# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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-81
_database_code_depnum_ccdc_archive 'CCDC 1827028'
_audit_update_record             
;
2018-04-09 deposited with the CCDC.
2018-06-05 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 O10 [16DMF+2H2O]'
_chemical_formula_sum            'C117 H164 Cu6 N16 O48'
_chemical_formula_weight         2943.94

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'
N N 0.0061 0.0033 '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'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   24.8102(15)
_cell_length_b                   33.4318(19)
_cell_length_c                   18.3552(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     15224.7(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    46239
_cell_measurement_theta_min      0.996
_cell_measurement_theta_max      27.56

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_F_000             6143
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    0.904
_shelx_estimated_absorpt_T_min   0.869
_shelx_estimated_absorpt_T_max   0.923
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.8742
_exptl_absorpt_correction_T_max  0.9263
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(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            46239
_diffrn_reflns_av_unetI/netI     0.1587
_diffrn_reflns_av_R_equivalents  0.0909
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.022
_diffrn_reflns_theta_max         27.564
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             17450
_reflns_number_gt                8870
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.939
_reflns_Friedel_fraction_max     0.996
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component perfect 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)+(0.0410P)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_abs_structure_details 
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_chemical_absolute_configuration ?
_refine_ls_number_reflns         17450
_refine_ls_number_parameters     468
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1345
_refine_ls_R_factor_gt           0.0681
_refine_ls_wR_factor_ref         0.1370
_refine_ls_wR_factor_gt          0.1234
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_restrained_S_all      1.015
_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_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 0.21893(4) 0.27421(3) 0.30141(5) 0.0302(2) Uani 1 1 d . . . . .
Cu2 Cu 0.29746(4) 0.23945(3) 0.37592(6) 0.0317(2) Uani 1 1 d . . . . .
Cu3 Cu 0.0000 0.13985(4) 0.10164(9) 0.0355(4) Uani 1 2 d S T P . .
Cu4 Cu 0.0000 0.06099(4) 0.11052(8) 0.0366(4) Uani 1 2 d S T P . .
O1 O 0.0564(2) 0.07162(16) 0.1829(3) 0.0399(15) Uani 1 1 d . . . . .
O2 O 0.0548(3) 0.13835(17) 0.1727(4) 0.065(2) Uani 1 1 d . . . . .
O3 O 0.1900(2) 0.21948(14) 0.2921(3) 0.0425(15) Uani 1 1 d . . . . .
O4 O 0.2568(2) 0.19062(15) 0.3541(3) 0.0453(17) Uani 1 1 d . . . . .
O5 O 0.0561(2) -0.06324(15) 0.5311(3) 0.0398(15) Uani 1 1 d . . . . .
O6 O 0.0541(3) -0.12992(18) 0.5270(4) 0.070(2) Uani 1 1 d . . . . .
O7 O 0.1746(2) -0.20638(14) 0.3831(3) 0.0423(15) Uani 1 1 d . . . . .
O8 O 0.2426(2) -0.17739(15) 0.3214(3) 0.0482(17) Uani 1 1 d . . . . .
O9 O 0.2662(2) 0.26329(17) 0.2182(3) 0.0441(16) Uani 1 1 d . . . . .
O10 O 0.3330(2) 0.23182(17) 0.2812(3) 0.0462(16) Uani 1 1 d . . . . .
O11 O 0.2500(3) 0.24981(17) -0.0412(3) 0.0428(15) Uani 1 1 d . . . . .
O12 O 0.3177(2) 0.22158(17) -0.1050(3) 0.0515(17) Uani 1 1 d . . . . .
O1W O 0.1575(3) 0.3077(2) 0.2482(4) 0.086(2) Uani 1 1 d . . . . .
H1WA H 0.1459 0.3035 0.2047 0.103 Uiso 1 1 d R U . . .
H1WB H 0.1405 0.3276 0.2668 0.103 Uiso 1 1 d R U . . .
O2W O 0.3584(3) 0.2097(3) 0.4361(4) 0.100(3) Uani 1 1 d . . . . .
H2WA H 0.3509 0.1854 0.4451 0.120 Uiso 1 1 d R U . . .
H2WB H 0.3673 0.2220 0.4749 0.120 Uiso 1 1 d R U . . .
O3W O 0.0000 0.2047(2) 0.0878(7) 0.101(2) Uani 1 2 d S T P . .
H3WA H 0.0278 0.2146 0.1079 0.121 Uiso 1 1 d R U . . .
O4W O 0.0000 -0.0020(2) 0.1226(5) 0.064(3) Uani 1 2 d S T P . .
H4WA H -0.0278 -0.0091 0.1464 0.077 Uiso 1 1 d R U . . .
C1 C 0.0741(4) 0.1062(3) 0.1984(5) 0.040(2) Uani 1 1 d . . . . .
C2 C 0.1228(4) 0.1096(2) 0.2473(4) 0.037(2) Uani 1 1 d . . . . .
C3 C 0.1485(3) 0.0747(2) 0.2728(4) 0.036(2) Uani 1 1 d . . . . .
H3 H 0.1333 0.0498 0.2632 0.044 Uiso 1 1 calc R U . . .
C4 C 0.1433(4) 0.1454(2) 0.2635(5) 0.040(2) Uani 1 1 d . . . . .
H4 H 0.1256 0.1683 0.2476 0.048 Uiso 1 1 calc R U . . .
C5 C 0.1910(3) 0.1491(2) 0.3041(5) 0.034(2) Uani 1 1 d . . . . .
C6 C 0.2164(4) 0.1159(2) 0.3284(4) 0.040(2) Uani 1 1 d . . . . .
H6 H 0.2475 0.1183 0.3562 0.048 Uiso 1 1 calc R U . . .
C7 C 0.1953(3) 0.0768(2) 0.3114(5) 0.037(2) Uani 1 1 d . . . . .
C8 C 0.2146(4) 0.1905(2) 0.3189(4) 0.033(2) Uani 1 1 d . . . . .
C9 C 0.2237(4) 0.0416(2) 0.3367(5) 0.043(2) Uani 1 1 d . . . . .
C10 C 0.1966(3) 0.0065(2) 0.3559(5) 0.047(3) Uani 1 1 d . . . . .
H10 H 0.1592 0.0063 0.3537 0.056 Uiso 1 1 calc R U . . .
C11 C 0.2814(4) 0.0399(3) 0.3384(6) 0.069(4) Uani 1 1 d . . . . .
H11 H 0.3022 0.0613 0.3221 0.083 Uiso 1 1 calc R U . . .
C12 C 0.2228(3) -0.0282(2) 0.3781(6) 0.046(2) Uani 1 1 d . . . . .
C13 C 0.3055(3) 0.0049(3) 0.3655(10) 0.101(5) Uani 1 1 d . . . . .
C14 C 0.3701(4) 0.0050(3) 0.3571(8) 0.101(2) Uani 1 1 d . . . . .
H14A H 0.3824 0.0318 0.3484 0.151 Uiso 1 1 calc R U . . .
H14B H 0.3862 -0.0051 0.4011 0.151 Uiso 1 1 calc R U . . .
H14C H 0.3803 -0.0118 0.3169 0.151 Uiso 1 1 calc R U . . .
C15 C 0.2779(5) -0.0283(3) 0.3779(8) 0.101(2) Uani 1 1 d . . . . .
H15 H 0.2963 -0.0521 0.3866 0.121 Uiso 1 1 calc R U . . .
C16 C 0.1925(3) -0.0642(2) 0.3950(5) 0.042(2) Uani 1 1 d . . . . .
C17 C 0.1461(4) -0.0627(2) 0.4399(4) 0.043(2) Uani 1 1 d . . . . .
H17 H 0.1343 -0.0383 0.4581 0.052 Uiso 1 1 calc R U . . .
C18 C 0.1184(4) -0.0969(2) 0.4568(5) 0.041(2) Uani 1 1 d . . . . .
C19 C 0.0730(4) -0.0968(3) 0.5104(5) 0.042(2) Uani 1 1 d . . . . .
C20 C 0.1334(4) -0.1336(3) 0.4292(5) 0.054(3) Uani 1 1 d . . . . .
H20 H 0.1138 -0.1567 0.4393 0.065 Uiso 1 1 calc R U . . .
C21 C 0.2070(4) -0.1018(2) 0.3676(5) 0.039(2) Uani 1 1 d . . . . .
H21 H 0.2364 -0.1038 0.3365 0.047 Uiso 1 1 calc R U . . .
C22 C 0.1800(4) -0.1344(2) 0.3849(5) 0.041(2) Uani 1 1 d D . . . .
C23 C 0.1984(4) -0.1764(2) 0.3619(5) 0.039(2) Uani 1 1 d D . . . .
C24 C 0.3095(4) 0.2436(2) 0.2237(5) 0.035(2) Uani 1 1 d . . . . .
C25 C 0.3350(4) 0.2310(2) 0.1513(4) 0.034(2) Uani 1 1 d . . . . .
C26 C 0.3811(3) 0.2095(2) 0.1482(5) 0.040(2) Uani 1 1 d . . . . .
H26 H 0.4009 0.2051 0.1905 0.048 Uiso 1 1 calc R U . . .
C27 C 0.3071(3) 0.2385(2) 0.0861(5) 0.038(2) Uani 1 1 d . . . . .
H27 H 0.2752 0.2531 0.0876 0.045 Uiso 1 1 calc R U . . .
C28 C 0.3251(3) 0.2250(2) 0.0217(4) 0.034(2) Uani 1 1 d . . . . .
C29 C 0.3988(4) 0.1941(2) 0.0837(5) 0.043(2) Uani 1 1 d . . . . .
C30 C 0.3721(3) 0.2019(2) 0.0190(4) 0.036(2) Uani 1 1 d . . . . .
H30 H 0.3851 0.1920 -0.0251 0.043 Uiso 1 1 calc R U . . .
C31 C 0.2971(4) 0.2322(2) -0.0434(5) 0.032(2) Uani 1 1 d . . . . .
C32 C 0.4516(3) 0.1707(3) 0.0792(5) 0.041(2) Uani 1 1 d . . . . .
C33 C 0.5000 0.1875(3) 0.0944(7) 0.042(3) Uani 1 2 d S T P . .
H33 H 0.5000 0.2125 0.1168 0.050 Uiso 1 2 calc R U P . .
C34 C 0.4519(4) 0.1332(3) 0.0427(5) 0.053(3) Uani 1 1 d . . . . .
H34 H 0.4197 0.1215 0.0279 0.063 Uiso 1 1 calc R U . . .
C35 C 0.5000 0.1146(4) 0.0295(11) 0.101(2) Uani 1 2 d S T P . .
C36 C 0.5000 0.0721(5) 0.0004(10) 0.114(7) Uani 1 2 d S T P . .
H36A H 0.4698 0.0683 -0.0280 0.136 Uiso 1 1 d R U . . .
H36B H 0.5000 0.0528 0.0381 0.136 Uiso 1 2 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 O8 1.914(6) 7 ?
Cu1 O12 1.948(6) 6 ?
Cu1 O9 1.959(5) . ?
Cu1 O3 1.973(5) . ?
Cu1 O1W 2.128(6) . ?
Cu1 Cu2 2.6490(13) . ?
Cu2 O7 1.943(5) 7 ?
Cu2 O11 1.956(6) 6 ?
Cu2 O4 1.960(5) . ?
Cu2 O10 1.965(5) . ?
Cu2 O2W 2.121(6) . ?
Cu3 O2 1.885(6) . ?
Cu3 O2 1.886(6) 3 ?
Cu3 O6 1.946(7) 2_554 ?
Cu3 O6 1.946(7) 4_554 ?
Cu3 O3W 2.182(8) . ?
Cu3 Cu4 2.6415(17) . ?
Cu4 O1 1.962(6) 3 ?
Cu4 O1 1.962(6) . ?
Cu4 O5 2.016(6) 2_554 ?
Cu4 O5 2.016(6) 4_554 ?
Cu4 O4W 2.119(8) . ?
O1 C1 1.269(9) . ?
O2 C1 1.267(9) . ?
O3 C8 1.246(9) . ?
O4 C8 1.231(9) . ?
O5 C19 1.257(9) . ?
O5 Cu4 2.016(6) 2 ?
O6 C19 1.239(10) . ?
O6 Cu3 1.946(7) 2 ?
O7 C23 1.227(9) . ?
O7 Cu2 1.943(5) 7_545 ?
O8 C23 1.326(10) . ?
O8 Cu1 1.914(6) 7_545 ?
O9 C24 1.265(9) . ?
O10 C24 1.267(9) . ?
O11 C31 1.310(9) . ?
O11 Cu2 1.956(6) 6_554 ?
O12 C31 1.292(9) . ?
O12 Cu1 1.948(6) 6_554 ?
O1W H1WA 0.8610 . ?
O1W H1WB 0.8600 . ?
O2W H2WA 0.8502 . ?
O2W H2WB 0.8501 . ?
O3W H3WA 0.8500 . ?
O4W H4WA 0.8500 . ?
C1 C2 1.510(12) . ?
C2 C4 1.332(10) . ?
C2 C3 1.410(11) . ?
C3 C7 1.363(11) . ?
C3 H3 0.9300 . ?
C4 C5 1.404(11) . ?
C4 H4 0.9300 . ?
C5 C6 1.353(10) . ?
C5 C8 1.524(10) . ?
C6 C7 1.441(11) . ?
C6 H6 0.9300 . ?
C7 C9 1.448(11) . ?
C9 C10 1.397(10) . ?
C9 C11 1.433(12) . ?
C10 C12 1.390(10) . ?
C10 H10 0.9300 . ?
C11 C13 1.407(12) . ?
C11 H11 0.9300 . ?
C12 C15 1.367(14) . ?
C12 C16 1.452(11) . ?
C13 C15 1.324(13) . ?
C13 C14 1.609(12) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15 0.9300 . ?
C16 C21 1.401(10) . ?
C16 C17 1.417(11) . ?
C17 C18 1.368(11) . ?
C17 H17 0.9300 . ?
C18 C20 1.380(11) . ?
C18 C19 1.496(12) . ?
C20 C22 1.413(12) . ?
C20 H20 0.9300 . ?
C21 C22 1.319(10) . ?
C21 H21 0.9300 . ?
C22 C23 1.533(9) . ?
C24 C25 1.533(11) . ?
C25 C26 1.351(11) . ?
C25 C27 1.405(10) . ?
C26 C29 1.365(11) . ?
C26 H26 0.9300 . ?
C27 C28 1.342(11) . ?
C27 H27 0.9300 . ?
C28 C30 1.399(11) . ?
C28 C31 1.403(11) . ?
C29 C30 1.385(11) . ?
C29 C32 1.527(11) . ?
C30 H30 0.9300 . ?
C32 C33 1.355(9) . ?
C32 C34 1.420(11) . ?
C33 C32 1.355(9) 3_655 ?
C33 H33 0.9300 . ?
C34 C35 1.367(10) . ?
C34 H34 0.9300 . ?
C35 C34 1.367(10) 3_655 ?
C35 C36 1.52(2) . ?
C36 H36A 0.9201 . ?
C36 H36B 0.9449 . ?

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
O8 Cu1 O12 90.1(2) 7 6 ?
O8 Cu1 O9 90.5(2) 7 . ?
O12 Cu1 O9 168.4(3) 6 . ?
O8 Cu1 O3 169.1(2) 7 . ?
O12 Cu1 O3 88.5(2) 6 . ?
O9 Cu1 O3 88.7(2) . . ?
O8 Cu1 O1W 90.0(3) 7 . ?
O12 Cu1 O1W 91.9(3) 6 . ?
O9 Cu1 O1W 99.7(3) . . ?
O3 Cu1 O1W 100.8(3) . . ?
O8 Cu1 Cu2 84.56(18) 7 . ?
O12 Cu1 Cu2 85.42(17) 6 . ?
O9 Cu1 Cu2 83.14(17) . . ?
O3 Cu1 Cu2 84.54(17) . . ?
O1W Cu1 Cu2 173.9(2) . . ?
O7 Cu2 O11 89.5(2) 7 6 ?
O7 Cu2 O4 166.7(2) 7 . ?
O11 Cu2 O4 90.1(2) 6 . ?
O7 Cu2 O10 91.2(2) 7 . ?
O11 Cu2 O10 168.8(2) 6 . ?
O4 Cu2 O10 86.7(2) . . ?
O7 Cu2 O2W 98.5(3) 7 . ?
O11 Cu2 O2W 96.3(3) 6 . ?
O4 Cu2 O2W 94.8(3) . . ?
O10 Cu2 O2W 94.6(3) . . ?
O7 Cu2 Cu1 83.57(17) 7 . ?
O11 Cu2 Cu1 83.01(17) 6 . ?
O4 Cu2 Cu1 83.18(17) . . ?
O10 Cu2 Cu1 85.98(17) . . ?
O2W Cu2 Cu1 177.8(2) . . ?
O2 Cu3 O2 92.3(5) . 3 ?
O2 Cu3 O6 168.5(2) . 2_554 ?
O2 Cu3 O6 89.2(3) 3 2_554 ?
O2 Cu3 O6 89.2(3) . 4_554 ?
O2 Cu3 O6 168.5(2) 3 4_554 ?
O6 Cu3 O6 87.1(5) 2_554 4_554 ?
O2 Cu3 O3W 96.1(3) . . ?
O2 Cu3 O3W 96.1(3) 3 . ?
O6 Cu3 O3W 95.0(3) 2_554 . ?
O6 Cu3 O3W 95.0(3) 4_554 . ?
O2 Cu3 Cu4 86.03(17) . . ?
O2 Cu3 Cu4 86.03(17) 3 . ?
O6 Cu3 Cu4 82.72(18) 2_554 . ?
O6 Cu3 Cu4 82.72(18) 4_554 . ?
O3W Cu3 Cu4 176.9(4) . . ?
O1 Cu4 O1 90.9(3) 3 . ?
O1 Cu4 O5 89.5(2) 3 2_554 ?
O1 Cu4 O5 167.1(2) . 2_554 ?
O1 Cu4 O5 167.1(2) 3 4_554 ?
O1 Cu4 O5 89.5(2) . 4_554 ?
O5 Cu4 O5 87.3(3) 2_554 4_554 ?
O1 Cu4 O4W 96.3(2) 3 . ?
O1 Cu4 O4W 96.3(2) . . ?
O5 Cu4 O4W 96.5(2) 2_554 . ?
O5 Cu4 O4W 96.5(2) 4_554 . ?
O1 Cu4 Cu3 82.01(16) 3 . ?
O1 Cu4 Cu3 82.01(16) . . ?
O5 Cu4 Cu3 85.31(15) 2_554 . ?
O5 Cu4 Cu3 85.31(15) 4_554 . ?
O4W Cu4 Cu3 177.6(3) . . ?
C1 O1 Cu4 124.3(5) . . ?
C1 O2 Cu3 123.5(6) . . ?
C8 O3 Cu1 120.7(5) . . ?
C8 O4 Cu2 123.3(5) . . ?
C19 O5 Cu4 118.8(6) . 2 ?
C19 O6 Cu3 125.8(6) . 2 ?
C23 O7 Cu2 124.8(5) . 7_545 ?
C23 O8 Cu1 122.8(5) . 7_545 ?
C24 O9 Cu1 122.9(5) . . ?
C24 O10 Cu2 119.4(5) . . ?
C31 O11 Cu2 126.6(5) . 6_554 ?
C31 O12 Cu1 124.6(6) . 6_554 ?
Cu1 O1W H1WA 125.5 . . ?
Cu1 O1W H1WB 125.2 . . ?
H1WA O1W H1WB 109.3 . . ?
Cu2 O2W H2WA 113.2 . . ?
Cu2 O2W H2WB 113.2 . . ?
H2WA O2W H2WB 110.9 . . ?
Cu3 O3W H3WA 109.6 . . ?
Cu4 O4W H4WA 109.3 . . ?
O2 C1 O1 123.9(8) . . ?
O2 C1 C2 117.4(8) . . ?
O1 C1 C2 118.6(8) . . ?
C4 C2 C3 119.8(8) . . ?
C4 C2 C1 120.3(8) . . ?
C3 C2 C1 119.8(7) . . ?
C7 C3 C2 120.9(7) . . ?
C7 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
C2 C4 C5 121.3(8) . . ?
C2 C4 H4 119.3 . . ?
C5 C4 H4 119.3 . . ?
C6 C5 C4 119.6(7) . . ?
C6 C5 C8 120.5(8) . . ?
C4 C5 C8 120.0(8) . . ?
C5 C6 C7 120.3(8) . . ?
C5 C6 H6 119.8 . . ?
C7 C6 H6 119.8 . . ?
C3 C7 C6 118.0(8) . . ?
C3 C7 C9 122.5(8) . . ?
C6 C7 C9 119.5(8) . . ?
O4 C8 O3 128.2(7) . . ?
O4 C8 C5 115.1(8) . . ?
O3 C8 C5 116.6(8) . . ?
C10 C9 C11 116.2(8) . . ?
C10 C9 C7 122.1(8) . . ?
C11 C9 C7 121.6(8) . . ?
C12 C10 C9 123.4(8) . . ?
C12 C10 H10 118.3 . . ?
C9 C10 H10 118.3 . . ?
C13 C11 C9 117.8(8) . . ?
C13 C11 H11 121.1 . . ?
C9 C11 H11 121.1 . . ?
C15 C12 C10 117.9(8) . . ?
C15 C12 C16 121.0(8) . . ?
C10 C12 C16 120.8(7) . . ?
C15 C13 C11 122.5(9) . . ?
C15 C13 C14 122.3(9) . . ?
C11 C13 C14 112.9(9) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 C12 121.1(10) . . ?
C13 C15 H15 119.4 . . ?
C12 C15 H15 119.4 . . ?
C21 C16 C17 116.6(8) . . ?
C21 C16 C12 122.3(8) . . ?
C17 C16 C12 121.0(8) . . ?
C18 C17 C16 120.8(8) . . ?
C18 C17 H17 119.6 . . ?
C16 C17 H17 119.6 . . ?
C17 C18 C20 121.6(9) . . ?
C17 C18 C19 121.8(8) . . ?
C20 C18 C19 116.4(8) . . ?
O6 C19 O5 126.7(9) . . ?
O6 C19 C18 116.5(8) . . ?
O5 C19 C18 116.8(8) . . ?
C18 C20 C22 116.7(9) . . ?
C18 C20 H20 121.7 . . ?
C22 C20 H20 121.7 . . ?
C22 C21 C16 121.7(8) . . ?
C22 C21 H21 119.1 . . ?
C16 C21 H21 119.1 . . ?
C21 C22 C20 122.5(8) . . ?
C21 C22 C23 122.6(8) . . ?
C20 C22 C23 114.8(8) . . ?
O7 C23 O8 123.6(7) . . ?
O7 C23 C22 121.2(8) . . ?
O8 C23 C22 115.1(7) . . ?
O9 C24 O10 128.2(8) . . ?
O9 C24 C25 115.1(8) . . ?
O10 C24 C25 116.6(8) . . ?
C26 C25 C27 118.4(8) . . ?
C26 C25 C24 122.1(8) . . ?
C27 C25 C24 119.1(8) . . ?
C25 C26 C29 120.7(9) . . ?
C25 C26 H26 119.7 . . ?
C29 C26 H26 119.7 . . ?
C28 C27 C25 121.7(8) . . ?
C28 C27 H27 119.2 . . ?
C25 C27 H27 119.2 . . ?
C27 C28 C30 119.7(8) . . ?
C27 C28 C31 121.7(8) . . ?
C30 C28 C31 118.5(8) . . ?
C26 C29 C30 121.2(8) . . ?
C26 C29 C32 121.1(8) . . ?
C30 C29 C32 117.5(8) . . ?
C29 C30 C28 118.2(8) . . ?
C29 C30 H30 120.9 . . ?
C28 C30 H30 120.9 . . ?
O12 C31 O11 120.2(8) . . ?
O12 C31 C28 120.1(8) . . ?
O11 C31 C28 119.6(8) . . ?
C33 C32 C34 117.3(9) . . ?
C33 C32 C29 122.4(8) . . ?
C34 C32 C29 118.7(8) . . ?
C32 C33 C32 124.8(11) . 3_655 ?
C32 C33 H33 117.6 . . ?
C32 C33 H33 117.6 3_655 . ?
C35 C34 C32 119.3(10) . . ?
C35 C34 H34 120.4 . . ?
C32 C34 H34 120.4 . . ?
C34 C35 C34 121.6(14) . 3_655 ?
C34 C35 C36 119.2(7) . . ?
C34 C35 C36 119.2(7) 3_655 . ?
C35 C36 H36A 109.0 . . ?
C35 C36 H36B 112.3 . . ?
H36A C36 H36B 108.8 . . ?

_refine_diff_density_max         1.063
_refine_diff_density_min         -0.943
_refine_diff_density_rms         0.105



# SQUEEZE RESULTS (APPEND TO CIF)
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 0.335 0.019 0.006 10047.3 4378.0
_platon_squeeze_details          
; The residual electron density of 4378 electrons per unit cell was tentatively assigned to 16 DMF and 2 H2O, which was mainly established according to the elemental analysis
;

_vrf_CHEMW03_ZJNU-81             
;
PROBLEM:    The ratio of given/expected molecular weight as
            calculated from the _atom_site* data lies outside
            the range 0.90 <> 1.10
           From the CIF: _cell_formula_units_Z                    4
           From the CIF: _chemical_formula_weight          2943.94
           TEST: Calculate formula weight from _atom_site_*
           atom     mass    num     sum
           C        12.01   69.00  828.76
           H         1.01   48.00   48.38
           Cu       63.55    6.00  381.28
           O        16.00   30.00  479.97
           N        14.01    0.00    0.00
           Calculated formula weight             1738.39


RESPONSE: The empirical formula contains the lattice molecules.
;
####################################################################### 
# 
# 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-82
_database_code_depnum_ccdc_archive 'CCDC 1827029'
_audit_update_record             
;
2018-04-09 deposited with the CCDC.
2018-06-05 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 O10 [5DMF.H2O]'
_chemical_formula_sum            'C38 H53 Cu2 N5 O16'
_chemical_formula_weight         962.93

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

_cell_length_a                   18.4999(3)
_cell_length_b                   18.4999(3)
_cell_length_c                   24.0168(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     7118.5(2)
_cell_formula_units_Z            6
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    25879
_cell_measurement_theta_min      0.966
_cell_measurement_theta_max      74.01

_exptl_crystal_description       needle
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_F_000             3012
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    1.696
_shelx_estimated_absorpt_T_min   0.728
_shelx_estimated_absorpt_T_max   0.935
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7735
_exptl_absorpt_correction_T_max  0.9478
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD area detector'
_diffrn_measurement_method       multi-scan
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25879
_diffrn_reflns_av_unetI/netI     0.0538
_diffrn_reflns_av_R_equivalents  0.0717
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.758
_diffrn_reflns_theta_max         74.090
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2701
_reflns_number_gt                2257
_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.
 
 _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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.1000P)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     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00016(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2701
_refine_ls_number_parameters     95
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0398
_refine_ls_wR_factor_ref         0.1368
_refine_ls_wR_factor_gt          0.1313
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_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 0.04826(2) 0.52413(2) 0.45518(2) 0.04446(18) Uani 1 2 d S T P . .
O1 O 0.11015(7) 0.62961(8) 0.49626(5) 0.0585(3) Uani 1 1 d . . . . .
O2 O 0.02799(8) 0.58894(9) 0.57163(5) 0.0599(4) Uani 1 1 d . . . . .
O1W O 0.12647(18) 0.56324(9) 0.38209(10) 0.0972(8) Uani 1 2 d S T P . .
H1WA H 0.1077 0.5229 0.3589 0.117 Uiso 1 1 d R U . . .
C1 C 0.08993(11) 0.64139(13) 0.54359(6) 0.0517(4) Uani 1 1 d . . . . .
C2 C 0.14548(10) 0.72496(11) 0.56966(7) 0.0508(4) Uani 1 1 d . . . . .
C3 C 0.22101(8) 0.77899(8) 0.54428(9) 0.0507(6) Uani 1 2 d S T P . .
H3A H 0.2353 0.7647 0.5106 0.061 Uiso 1 2 calc R U P . .
C4 C 0.12380(11) 0.74627(12) 0.62036(7) 0.0542(4) Uani 1 1 d . . . . .
H4A H 0.0736 0.7093 0.6375 0.065 Uiso 1 1 calc R U . . .
C5 C 0.17737(9) 0.82263(9) 0.64511(9) 0.0527(5) Uani 1 2 d S T P . .
C6 C 0.15456(9) 0.84544(9) 0.69979(10) 0.0557(6) Uani 1 2 d S T P . .
C9 C 0.17641(13) 0.82359(13) 0.7500 0.0568(8) Uani 1 4 d S T P . .
C7 C 0.11268(12) 0.88732(12) 0.70022(13) 0.1206(18) Uani 1 2 d S T P . .
H7A H 0.0982 0.9018 0.6666 0.145 Uiso 1 2 calc R U P . .
C8 C 0.09041(19) 0.90959(19) 0.7500 0.189(5) Uani 1 4 d S T P . .
H8A H 0.0614 0.9386 0.7500 0.227 Uiso 1 4 calc R U P . .
C10 C 0.22242(19) 0.77758(19) 0.7500 0.156(4) Uani 1 4 d S T P . .
H10B H 0.2324 0.7676 0.7877 0.233 Uiso 0.5 2 d R U P . .
H10A H 0.1900 0.7249 0.7312 0.233 Uiso 0.5 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 1.9568(13) 13_566 ?
Cu1 O2 1.9568(13) 9_556 ?
Cu1 O1 1.9641(13) . ?
Cu1 O1 1.9642(13) 21_565 ?
Cu1 O1W 2.157(2) . ?
Cu1 Cu1 2.6505(6) 13_566 ?
O1 C1 1.249(2) . ?
O2 C1 1.263(2) . ?
O2 Cu1 1.9568(13) 13_566 ?
C1 C2 1.500(3) . ?
C2 C3 1.388(2) . ?
C2 C4 1.399(2) . ?
C3 C2 1.388(2) 19_665 ?
C4 C5 1.390(2) . ?
C5 C4 1.390(2) 19_665 ?
C5 C6 1.503(3) . ?
C6 C7 1.342(4) . ?
C6 C9 1.394(3) . ?
C9 C6 1.394(3) 16_557 ?
C9 C10 1.474(7) . ?
C7 C8 1.392(4) . ?
C8 C7 1.392(4) 16_557 ?

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 90.24(9) 13_566 9_556 ?
O2 Cu1 O1 167.91(5) 13_566 . ?
O2 Cu1 O1 89.03(6) 9_556 . ?
O2 Cu1 O1 89.03(6) 13_566 21_565 ?
O2 Cu1 O1 167.91(5) 9_556 21_565 ?
O1 Cu1 O1 89.17(8) . 21_565 ?
O2 Cu1 O1W 95.45(7) 13_566 . ?
O2 Cu1 O1W 95.45(7) 9_556 . ?
O1 Cu1 O1W 96.63(7) . . ?
O1 Cu1 O1W 96.63(7) 21_565 . ?
O2 Cu1 Cu1 84.43(4) 13_566 13_566 ?
O2 Cu1 Cu1 84.43(4) 9_556 13_566 ?
O1 Cu1 Cu1 83.49(4) . 13_566 ?
O1 Cu1 Cu1 83.49(4) 21_565 13_566 ?
O1W Cu1 Cu1 179.83(8) . 13_566 ?
C1 O1 Cu1 123.61(12) . . ?
C1 O2 Cu1 122.53(12) . 13_566 ?
O1 C1 O2 125.92(18) . . ?
O1 C1 C2 116.68(16) . . ?
O2 C1 C2 117.39(15) . . ?
C3 C2 C4 120.43(17) . . ?
C3 C2 C1 118.90(16) . . ?
C4 C2 C1 120.57(16) . . ?
C2 C3 C2 119.4(2) 19_665 . ?
C5 C4 C2 119.97(17) . . ?
C4 C5 C4 119.7(2) 19_665 . ?
C4 C5 C6 120.10(11) 19_665 . ?
C4 C5 C6 120.10(11) . . ?
C7 C6 C9 119.7(3) . . ?
C7 C6 C5 119.5(2) . . ?
C9 C6 C5 120.8(3) . . ?
C6 C9 C6 119.7(4) . 16_557 ?
C6 C9 C10 120.14(19) . . ?
C6 C9 C10 120.14(19) 16_557 . ?
C6 C7 C8 121.3(3) . . ?
C7 C8 C7 118.3(5) 16_557 . ?

_refine_diff_density_max         0.449
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.070



# SQUEEZE RESULTS (APPEND TO CIF)
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 -0.042 -0.030 -0.002 4494.7 1110.2
_platon_squeeze_details          
; The residual electron density of 1110.2 electrons per unit cell was tentatively assigned to 5 DMF and 1 H2O, which was mainly established according to the elemental analysis
;


_vrf_CHEMW03_ZJNU-82             
;
PROBLEM:   The ratio of given/expected molecular weight as
            calculated from the _atom_site* data lies outside
            the range 0.90 <> 1.10
           From the CIF: _cell_formula_units_Z                    6
           From the CIF: _chemical_formula_weight           962.93
           TEST: Calculate formula weight from _atom_site_*
           atom     mass    num     sum
           C        12.01   23.00  276.25
           H         1.01   16.00   16.13
           Cu       63.55    2.00  127.09
           O        16.00   10.00  159.99
           N        14.01    0.00    0.00
           Calculated formula weight              579.46

RESPONSE: The empirical formula contains the lattice molecules.
;
####################################################################### 
# 
# 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-83
_database_code_depnum_ccdc_archive 'CCDC 1827030'
_audit_update_record             
;
2018-04-09 deposited with the CCDC.
2018-06-05 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 O10 [5DMF]'
_chemical_formula_sum            'C38 H51 Cu2 N5 O15'
_chemical_formula_weight         944.94

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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 0.3200 1.2650 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 '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      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                   18.4882(4)
_cell_length_b                   18.4882(4)
_cell_length_c                   23.4316(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     6936.2(4)
_cell_formula_units_Z            6
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    40995
_cell_measurement_theta_min      0.996
_cell_measurement_theta_max      27.49

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_F_000             2952
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.987
_shelx_estimated_absorpt_T_min   0.891
_shelx_estimated_absorpt_T_max   0.908
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.8947
_exptl_absorpt_correction_T_max  0.9112
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(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            40995
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_av_R_equivalents  0.0634
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.272
_diffrn_reflns_theta_max         27.490
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2968
_reflns_number_gt                1768
_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.
 
 _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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0950P)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         2968
_refine_ls_number_parameters     96
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0885
_refine_ls_R_factor_gt           0.0532
_refine_ls_wR_factor_ref         0.1670
_refine_ls_wR_factor_gt          0.1566
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001

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 0.52389(2) 0.47611(2) 0.04620(2) 0.0559(2) Uani 1 2 d S T P . .
O1 O 0.41031(13) 0.43910(14) 0.07316(10) 0.0707(6) Uani 1 1 d . . . . .
O2 O 0.37130(12) 0.48138(14) -0.00506(10) 0.0713(6) Uani 1 1 d . . . . .
O1W O 0.56130(14) 0.43870(14) 0.1245(2) 0.1365(17) Uani 1 2 d S T P . .
H1WA H 0.6117 0.4498 0.1215 0.164 Uiso 1 1 d R U . . .
C1 C 0.35961(19) 0.45024(19) 0.04393(15) 0.0604(8) Uani 1 1 d . . . . .
C2 C 0.27500(17) 0.42066(18) 0.06973(13) 0.0560(7) Uani 1 1 d . . . . .
C3 C 0.25146(18) 0.37325(19) 0.11871(13) 0.0637(8) Uani 1 1 d . . . . .
H3 H 0.2886 0.3580 0.1357 0.076 Uiso 1 1 calc R U . . .
C4 C 0.22146(13) 0.4429(3) 0.04431(17) 0.0582(10) Uani 1 2 d S T P . .
H4 H 0.2367 0.4734 0.0095 0.070 Uiso 1 2 calc R U P . .
C5 C 0.17353(14) 0.3471(3) 0.14399(18) 0.0643(11) Uani 1 2 d S T P . .
C6 C 0.16903(19) 0.3381(4) 0.2500 0.0590(14) Uani 1 4 d S T P . .
H6 H 0.1987 0.3974 0.2500 0.071 Uiso 1 4 calc R U P . .
C7 C 0.14882(13) 0.2976(3) 0.1992(2) 0.0651(11) Uani 1 2 d S T P . .
C8 C 0.1063(2) 0.2126(4) 0.1991(3) 0.167(4) Uani 1 2 d DS T P . .
C9 C 0.0834(4) 0.1667(7) 0.1440(5) 0.220(11) Uani 0.5 2 d DS T P . .
H8A H 0.0908 0.1820 0.1644 0.264 Uiso 0.5 2 d R U P A 2
H9A H 0.0538 0.1079 0.1504 0.264 Uiso 0.5 2 d R U P . .
H9B H 0.0486 0.1820 0.1228 0.264 Uiso 0.5 1 d R U P . .
C10 C 0.0857(3) 0.1713(6) 0.2500 0.230(9) Uani 1 4 d S T P . .
H10A H 0.0560 0.1120 0.2500 0.276 Uiso 1 4 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 O2 1.944(2) 10 ?
Cu1 O2 1.944(2) 13_665 ?
Cu1 O1 1.960(2) . ?
Cu1 O1 1.960(2) 22_665 ?
Cu1 O1W 2.192(4) . ?
Cu1 Cu1 2.6512(10) 13_665 ?
O1 C1 1.258(3) . ?
O2 C1 1.254(4) . ?
O2 Cu1 1.944(2) 13_665 ?
O1W H1WA 0.8514 . ?
C1 C2 1.502(4) . ?
C2 C3 1.376(4) . ?
C2 C4 1.383(3) . ?
C3 C5 1.401(4) . ?
C3 H3 0.9500 . ?
C4 C2 1.383(3) 20 ?
C4 H4 0.9500 . ?
C5 C3 1.401(4) 20 ?
C5 C7 1.516(6) . ?
C6 C7 1.355(5) 16_556 ?
C6 C7 1.355(5) . ?
C6 H6 0.9500 . ?
C7 C8 1.362(7) . ?
C8 C10 1.363(7) . ?
C8 C9 1.487(11) . ?
C8 H8A 0.9503 . ?
C9 H8A 0.5371 . ?
C9 H9A 0.9540 . ?
C9 H9B 0.9588 . ?
C10 C8 1.363(7) 16_556 ?
C10 H10A 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
O2 Cu1 O2 88.94(13) 10 13_665 ?
O2 Cu1 O1 89.04(10) 10 . ?
O2 Cu1 O1 168.11(9) 13_665 . ?
O2 Cu1 O1 168.12(9) 10 22_665 ?
O2 Cu1 O1 89.04(10) 13_665 22_665 ?
O1 Cu1 O1 90.53(14) . 22_665 ?
O2 Cu1 O1W 97.75(11) 10 . ?
O2 Cu1 O1W 97.75(11) 13_665 . ?
O1 Cu1 O1W 94.13(12) . . ?
O1 Cu1 O1W 94.12(12) 22_665 . ?
O2 Cu1 Cu1 83.75(7) 10 13_665 ?
O2 Cu1 Cu1 83.75(7) 13_665 13_665 ?
O1 Cu1 Cu1 84.38(7) . 13_665 ?
O1 Cu1 Cu1 84.38(7) 22_665 13_665 ?
O1W Cu1 Cu1 177.87(14) . 13_665 ?
C1 O1 Cu1 121.6(2) . . ?
C1 O2 Cu1 123.22(19) . 13_665 ?
Cu1 O1W H1WA 109.6 . . ?
O1 C1 O2 127.0(3) . . ?
O1 C1 C2 116.5(3) . . ?
O2 C1 C2 116.4(3) . . ?
C3 C2 C4 120.2(3) . . ?
C3 C2 C1 120.5(3) . . ?
C4 C2 C1 119.2(3) . . ?
C2 C3 C5 121.1(3) . . ?
C2 C3 H3 119.5 . . ?
C5 C3 H3 119.5 . . ?
C2 C4 C2 119.7(4) . 20 ?
C2 C4 H4 120.1 . . ?
C2 C4 H4 120.1 20 . ?
C3 C5 C3 117.6(4) . 20 ?
C3 C5 C7 121.1(2) . . ?
C3 C5 C7 121.1(2) 20 . ?
C7 C6 C7 123.0(6) 16_556 . ?
C7 C6 H6 118.5 16_556 . ?
C7 C6 H6 118.5 . . ?
C6 C7 C8 118.5(5) . . ?
C6 C7 C5 120.0(4) . . ?
C8 C7 C5 121.4(5) . . ?
C10 C8 C7 119.0(6) . . ?
C10 C8 C9 121.4(7) . . ?
C7 C8 C9 119.6(7) . . ?
C10 C8 H8A 119.9 . . ?
C7 C8 H8A 121.1 . . ?
C9 C8 H8A 1.5 . . ?
C8 C9 H8A 2.6 . . ?
C8 C9 H9A 110.5 . . ?
H8A C9 H9A 108.0 . . ?
C8 C9 H9B 109.0 . . ?
H8A C9 H9B 109.9 . . ?
H9A C9 H9B 109.2 . . ?
C8 C10 C8 122.0(8) 16_556 . ?
C8 C10 H10A 119.0 16_556 . ?
C8 C10 H10A 119.0 . . ?

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
Cu1 O1 C1 O2 3.2(5) . . . . ?
Cu1 O1 C1 C2 -178.80(18) . . . . ?
Cu1 O2 C1 O1 -2.3(5) 13_665 . . . ?
Cu1 O2 C1 C2 179.78(18) 13_665 . . . ?
O1 C1 C2 C3 -9.2(4) . . . . ?
O2 C1 C2 C3 169.0(3) . . . . ?
O1 C1 C2 C4 169.6(3) . . . . ?
O2 C1 C2 C4 -12.2(4) . . . . ?
C4 C2 C3 C5 -0.4(5) . . . . ?
C1 C2 C3 C5 178.4(3) . . . . ?
C3 C2 C4 C2 3.0(6) . . . 20 ?
C1 C2 C4 C2 -175.8(2) . . . 20 ?
C2 C3 C5 C3 -2.1(6) . . . 20 ?
C2 C3 C5 C7 -177.6(3) . . . . ?
C7 C6 C7 C8 -0.001(3) 16_556 . . . ?
C7 C6 C7 C5 180.000(2) 16_556 . . . ?
C3 C5 C7 C6 87.7(3) . . . . ?
C3 C5 C7 C6 -87.7(3) 20 . . . ?
C3 C5 C7 C8 -92.3(3) . . . . ?
C3 C5 C7 C8 92.3(3) 20 . . . ?
C6 C7 C8 C10 0.000(1) . . . . ?
C5 C7 C8 C10 180.000(1) . . . . ?
C6 C7 C8 C9 179.999(1) . . . . ?
C5 C7 C8 C9 -0.002(2) . . . . ?
C9 C8 C10 C8 180.002(3) . . . 16_556 ?

_refine_diff_density_max         0.366
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.070




# SQUEEZE RESULTS (APPEND TO CIF)
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 -0.038 -0.027 -0.002 4236.3 736.2
_platon_squeeze_details          
; The residual electron density of 736.2 electrons per unit cell was tentatively assigned to 5 DMF, which was mainly established according to the elemental analysis
;


_vrf_CHEMW03_ZJNU-83             
;
PROBLEM:  The ratio of given/expected molecular weight as
            calculated from the _atom_site* data lies outside
            the range 0.90 <> 1.10
           From the CIF: _cell_formula_units_Z                    6
           From the CIF: _chemical_formula_weight           944.94
           TEST: Calculate formula weight from _atom_site_*
           atom     mass    num     sum
           C        12.01   23.00  276.25
           H         1.01   16.00   16.13
           Cu       63.55    2.00  127.09
           O        16.00   10.00  159.99
           N        14.01    0.00    0.00
           Calculated formula weight              579.46

RESPONSE: The empirical formula contains the lattice molecules.
;
