
_cell_measurement_theta_max      56

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_F_000             6960
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.070
_exptl_absorpt_coefficient_mu    0.860
_shelx_estimated_absorpt_T_min   0.889
_shelx_estimated_absorpt_T_max   0.942
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.907
_exptl_absorpt_correction_T_max  0.945
_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 SMART APEX II CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            50295
_diffrn_reflns_av_unetI/netI     0.0421
_diffrn_reflns_av_R_equivalents  0.0640
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.276
_diffrn_reflns_theta_max         28.279
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             7179
_reflns_number_gt                5109
_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    'SHELXS-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          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.3300P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7179
_refine_ls_number_parameters     176
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1470
_refine_ls_R_factor_gt           0.1166
_refine_ls_wR_factor_ref         0.3882
_refine_ls_wR_factor_gt          0.3343
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_platon_squeeze_details 
;
The solvent molecules were highly disordered, and thus their locations
cannot be precisely determined. To address this issue, electron density 
peaks of solvent molecules were removed by the PLATON/SQUEEZE procedure,
therefore producing a set of solvent-free diffraction intensities for 
further structural refinement.
;
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 0.5000 0.18655(5) 0.22366(5) 0.0409(3) Uani 1 2 d S T P . .
Cu2 Cu 0.5000 0.26494(5) 0.29367(5) 0.0443(4) Uani 1 2 d S T P . .
O1W O 0.5000 0.1228(5) 0.1679(5) 0.087(3) Uani 1 2 d S T P . .
O1 O 0.4455(3) 0.2291(2) 0.1889(3) 0.0608(16) Uani 1 1 d . . . . .
O2 O 0.4449(3) 0.2950(3) 0.2489(3) 0.0639(17) Uani 1 1 d . . . . .
O2W O 0.5000 0.3265(7) 0.3496(8) 0.173(10) Uani 1 2 d S T P . .
O3 O 0.3285(3) 0.4441(3) 0.2238(2) 0.0550(14) Uani 1 1 d . . . . .
O4 O 0.2681(2) 0.4437(3) 0.1572(2) 0.0532(14) Uani 1 1 d . . . . .
O5 O 0.3439(4) 0.3550(4) 0.0000 0.064(2) Uani 1 2 d S T P . .
C1 C 0.3878(4) 0.3002(4) 0.1749(3) 0.0516(18) Uani 1 1 d . . . . .
C2 C 0.3701(3) 0.3504(3) 0.1913(4) 0.0537(18) Uani 1 1 d . . . . .
H2A H 0.3841 0.3669 0.2220 0.064 Uiso 1 1 calc R U . . .
C3 C 0.3304(3) 0.3757(3) 0.1604(3) 0.0496(16) Uani 1 1 d . . . . .
C4 C 0.3129(3) 0.3525(4) 0.1150(3) 0.0541(19) Uani 1 1 d . . . . .
H4A H 0.2877 0.3704 0.0938 0.065 Uiso 1 1 calc R U . . .
C5 C 0.3308(4) 0.3040(4) 0.0995(4) 0.059(2) Uani 1 1 d . . . . .
C6 C 0.3677(4) 0.2780(3) 0.1305(3) 0.057(2) Uani 1 1 d . . . . .
H6A H 0.3793 0.2438 0.1203 0.068 Uiso 1 1 calc R U . . .
C7 C 0.4298(3) 0.2723(3) 0.2053(4) 0.0512(18) Uani 1 1 d . . . . .
C8 C 0.3062(4) 0.4244(3) 0.1820(3) 0.0507(18) Uani 1 1 d . . . . .
C9 C 0.3134(4) 0.2782(4) 0.0489(4) 0.061(2) Uani 1 1 d . . . . .
C10 C 0.3220(5) 0.3044(4) 0.0000 0.051(3) Uani 1 2 d S T P . .
C11 C 0.2914(5) 0.2289(4) 0.0458(5) 0.074(3) Uani 1 1 d . . . . .
H11A H 0.2809 0.2123 0.0777 0.089 Uiso 1 1 calc R U . . .
C12 C 0.2837(7) 0.2025(6) 0.0000 0.071(4) Uani 1 2 d S T P . .
H12A H 0.2733 0.1665 0.0000 0.085 Uiso 1 2 calc R U P . .
C13 C 0.3939(8) 0.3590(7) 0.0000 0.091(5) Uani 1 2 d S T P . .
H13A H 0.4044 0.3955 0.0000 0.137 Uiso 1 2 d R U P . .
H13B H 0.4076 0.3419 0.0310 0.137 Uiso 1 1 d R U . . .


_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 O4 1.961(5) 22_655 ?
Cu1 O4 1.961(5) 9 ?
Cu1 O1 1.959(6) . ?
Cu1 O1 1.959(6) 15_655 ?
Cu1 O1W 2.144(10) . ?
Cu1 Cu2 2.6606(17) . ?
Cu2 O3 1.966(6) 9 ?
Cu2 O3 1.966(6) 22_655 ?
Cu2 O2 1.951(7) . ?
Cu2 O2 1.951(7) 15_655 ?
Cu2 O2W 2.105(12) . ?
O1 C7 1.236(10) . ?
O2 C7 1.303(12) . ?
O3 C8 1.300(11) . ?
O3 Cu2 1.966(6) 5 ?
O4 C8 1.250(10) . ?
O4 Cu1 1.961(5) 5 ?
O5 C13 1.27(2) . ?
O5 C10 1.396(16) . ?
C1 C6 1.356(12) . ?
C1 C2 1.411(12) . ?
C1 C7 1.490(12) . ?
C2 C3 1.426(11) . ?
C2 H2A 0.9500 . ?
C3 C4 1.365(13) . ?
C3 C8 1.480(11) . ?
C4 C5 1.366(13) . ?
C4 H4A 0.9500 . ?
C5 C6 1.388(13) . ?
C5 C9 1.504(14) . ?
C6 H6A 0.9500 . ?
C9 C11 1.367(14) . ?
C9 C10 1.421(12) . ?
C10 C9 1.421(12) 14 ?
C11 C12 1.352(15) . ?
C11 H11A 0.9500 . ?
C12 C11 1.352(15) 14 ?
C12 H12A 0.9500 . ?
C13 H13A 0.9601 . ?
C13 H13B 0.9599 . ?

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
O4 Cu1 O4 93.2(4) 22_655 9 ?
O4 Cu1 O1 167.8(3) 22_655 . ?
O4 Cu1 O1 87.4(3) 9 . ?
O4 Cu1 O1 87.4(3) 22_655 15_655 ?
O4 Cu1 O1 167.8(3) 9 15_655 ?
O1 Cu1 O1 89.5(4) . 15_655 ?
O4 Cu1 O1W 95.3(3) 22_655 . ?
O4 Cu1 O1W 95.3(3) 9 . ?
O1 Cu1 O1W 96.8(3) . . ?
O1 Cu1 O1W 96.8(3) 15_655 . ?
O4 Cu1 Cu2 84.28(18) 22_655 . ?
O4 Cu1 Cu2 84.28(18) 9 . ?
O1 Cu1 Cu2 83.7(2) . . ?
O1 Cu1 Cu2 83.7(2) 15_655 . ?
O1W Cu1 Cu2 179.4(4) . . ?
O3 Cu2 O3 92.1(4) 9 22_655 ?
O3 Cu2 O2 87.3(3) 9 . ?
O3 Cu2 O2 169.0(3) 22_655 . ?
O3 Cu2 O2 169.0(3) 9 15_655 ?
O3 Cu2 O2 87.3(3) 22_655 15_655 ?
O2 Cu2 O2 91.2(5) . 15_655 ?
O3 Cu2 O2W 95.2(5) 9 . ?
O3 Cu2 O2W 95.2(5) 22_655 . ?
O2 Cu2 O2W 95.9(5) . . ?
O2 Cu2 O2W 95.9(5) 15_655 . ?
O3 Cu2 Cu1 84.52(18) 9 . ?
O3 Cu2 Cu1 84.52(18) 22_655 . ?
O2 Cu2 Cu1 84.5(2) . . ?
O2 Cu2 Cu1 84.5(2) 15_655 . ?
O2W Cu2 Cu1 179.5(6) . . ?
C7 O1 Cu1 124.2(6) . . ?
C7 O2 Cu2 122.1(5) . . ?
C8 O3 Cu2 120.7(5) . 5 ?
C8 O4 Cu1 122.4(5) . 5 ?
C13 O5 C10 118.1(12) . . ?
C6 C1 C2 119.9(8) . . ?
C6 C1 C7 119.9(8) . . ?
C2 C1 C7 120.2(8) . . ?
C1 C2 C3 117.9(8) . . ?
C1 C2 H2A 121.1 . . ?
C3 C2 H2A 121.1 . . ?
C4 C3 C2 119.8(8) . . ?
C4 C3 C8 122.3(8) . . ?
C2 C3 C8 117.6(7) . . ?
C3 C4 C5 121.4(8) . . ?
C3 C4 H4A 119.3 . . ?
C5 C4 H4A 119.3 . . ?
C6 C5 C4 119.2(9) . . ?
C6 C5 C9 118.1(8) . . ?
C4 C5 C9 122.6(8) . . ?
C1 C6 C5 121.6(8) . . ?
C1 C6 H6A 119.2 . . ?
C5 C6 H6A 119.2 . . ?
O1 C7 O2 125.5(8) . . ?
O1 C7 C1 118.4(8) . . ?
O2 C7 C1 116.0(7) . . ?
O4 C8 O3 126.5(7) . . ?
O4 C8 C3 117.3(7) . . ?
O3 C8 C3 116.1(7) . . ?
C11 C9 C10 116.0(10) . . ?
C11 C9 C5 124.4(10) . . ?
C10 C9 C5 119.6(9) . . ?
C9 C10 C9 121.2(11) . 14 ?
C9 C10 O5 119.3(6) . . ?
C9 C10 O5 119.3(6) 14 . ?
C9 C11 C12 123.9(12) . . ?
C9 C11 H11A 118.0 . . ?
C12 C11 H11A 118.0 . . ?
C11 C12 C11 118.0(15) 14 . ?
C11 C12 H12A 121.0 14 . ?
C11 C12 H12A 121.0 . . ?
O5 C13 H13A 110.8 . . ?
O5 C13 H13B 108.8 . . ?
H13A C13 H13B 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 1.2(13) . . . . ?
C7 C1 C2 C3 179.0(8) . . . . ?
C1 C2 C3 C4 -3.5(12) . . . . ?
C1 C2 C3 C8 170.9(8) . . . . ?
C2 C3 C4 C5 3.1(14) . . . . ?
C8 C3 C4 C5 -171.1(9) . . . . ?
C3 C4 C5 C6 -0.3(15) . . . . ?
C3 C4 C5 C9 -178.2(9) . . . . ?
C2 C1 C6 C5 1.6(14) . . . . ?
C7 C1 C6 C5 -176.3(9) . . . . ?
C4 C5 C6 C1 -2.1(15) . . . . ?
C9 C5 C6 C1 175.9(9) . . . . ?
Cu1 O1 C7 O2 -3.3(14) . . . . ?
Cu1 O1 C7 C1 -179.6(6) . . . . ?
Cu2 O2 C7 O1 4.3(14) . . . . ?
Cu2 O2 C7 C1 -179.4(6) . . . . ?
C6 C1 C7 O1 0.0(13) . . . . ?
C2 C1 C7 O1 -177.8(8) . . . . ?
C6 C1 C7 O2 -176.6(9) . . . . ?
C2 C1 C7 O2 5.5(12) . . . . ?
Cu1 O4 C8 O3 -14.8(12) 5 . . . ?
Cu1 O4 C8 C3 168.8(6) 5 . . . ?
Cu2 O3 C8 O4 15.3(12) 5 . . . ?
Cu2 O3 C8 C3 -168.2(6) 5 . . . ?
C4 C3 C8 O4 0.6(13) . . . . ?
C2 C3 C8 O4 -173.6(8) . . . . ?
C4 C3 C8 O3 -176.2(8) . . . . ?
C2 C3 C8 O3 9.6(12) . . . . ?
C6 C5 C9 C11 57.4(15) . . . . ?
C4 C5 C9 C11 -124.7(13) . . . . ?
C6 C5 C9 C10 -119.6(11) . . . . ?
C4 C5 C9 C10 58.3(15) . . . . ?
C11 C9 C10 C9 -7(2) . . . 14 ?
C5 C9 C10 C9 170.6(7) . . . 14 ?
C11 C9 C10 O5 179.5(11) . . . . ?
C5 C9 C10 O5 -3.3(16) . . . . ?
C13 O5 C10 C9 87.0(10) . . . . ?
C13 O5 C10 C9 -87.0(10) . . . 14 ?
C10 C9 C11 C12 8(2) . . . . ?
C5 C9 C11 C12 -169.0(14) . . . . ?
C9 C11 C12 C11 -9(3) . . . 14 ?

_refine_diff_density_max         2.326
_refine_diff_density_min         -1.033
_refine_diff_density_rms         0.180

_vrf_PLAT084_d_sq                
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.39 Report
RESPONSE: We made several attempts to obtain better quality data for
this structure, however, due to disorder, poor crystal
quality etc. the wR2 value is high. We are confidant the structural
characterization is valid.
;




####################################################################### 
# 
# 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-103
_database_code_depnum_ccdc_archive 'CCDC 1895250'
loop_
_audit_author_name
_audit_author_address
'Yabing He' 'Zhejiang Normal University'
_audit_update_record             
;
2019-09-16 deposited with the CCDC.	2019-09-20 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         '[C22H15Cu2NO10].5DMF.H2O'
_chemical_formula_sum            'C37 H52 Cu2 N6 O16'
_chemical_formula_weight         963.95

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'
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'

_space_group_crystal_system      hexagonal
_space_group_IT_number           194
_space_group_name_H-M_alt        'P 63/m m c'
_space_group_name_Hall           '-P 6c 2c'

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

_cell_length_a                   18.5762(5)
_cell_length_b                   18.5762(5)
_cell_length_c                   23.8042(16)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     7113.7(6)
_cell_formula_units_Z            6
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    74827
_cell_measurement_theta_min      3
_cell_measurement_theta_max      26

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_F_000             3011
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.966
_shelx_estimated_absorpt_T_min   0.816
_shelx_estimated_absorpt_T_max   0.910
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.812
_exptl_absorpt_correction_T_max  0.908
_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            74827
_diffrn_reflns_av_unetI/netI     0.0151
_diffrn_reflns_av_R_equivalents  0.0594
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.673
_diffrn_reflns_theta_max         24.994
_diffrn_reflns_theta_full        24.994
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             2361
_reflns_number_gt                1822
_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)+(0.3700P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2361
_refine_ls_number_parameters     86
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.1159
_refine_ls_R_factor_gt           0.0941
_refine_ls_wR_factor_ref         0.4170
_refine_ls_wR_factor_gt          0.3623
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_restrained_S_all      1.093
_refine_ls_shift/su_max          0.031
_refine_ls_shift/su_mean         0.004
_refine_ls_platon_squeeze_details 
;
The solvent molecules were highly disordered, and thus their locations
cannot be precisely determined. To address this issue, electron density 
peaks of solvent molecules were removed by the PLATON/SQUEEZE procedure,
therefore producing a set of solvent-free diffraction intensities for 
further structural refinement.
;
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 -0.04727(5) 0.47637(2) 0.04586(3) 0.0446(6) Uani 1 2 d S T P . .
O1 O 0.0305(2) 0.4407(3) 0.07111(18) 0.0615(11) Uani 1 1 d . . . . .
O1W O -0.1166(7) 0.4417(3) 0.1224(4) 0.123(3) Uani 1 2 d S T P . .
O2 O 0.1107(2) 0.4822(3) -0.00568(18) 0.0642(12) Uani 1 1 d . . . . .
C1 C 0.0899(3) 0.4506(4) 0.0429(2) 0.0522(14) Uani 1 1 d . . . . .
C2 C 0.1467(3) 0.4238(3) 0.0680(3) 0.0516(13) Uani 1 1 d . . . . .
C3 C 0.2220(3) 0.4441(5) 0.0436(3) 0.054(2) Uani 1 2 d S T P . .
H3A H 0.2365 0.4730 0.0088 0.065 Uiso 1 2 calc R U P . .
C4 C 0.1254(3) 0.3796(4) 0.1193(2) 0.0582(14) Uani 1 1 d . . . . .
H4A H 0.0744 0.3660 0.1371 0.070 Uiso 1 1 calc R U . . .
C5 C 0.1780(3) 0.3559(6) 0.1441(3) 0.0578(19) Uani 1 2 d S T P A .
C6 C 0.1546(3) 0.3093(6) 0.2000(4) 0.134(4) Uani 1 2 d DS T P . .
C7 C 0.1747(10) 0.349(2) 0.2500 0.134(4) Uani 0.5 4 d DS T P A 1
C8 C 0.1125(5) 0.2250(10) 0.2064(9) 0.134(4) Uani 0.5 2 d DS T P A 1
H8A H 0.0993 0.1986 0.1707 0.161 Uiso 0.5 2 calc R U P A 1
C9 C 0.0819(8) 0.1639(16) 0.2500 0.134(4) Uani 0.5 4 d DS T P A 1
H9A H 0.0524 0.1048 0.2500 0.161 Uiso 0.5 4 calc R U P A 1
N1 N 0.2203(11) 0.441(2) 0.2500 0.134(4) Uani 0.5 4 d DS T P A 1
H1A H 0.2343 0.4715 0.2173 0.161 Uiso 0.5 2 d R U P A 1
C7' C 0.1747(10) 0.349(2) 0.2500 0.134(4) Uani 0.5 4 d DS T P A 2
C8' C 0.1133(5) 0.2265(10) 0.1942(8) 0.134(4) Uani 0.5 2 d DS T P A 2
H8'A H 0.0982 0.1964 0.1599 0.161 Uiso 0.5 2 calc R U P A 2
C9' C 0.0959(9) 0.1919(18) 0.2500 0.134(4) Uani 0.5 4 d DS T P A 2
H9'A H 0.0664 0.1328 0.2500 0.161 Uiso 0.5 4 calc R U P A 2
N1' N 0.2204(11) 0.441(2) 0.2500 0.134(4) Uani 0.5 4 d DS T P A 2
H1'A H 0.2344 0.4644 0.2173 0.161 Uiso 0.5 2 d R U P A 2


_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 1.951(4) 12 ?
Cu1 O2 1.951(4) 13_565 ?
Cu1 O1 1.961(4) 24_565 ?
Cu1 O1 1.961(4) . ?
Cu1 O1W 2.136(7) . ?
Cu1 Cu1 2.6609(16) 13_565 ?
O1 C1 1.224(7) . ?
O2 C1 1.266(7) . ?
O2 Cu1 1.951(4) 13_565 ?
C1 C2 1.498(8) . ?
C2 C3 1.383(6) . ?
C2 C4 1.414(8) . ?
C3 C2 1.382(6) 20 ?
C3 H3A 0.9500 . ?
C4 C5 1.387(7) . ?
C4 H4A 0.9500 . ?
C5 C4 1.387(7) 20 ?
C5 C6 1.527(12) . ?
C6 C8' 1.338(17) . ?
C6 C7' 1.355(17) . ?
C6 C7 1.354(17) . ?
C6 C8 1.365(16) . ?
C7 C6 1.354(17) 16_556 ?
C7 N1 1.468(19) . ?
C8 C9 1.430(16) . ?
C8 H8A 0.9500 . ?
C9 C8 1.430(16) 16_556 ?
C9 H9A 0.9500 . ?
N1 H1A 0.9254 . ?
C7' N1' 1.469(19) . ?
C7' C6 1.355(17) 16_556 ?
C8' C9' 1.440(16) . ?
C8' H8'A 0.9500 . ?
C9' C8' 1.440(16) 16_556 ?
C9' H9'A 0.9500 . ?
N1' H1'A 0.8681 . ?

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 88.4(3) 12 13_565 ?
O2 Cu1 O1 167.54(18) 12 24_565 ?
O2 Cu1 O1 89.54(19) 13_565 24_565 ?
O2 Cu1 O1 89.54(19) 12 . ?
O2 Cu1 O1 167.54(18) 13_565 . ?
O1 Cu1 O1 89.9(3) 24_565 . ?
O2 Cu1 O1W 98.3(3) 12 . ?
O2 Cu1 O1W 98.3(3) 13_565 . ?
O1 Cu1 O1W 94.1(3) 24_565 . ?
O1 Cu1 O1W 94.1(3) . . ?
O2 Cu1 Cu1 84.07(13) 12 13_565 ?
O2 Cu1 Cu1 84.07(13) 13_565 13_565 ?
O1 Cu1 Cu1 83.49(12) 24_565 13_565 ?
O1 Cu1 Cu1 83.49(12) . 13_565 ?
O1W Cu1 Cu1 176.6(4) . 13_565 ?
C1 O1 Cu1 122.8(4) . . ?
C1 O2 Cu1 121.7(4) . 13_565 ?
O1 C1 O2 127.9(5) . . ?
O1 C1 C2 117.6(5) . . ?
O2 C1 C2 114.5(5) . . ?
C3 C2 C4 118.2(5) . . ?
C3 C2 C1 121.9(6) . . ?
C4 C2 C1 119.9(5) . . ?
C2 C3 C2 122.5(8) . 20 ?
C2 C3 H3A 118.8 . . ?
C2 C3 H3A 118.8 20 . ?
C5 C4 C2 121.0(5) . . ?
C5 C4 H4A 119.5 . . ?
C2 C4 H4A 119.5 . . ?
C4 C5 C4 119.2(7) . 20 ?
C4 C5 C6 120.3(4) . . ?
C4 C5 C6 120.3(4) 20 . ?
C8' C6 C7' 124.3(16) . . ?
C7 C6 C8 112.0(17) . . ?
C8' C6 C5 113.6(10) . . ?
C7' C6 C5 122.1(14) . . ?
C7 C6 C5 122.2(14) . . ?
C8 C6 C5 125.9(12) . . ?
C6 C7 C6 123(3) 16_556 . ?
C6 C7 N1 118.4(13) 16_556 . ?
C6 C7 N1 118.4(13) . . ?
C9 C8 C6 140(2) . . ?
C9 C8 H8A 110.0 . . ?
C6 C8 H8A 110.0 . . ?
C8 C9 C8 93(2) . 16_556 ?
C8 C9 H9A 133.5 . . ?
C8 C9 H9A 133.5 16_556 . ?
C7 N1 H1A 122.6 . . ?
N1' C7' C6 118.5(13) . 16_556 ?
N1' C7' C6 118.5(13) . . ?
C6 C7' C6 123(3) 16_556 . ?
C6 C8' C9' 106.9(19) . . ?
C6 C8' H8'A 126.5 . . ?
C9' C8' H8'A 126.5 . . ?
C8' C9' C8' 134(3) . 16_556 ?
C8' C9' H9'A 112.8 . . ?
C8' C9' H9'A 112.8 16_556 . ?
C7' N1' H1'A 116.0 . . ?

_refine_diff_density_max         2.182
_refine_diff_density_min         -1.245
_refine_diff_density_rms         0.126

_vrf_PLAT973_d_sq                
;
PROBLEM: Check Calcd Positive Resid. Density on       Cu1       2.15 eA-3
RESPONSE: The distance between residual density maximum peak and the metal atom is 0.03/A.
The residual density peak doesn't make sense in chemistry.
;

_vrf_PLAT084_d_sq                
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.41 Report
RESPONSE: We made several attempts to obtain better quality data for
this structure, however, due to disorder, poor crystal
quality etc. the wR2 value is high. We are confidant the structural
characterization is valid.
;



