# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_JXNU-16F
_database_code_depnum_ccdc_archive 'CCDC 2216657'
loop_
_audit_author_name
_audit_author_address
'Qing-Yan Liu'
;Jiangxi Normal University
China
;
_audit_update_record             
;
2022-12-08 deposited with the CCDC.	2023-01-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C46 H20 Cu2 F8 N2 O8, 4[C3H7NO], 5[H2O]'
_chemical_formula_sum            'C58 H58 Cu2 F8 N6 O17'
_chemical_formula_weight         1390.18

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
F F 0.0171 0.0103 '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'

_space_group_crystal_system      cubic
_space_group_IT_number           223
_space_group_name_H-M_alt        'P m -3 n'
_space_group_name_Hall           '-P 4n 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'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'x+1/2, z+1/2, -y+1/2'
'-x+1/2, z+1/2, y+1/2'
'-x+1/2, -z+1/2, -y+1/2'
'x+1/2, -z+1/2, y+1/2'
'z+1/2, y+1/2, -x+1/2'
'z+1/2, -y+1/2, x+1/2'
'-z+1/2, y+1/2, x+1/2'
'-z+1/2, -y+1/2, -x+1/2'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-y-1/2, -x-1/2, z-1/2'
'y-1/2, x-1/2, z-1/2'
'-y-1/2, x-1/2, -z-1/2'
'y-1/2, -x-1/2, -z-1/2'
'-x-1/2, -z-1/2, y-1/2'
'x-1/2, -z-1/2, -y-1/2'
'x-1/2, z-1/2, y-1/2'
'-x-1/2, z-1/2, -y-1/2'
'-z-1/2, -y-1/2, x-1/2'
'-z-1/2, y-1/2, -x-1/2'
'z-1/2, -y-1/2, -x-1/2'
'z-1/2, y-1/2, x-1/2'

_cell_length_a                   27.5946(3)
_cell_length_b                   27.5946(3)
_cell_length_c                   27.5946(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     21012.2(7)
_cell_formula_units_Z            6
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5207
_cell_measurement_theta_min      3.6190
_cell_measurement_theta_max      25.3510

_exptl_crystal_description       polyhedron
_exptl_crystal_colour            BLUE
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    0.659
_exptl_crystal_F_000             4284
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.347
_shelx_estimated_absorpt_T_min   0.956
_shelx_estimated_absorpt_T_max   0.966
_exptl_absorpt_correction_T_min  0.84261
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, EosS2'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            EosS2
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19530
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.383
_diffrn_reflns_theta_max         26.363
_diffrn_reflns_theta_full        26.000
_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             3815
_reflns_number_gt                2650
_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       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXT 2015 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2005)'
_computing_publication_material  'DIAMOND (Brandenburg, 2005)'
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1195P)²+3.2221P] 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_number_reflns         3815
_refine_ls_number_parameters     125
_refine_ls_number_restraints     157
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_gt           0.0590
_refine_ls_wR_factor_ref         0.2005
_refine_ls_wR_factor_gt          0.1823
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.186
_refine_ls_shift/su_max          0.001
_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 0.000000 0.70257(2) 0.500000 0.0430(2) Uani 1 4 d S T P B .
O1 O 0.05042(6) 0.70984(6) 0.55029(7) 0.0652(5) Uani 1 1 d . . . . .
C1 C 0.06465(9) 0.750000 0.56465(9) 0.0530(8) Uani 1 2 d S T P . .
C2 C 0.10327(9) 0.750000 0.60327(9) 0.0617(9) Uani 1 2 d DS T P . .
F1 F 0.1492(4) 0.8052(4) 0.5618(4) 0.266(7) Uani 0.5 1 d D U P A 1
C3 C 0.1390(4) 0.7820(3) 0.6054(4) 0.117(4) Uani 0.5 1 d D U P A 1
C4 C 0.1765(4) 0.7808(4) 0.6380(3) 0.108(4) Uani 0.5 1 d D U P A 1
H4 H 0.202665 0.801569 0.633851 0.130 Uiso 0.5 1 calc R U P A 1
C5 C 0.17596(9) 0.750000 0.67596(9) 0.0669(11) Uani 1 2 d DS T P . .
C6 C 0.21397(9) 0.750000 0.71397(9) 0.0725(12) Uani 1 2 d S T P A .
C7 C 0.250000 0.78529(9) 0.71471(9) 0.0748(12) Uani 1 2 d S T P . .
H7 H 0.250000 0.809120 0.690880 0.090 Uiso 1 2 calc R U P A .
N1 N 0.000000 0.62658(14) 0.500000 0.0583(10) Uani 1 4 d DS T P . .
F1A F 0.1612(2) 0.7768(3) 0.54968(18) 0.130(3) Uani 0.5 1 d D U P A 2
C3A C 0.1505(2) 0.7618(3) 0.5948(2) 0.0643(19) Uani 0.5 1 d D U P A 2
C4A C 0.1871(3) 0.7612(3) 0.6286(3) 0.072(2) Uani 0.5 1 d D U P A 2
H4A H 0.218814 0.768311 0.619595 0.087 Uiso 0.5 1 calc R U P A 2
C8 C 0.000000 0.52676(18) 0.500000 0.0756(16) Uani 1 4 d DS T P . .
C9 C 0.000000 0.6031(3) 0.4614(3) 0.112(3) Uani 0.55 2 d DS TU P B 1
H9 H 0.000000 0.620445 0.432536 0.134 Uiso 0.55 2 calc R U P B 1
C10 C 0.000000 0.5524(3) 0.4584(3) 0.121(3) Uani 0.55 2 d DS TU P B 1
H10 H 0.000000 0.536827 0.428522 0.145 Uiso 0.55 2 calc R U P B 1
C9A C -0.0377(4) 0.6027(3) 0.500000 0.116(4) Uani 0.45 2 d DS TU P B 2
H9A H -0.066718 0.619753 0.500000 0.139 Uiso 0.45 2 calc R U P B 2
C10A C -0.0406(4) 0.5516(4) 0.500000 0.127(4) Uani 0.45 2 d DS TU P B 2
H10A H -0.070499 0.535979 0.500000 0.153 Uiso 0.45 2 calc R U P B 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 O1 1.9752(17) 3_556 ?
Cu1 O1 1.9752(17) 28 ?
Cu1 O1 1.9752(17) 26_556 ?
Cu1 O1 1.9752(17) . ?
Cu1 N1 2.097(4) . ?
Cu1 Cu1 2.6174(9) 45_676 ?
O1 C1 1.241(2) . ?
C1 C2 1.507(5) . ?
C2 C3 1.325(8) 22_465 ?
C2 C3 1.325(8) . ?
C2 C3A 1.364(7) . ?
C2 C3A 1.364(7) 22_465 ?
F1 C3 1.392(10) . ?
C3 C4 1.370(10) . ?
C4 C5 1.349(8) . ?
C4 H4 0.9300 . ?
C5 C4A 1.379(7) 22_465 ?
C5 C4A 1.379(7) . ?
C5 C6 1.483(5) . ?
C6 C7 1.392(2) . ?
C6 C7 1.392(2) 10_656 ?
C7 H7 0.9300 . ?
N1 C9A 1.231(10) . ?
N1 C9A 1.231(10) 3_556 ?
N1 C9 1.247(8) 26_556 ?
N1 C9 1.247(8) . ?
F1A C3A 1.346(7) . ?
C3A C4A 1.373(8) . ?
C4A H4A 0.9300 . ?
C8 C10A 1.314(11) . ?
C8 C10A 1.314(11) 3_556 ?
C8 C10 1.348(9) 26_556 ?
C8 C10 1.348(9) . ?
C8 C8 1.477(10) 25_566 ?
C9 C10 1.401(10) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C9A C10A 1.411(12) . ?
C9A H9A 0.9300 . ?
C10A H10A 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 O1 89.27(11) 3_556 28 ?
O1 Cu1 O1 89.55(11) 3_556 26_556 ?
O1 Cu1 O1 168.34(10) 28 26_556 ?
O1 Cu1 O1 168.34(10) 3_556 . ?
O1 Cu1 O1 89.55(11) 28 . ?
O1 Cu1 O1 89.27(11) 26_556 . ?
O1 Cu1 N1 95.83(5) 3_556 . ?
O1 Cu1 N1 95.83(5) 28 . ?
O1 Cu1 N1 95.83(5) 26_556 . ?
O1 Cu1 N1 95.83(5) . . ?
O1 Cu1 Cu1 84.17(5) 3_556 45_676 ?
O1 Cu1 Cu1 84.17(5) 28 45_676 ?
O1 Cu1 Cu1 84.17(5) 26_556 45_676 ?
O1 Cu1 Cu1 84.17(5) . 45_676 ?
N1 Cu1 Cu1 180.0 . 45_676 ?
C1 O1 Cu1 122.56(18) . . ?
O1 C1 O1 126.5(3) . 22_465 ?
O1 C1 C2 116.73(16) . . ?
O1 C1 C2 116.73(16) 22_465 . ?
C3 C2 C3 112.2(8) 22_465 . ?
C3 C2 C3A 30.4(6) 22_465 22_465 ?
C3 C2 C3A 104.1(4) . 22_465 ?
C3 C2 C1 123.9(4) 22_465 . ?
C3 C2 C1 123.9(4) . . ?
C3A C2 C1 123.7(3) . . ?
C3A C2 C1 123.7(3) 22_465 . ?
C2 C3 C4 125.1(7) . . ?
C2 C3 F1 114.7(8) . . ?
C4 C3 F1 115.2(8) . . ?
C5 C4 C3 121.1(8) . . ?
C5 C4 H4 119.4 . . ?
C3 C4 H4 119.4 . . ?
C4 C5 C4 114.3(8) 22_465 . ?
C4 C5 C4A 28.3(6) 22_465 22_465 ?
C4 C5 C4A 108.9(4) . 22_465 ?
C4A C5 C4A 118.3(7) 22_465 . ?
C4 C5 C6 122.8(4) 22_465 . ?
C4 C5 C6 122.8(4) . . ?
C4A C5 C6 120.9(4) 22_465 . ?
C4A C5 C6 120.9(4) . . ?
C7 C6 C7 117.9(4) . 10_656 ?
C7 C6 C5 121.03(19) . . ?
C7 C6 C5 121.03(19) 10_656 . ?
C6 C7 C6 122.1(4) . 7_665 ?
C6 C7 H7 119.0 . . ?
C6 C7 H7 119.0 7_665 . ?
C9 N1 C9 117.3(8) 26_556 . ?
C9A N1 Cu1 122.4(5) . . ?
C9A N1 Cu1 122.4(5) 3_556 . ?
C9 N1 Cu1 121.3(4) 26_556 . ?
C9 N1 Cu1 121.3(4) . . ?
F1A C3A C2 116.1(5) . . ?
F1A C3A C4A 118.0(6) . . ?
C2 C3A C4A 125.8(6) . . ?
C3A C4A C5 118.8(7) . . ?
C3A C4A H4A 120.6 . . ?
C5 C4A H4A 120.6 . . ?
C10A C8 C10A 117.1(10) . 3_556 ?
C10 C8 C10 116.7(8) 26_556 . ?
C10 C8 C8 121.6(4) 26_556 25_566 ?
C10 C8 C8 121.6(4) . 25_566 ?
N1 C9 C10 124.7(8) . . ?
N1 C9 H9 117.6 . . ?
C10 C9 H9 117.6 . . ?
C8 C10 C9 118.3(7) . . ?
C8 C10 H10 120.9 . . ?
C9 C10 H10 120.9 . . ?
N1 C9A C10A 125.7(10) . . ?
N1 C9A H9A 117.1 . . ?
C10A C9A H9A 117.1 . . ?
C8 C10A C9A 118.1(10) . . ?
C8 C10A H10A 120.9 . . ?
C9A C10A H10A 120.9 . . ?

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 O1 -0.10(8) . . . 22_465 ?
Cu1 O1 C1 C2 179.90(8) . . . . ?
O1 C1 C2 C3 -36.7(7) . . . 22_465 ?
O1 C1 C2 C3 143.3(7) 22_465 . . 22_465 ?
O1 C1 C2 C3 143.3(7) . . . . ?
O1 C1 C2 C3 -36.7(7) 22_465 . . . ?
O1 C1 C2 C3A 106.5(4) . . . . ?
O1 C1 C2 C3A -73.5(4) 22_465 . . . ?
O1 C1 C2 C3A -73.5(4) . . . 22_465 ?
O1 C1 C2 C3A 106.5(4) 22_465 . . 22_465 ?
C3 C2 C3 C4 4.9(9) 22_465 . . . ?
C1 C2 C3 C4 -175.1(9) . . . . ?
C3 C2 C3 F1 158.6(14) 22_465 . . . ?
C1 C2 C3 F1 -21.4(14) . . . . ?
C2 C3 C4 C5 -10.0(19) . . . . ?
F1 C3 C4 C5 -163.6(11) . . . . ?
C3 C4 C5 C4 4.5(8) . . . 22_465 ?
C3 C4 C5 C6 -175.5(8) . . . . ?
C4 C5 C6 C7 -173.8(6) 22_465 . . . ?
C4 C5 C6 C7 6.2(6) . . . . ?
C4A C5 C6 C7 -140.4(4) 22_465 . . . ?
C4A C5 C6 C7 39.6(4) . . . . ?
C4 C5 C6 C7 6.2(6) 22_465 . . 10_656 ?
C4 C5 C6 C7 -173.8(6) . . . 10_656 ?
C4A C5 C6 C7 39.6(4) 22_465 . . 10_656 ?
C4A C5 C6 C7 -140.4(4) . . . 10_656 ?
C7 C6 C7 C6 0.000(2) 10_656 . . 7_665 ?
C5 C6 C7 C6 180.000(1) . . . 7_665 ?
C3A C2 C3A F1A -175.9(9) 22_465 . . . ?
C1 C2 C3A F1A 4.1(9) . . . . ?
C3A C2 C3A C4A 1.5(6) 22_465 . . . ?
C1 C2 C3A C4A -178.5(6) . . . . ?
F1A C3A C4A C5 174.4(7) . . . . ?
C2 C3A C4A C5 -3.0(12) . . . . ?
C4A C5 C4A C3A 1.4(6) 22_465 . . . ?
C6 C5 C4A C3A -178.6(6) . . . . ?
C9 N1 C9 C10 0.000(3) 26_556 . . . ?
Cu1 N1 C9 C10 180.000(2) . . . . ?
C10 C8 C10 C9 0.000(3) 26_556 . . . ?
C8 C8 C10 C9 180.000(2) 25_566 . . . ?
N1 C9 C10 C8 0.000(3) . . . . ?
C9A N1 C9A C10A 0.0 3_556 . . . ?
Cu1 N1 C9A C10A 180.0 . . . . ?
C10A C8 C10A C9A 0.0 3_556 . . . ?
C8 C8 C10A C9A 180.0 25_566 . . . ?
N1 C9A C10A C8 0.0 . . . . ?

_refine_diff_density_max         0.634
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.045




# start Validation Reply Form
_vrf_PLAT910_JXNU-16F            
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         14 Note  
RESPONSE:  It may be relevant for SQUEEZE modelling refinement technique.
;
# end Validation Reply Form
