# Supplementary Information (SI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2025

####################################################################### 
# 
# 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_SUM-23A
_database_code_depnum_ccdc_archive 'CCDC 2410552'
loop_
_audit_author_name
_audit_author_address
'Chong Liu'
;Sichuan University
China
;
_audit_update_record             
;
2025-01-25 deposited with the CCDC.	2025-02-09 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT420_SUM-23A             
;
PROBLEM: D-H Bond Without Acceptor  O6A      --H6AA     .     Please Check
RESPONSE: The water molecule containing O6A/H6AA/H6AB could form hydrogen bonds with other solvent molecules in the lattice that cannot be crystallographically located.
;
_vrf_PLAT420_SUM-23A_2           
;
PROBLEM: D-H Bond Without Acceptor  O6A      --H6AB     .     Please Check
RESPONSE: The water molecule containing O6A/H6AA/H6AB could form hydrogen bonds with other solvent molecules in the lattice that cannot be crystallographically located.
;
_vrf_PLAT420_SUM-23A_3           
;
PROBLEM: D-H Bond Without Acceptor  O6       --H6A      .     Please Check
RESPONSE: The water molecule containing O6/H6A/H6B could form hydrogen bonds with other solvent molecules in the lattice that cannot be crystallographically located.
;
_vrf_PLAT420_SUM-23A_4           
;
PROBLEM: D-H Bond Without Acceptor  O6       --H6B      .     Please Check
RESPONSE: The water molecule containing O6/H6A/H6B could form hydrogen bonds with other solvent molecules in the lattice that cannot be crystallographically located.
;
# Added during the CSD deposition process: Monday 16 December 2024 10:43 AM
# end Validation Reply Form

_audit_creation_date             2024-12-14
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        SUM-23A
_chemical_formula_moiety         'C48 H40 Cu10 N16 O20, H4 O2'
_chemical_formula_sum            'C48 H44 Cu10 N16 O22'
_chemical_formula_weight         1832.39
_chemical_absolute_configuration ?
_chemical_melting_point          ?
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'
N N 0.0311 0.0180 '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'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           120
_space_group_name_H-M_alt        'I -4 c 2'
_space_group_name_Hall           'I -4 -2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'x, -y, z+1/2'
'-x, y, z+1/2'
'y, x, -z+1/2'
'-y, -x, -z+1/2'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1'
'-x+1/2, y+1/2, z+1'
'y+1/2, x+1/2, -z+1'
'-y+1/2, -x+1/2, -z+1'

_cell_length_a                   23.1107(2)
_cell_length_b                   23.1107(2)
_cell_length_c                   18.0067(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9617.5(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9752
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      79.58
_cell_measurement_theta_min      4.93
_shelx_estimated_absorpt_T_max   0.764
_shelx_estimated_absorpt_T_min   0.708
_exptl_absorpt_coefficient_mu    2.849
_exptl_absorpt_correction_T_max  0.7543
_exptl_absorpt_correction_T_min  0.6606
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0664 before and 0.0551 after correction.
The Ratio of minimum to maximum transmission is 0.8758.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3640
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_unetI/netI     0.0148
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            74193
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         80.010
_diffrn_reflns_theta_min         2.704
_diffrn_ambient_temperature      193.0
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_diffrn_source_current           1.1
_diffrn_source_power             0.055
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.854
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.971
_reflns_number_gt                4958
_reflns_number_total             5155
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'APEX4 V2022.1-1 (Bruker, 2022)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.727
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.05(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         5155
_refine_ls_number_restraints     32
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0338
_refine_ls_restrained_S_all      1.098
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0458P)²+21.1737P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0922
_refine_ls_wR_factor_ref         0.0930
_refine_special_details          
'Refined as a 2-component inversion twin.,SQUEEZE'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.95(4)
 0.05(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Restrained distances
 Cu2-O6 \\sim Cu2-O6A
 with sigma of 0.02
 Cu1-O7 \\sim Cu1-O7A
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
O7 \\sim O7A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
O6A \\sim O6: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
Uanis(O7) \\sim Ueq, Uanis(O7A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O6A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
5. Others
 Fixed Sof: O6A(0.5) H6AA(0.5) H6AB(0.5) O7(0.25) H7A(0.25) H7B(0.25) O6(0.5)
 H6A(0.5) H6B(0.5) O7A(0.25) H7AA(0.25) H7AB(0.25)
6.a Riding coordinates:
 O6A(H6AA,H6AB), O7(H7A,H7B), O6(H6A,H6B), O7A(H7AA,H7AB)
6.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C9(H9), C3(H3), C6(H6), C11(H11), C12(H12), C4(H4), C5(H5)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.500000 0.500000 0.500000 0.0232(3) Uani 1 4 d DS T P . .
Cu4 Cu 1.000000 0.500000 0.250000 0.0281(3) Uani 1 4 d S T P . .
Cu3 Cu 0.87849(3) 0.56627(3) 0.27174(4) 0.03205(18) Uani 1 1 d . . . . .
Cu2 Cu 0.54108(3) 0.63113(3) 0.48052(4) 0.02903(17) Uani 1 1 d D . . . .
O4 O 0.95771(11) 0.57141(13) 0.2408(2) 0.0299(7) Uani 1 1 d . . . . .
O1 O 0.56483(11) 0.55356(12) 0.5067(2) 0.0287(6) Uani 1 1 d . . . . .
O2 O 0.60980(13) 0.62608(13) 0.4194(2) 0.0356(8) Uani 1 1 d . . . . .
O3 O 0.89972(15) 0.63702(14) 0.3235(2) 0.0420(9) Uani 1 1 d . . . . .
N4 N 1.01303(16) 0.79927(16) 0.4265(2) 0.0344(9) Uani 1 1 d . . . . .
N1 N 0.61629(15) 0.53539(15) 0.4702(2) 0.0287(8) Uani 1 1 d . . . . .
N3 N 0.98613(16) 0.62050(14) 0.2682(3) 0.0333(9) Uani 1 1 d . . . . .
N2 N 0.79851(16) 0.56568(17) 0.3148(3) 0.0382(10) Uani 1 1 d . . . . .
C8 C 0.9760(2) 0.7020(2) 0.3501(3) 0.0386(12) Uani 1 1 d . . . . .
C2 C 0.69233(17) 0.57088(18) 0.3890(3) 0.0297(9) Uani 1 1 d . . . . .
C7 C 0.9515(2) 0.64970(18) 0.3117(3) 0.0363(11) Uani 1 1 d . . . . .
C1 C 0.63608(18) 0.57758(18) 0.4285(3) 0.0279(9) Uani 1 1 d . . . . .
C10 C 0.9591(2) 0.7941(2) 0.4045(4) 0.0460(13) Uani 1 1 d . . . . .
H10 H 0.932969 0.824604 0.415659 0.055 Uiso 1 1 calc R U . . .
C9 C 0.9385(2) 0.7470(3) 0.3663(4) 0.0551(17) Uani 1 1 d . . . . .
H9 H 0.899163 0.745323 0.351255 0.066 Uiso 1 1 calc R U . . .
C3 C 0.7256(2) 0.5210(2) 0.3877(4) 0.0485(14) Uani 1 1 d . . . . .
H3 H 0.711880 0.486916 0.411349 0.058 Uiso 1 1 calc R U . . .
O6A O 0.6020(12) 0.6780(10) 0.5645(12) 0.066(5) Uani 0.5 1 d D U P A 2
H6AA H 0.620025 0.714649 0.557856 0.099 Uiso 0.5 1 d R U P A 2
H6AB H 0.614635 0.665839 0.612506 0.099 Uiso 0.5 1 d R U P A 2
C6 C 0.7139(2) 0.6181(2) 0.3501(4) 0.0540(17) Uani 1 1 d . . . . .
H6 H 0.692259 0.652958 0.347473 0.065 Uiso 1 1 calc R U . . .
C11 C 1.0495(2) 0.7561(3) 0.4105(4) 0.0578(18) Uani 1 1 d . . . . .
H11 H 1.088592 0.758733 0.426398 0.069 Uiso 1 1 calc R U . . .
C12 C 1.0321(3) 0.7082(3) 0.3717(5) 0.0598(18) Uani 1 1 d . . . . .
H12 H 1.059455 0.678903 0.359870 0.072 Uiso 1 1 calc R U . . .
C4 C 0.7783(2) 0.5204(2) 0.3524(4) 0.0466(13) Uani 1 1 d . . . . .
H4 H 0.801199 0.486346 0.354942 0.056 Uiso 1 1 calc R U . . .
C5 C 0.7672(2) 0.6140(2) 0.3151(5) 0.065(2) Uani 1 1 d . . . . .
H5 H 0.781965 0.647099 0.290283 0.078 Uiso 1 1 calc R U . . .
O7 O 0.4910(16) 0.4729(9) 0.3656(9) 0.052(6) Uani 0.25 1 d D U P B 1
H7A H 0.458775 0.478102 0.341511 0.078 Uiso 0.25 1 d R U P B 1
H7B H 0.517645 0.474272 0.331491 0.078 Uiso 0.25 1 d R U P B 1
O6 O 0.5964(12) 0.6583(10) 0.5824(12) 0.073(6) Uani 0.5 1 d D U P A 1
H6A H 0.592168 0.646276 0.636989 0.110 Uiso 0.5 1 d R U P A 1
H6B H 0.630908 0.686086 0.583249 0.110 Uiso 0.5 1 d R U P A 1
O7A O 0.5091(12) 0.5085(11) 0.3641(7) 0.030(5) Uani 0.25 1 d D U P C 2
H7AA H 0.484294 0.536413 0.358144 0.045 Uiso 0.25 1 d R U P C 2
H7AB H 0.539364 0.514803 0.336614 0.045 Uiso 0.25 1 d R U P C 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 1.947(3) . ?
Cu1 O1 1.947(3) 3_566 ?
Cu1 O1 1.947(3) 2_665 ?
Cu1 O1 1.947(3) 4_656 ?
Cu4 O4 1.925(3) . ?
Cu4 O4 1.925(3) 2_765 ?
Cu4 O4 1.925(3) 11_565 ?
Cu4 O4 1.925(3) 12_645 ?
Cu3 O4 1.917(3) . ?
Cu3 O3 1.945(3) . ?
Cu3 N3 1.987(4) 12_645 ?
Cu3 N2 2.004(4) . ?
Cu2 O1 1.933(3) . ?
Cu2 O2 1.936(3) . ?
Cu2 N4 1.988(4) 13_464 ?
Cu2 N1 2.007(4) 4_656 ?
Cu2 O6A 2.333(14) . ?
Cu2 O6 2.322(15) . ?
O4 N3 1.401(4) . ?
O1 N1 1.422(5) . ?
O2 C1 1.285(5) . ?
O3 C7 1.251(6) . ?
N4 C10 1.312(7) . ?
N4 C11 1.338(7) . ?
N1 C1 1.312(6) . ?
N3 C7 1.307(6) . ?
N2 C4 1.331(7) . ?
N2 C5 1.330(7) . ?
C8 C7 1.502(6) . ?
C8 C9 1.385(7) . ?
C8 C12 1.362(8) . ?
C2 C1 1.490(6) . ?
C2 C3 1.387(7) . ?
C2 C6 1.388(7) . ?
C10 H10 0.9500 . ?
C10 C9 1.373(8) . ?
C9 H9 0.9500 . ?
C3 H3 0.9500 . ?
C3 C4 1.373(7) . ?
O6A H6AA 0.9522 . ?
O6A H6AB 0.9536 . ?
C6 H6 0.9500 . ?
C6 C5 1.387(7) . ?
C11 H11 0.9500 . ?
C11 C12 1.369(8) . ?
C12 H12 0.9500 . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
O7 O7 1.32(4) 2_665 ?
O7 H7A 0.8698 . ?
O7 H7B 0.8697 . ?
O6 H6A 1.0265 . ?
O6 H6B 1.0248 . ?
O7A O7A 0.57(4) 2_665 ?
O7A H7AA 0.8705 . ?
O7A H7AB 0.8699 . ?

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 172.9(2) . 2_665 ?
O1 Cu1 O1 90.218(14) 2_665 4_656 ?
O1 Cu1 O1 90.220(14) . 4_656 ?
O1 Cu1 O1 90.216(14) . 3_566 ?
O1 Cu1 O1 90.218(14) 2_665 3_566 ?
O1 Cu1 O1 172.9(2) 3_566 4_656 ?
O4 Cu4 O4 90.425(19) . 11_565 ?
O4 Cu4 O4 90.426(18) 12_645 2_765 ?
O4 Cu4 O4 170.1(2) . 2_765 ?
O4 Cu4 O4 90.428(19) . 12_645 ?
O4 Cu4 O4 170.1(2) 11_565 12_645 ?
O4 Cu4 O4 90.426(19) 11_565 2_765 ?
O4 Cu3 O3 81.16(13) . . ?
O4 Cu3 N3 86.63(13) . 12_645 ?
O4 Cu3 N2 173.39(18) . . ?
O3 Cu3 N3 162.58(15) . 12_645 ?
O3 Cu3 N2 93.04(15) . . ?
N3 Cu3 N2 98.31(16) 12_645 . ?
O1 Cu2 O2 81.35(13) . . ?
O1 Cu2 N4 164.15(17) . 13_464 ?
O1 Cu2 N1 89.07(13) . 4_656 ?
O1 Cu2 O6A 95.8(6) . . ?
O1 Cu2 O6 84.4(6) . . ?
O2 Cu2 N4 92.19(15) . 13_464 ?
O2 Cu2 N1 164.47(15) . 4_656 ?
O2 Cu2 O6A 84.3(8) . . ?
O2 Cu2 O6 90.8(8) . . ?
N4 Cu2 N1 93.87(15) 13_464 4_656 ?
N4 Cu2 O6A 98.0(6) 13_464 . ?
N4 Cu2 O6 110.3(6) 13_464 . ?
N1 Cu2 O6A 108.9(7) 4_656 . ?
N1 Cu2 O6 100.4(8) 4_656 . ?
Cu3 O4 Cu4 113.99(15) . . ?
N3 O4 Cu4 115.2(2) . . ?
N3 O4 Cu3 113.3(2) . . ?
Cu2 O1 Cu1 110.85(13) . . ?
N1 O1 Cu1 115.3(2) . . ?
N1 O1 Cu2 113.5(2) . . ?
C1 O2 Cu2 111.6(3) . . ?
C7 O3 Cu3 110.9(3) . . ?
C10 N4 Cu2 122.0(3) . 13_564 ?
C10 N4 C11 117.7(4) . . ?
C11 N4 Cu2 120.3(4) . 13_564 ?
O1 N1 Cu2 101.4(2) . 3_566 ?
C1 N1 Cu2 147.9(3) . 3_566 ?
C1 N1 O1 109.6(3) . . ?
O4 N3 Cu3 108.6(2) . 11_565 ?
C7 N3 Cu3 141.4(3) . 11_565 ?
C7 N3 O4 110.0(3) . . ?
C4 N2 Cu3 121.7(3) . . ?
C4 N2 C5 117.8(4) . . ?
C5 N2 Cu3 119.9(3) . . ?
C9 C8 C7 117.8(5) . . ?
C12 C8 C7 125.1(4) . . ?
C12 C8 C9 117.1(5) . . ?
C3 C2 C1 125.4(4) . . ?
C3 C2 C6 116.5(4) . . ?
C6 C2 C1 118.2(4) . . ?
O3 C7 N3 124.5(4) . . ?
O3 C7 C8 118.1(4) . . ?
N3 C7 C8 117.4(4) . . ?
O2 C1 N1 123.8(4) . . ?
O2 C1 C2 116.2(4) . . ?
N1 C1 C2 120.0(4) . . ?
N4 C10 H10 118.2 . . ?
N4 C10 C9 123.5(5) . . ?
C9 C10 H10 118.2 . . ?
C8 C9 H9 120.5 . . ?
C10 C9 C8 119.0(5) . . ?
C10 C9 H9 120.5 . . ?
C2 C3 H3 119.7 . . ?
C4 C3 C2 120.5(5) . . ?
C4 C3 H3 119.7 . . ?
Cu2 O6A H6AA 126.5 . . ?
Cu2 O6A H6AB 129.5 . . ?
H6AA O6A H6AB 104.0 . . ?
C2 C6 H6 120.2 . . ?
C5 C6 C2 119.6(5) . . ?
C5 C6 H6 120.2 . . ?
N4 C11 H11 119.0 . . ?
N4 C11 C12 121.9(5) . . ?
C12 C11 H11 119.0 . . ?
C8 C12 C11 120.7(5) . . ?
C8 C12 H12 119.7 . . ?
C11 C12 H12 119.7 . . ?
N2 C4 C3 122.6(5) . . ?
N2 C4 H4 118.7 . . ?
C3 C4 H4 118.7 . . ?
N2 C5 C6 122.9(5) . . ?
N2 C5 H5 118.6 . . ?
C6 C5 H5 118.6 . . ?
O7 O7 H7A 98.1 2_665 . ?
O7 O7 H7B 75.1 2_665 . ?
H7A O7 H7B 104.5 . . ?
Cu2 O6 H6A 129.2 . . ?
Cu2 O6 H6B 127.6 . . ?
H6A O6 H6B 103.2 . . ?
O7A O7A H7AA 91.3 2_665 . ?
O7A O7A H7AB 134.7 2_665 . ?
H7AA O7A H7AB 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
Cu1 O1 N1 Cu2 -56.8(3) . . . 3_566 ?
Cu1 O1 N1 C1 131.3(3) . . . . ?
Cu4 O4 N3 Cu3 48.6(3) . . . 11_565 ?
Cu4 O4 N3 C7 -130.8(4) . . . . ?
Cu3 O4 N3 Cu3 -177.68(18) . . . 11_565 ?
Cu3 O4 N3 C7 2.9(5) . . . . ?
Cu3 O3 C7 N3 2.4(7) . . . . ?
Cu3 O3 C7 C8 -177.5(4) . . . . ?
Cu3 N3 C7 O3 177.3(4) 11_565 . . . ?
Cu3 N3 C7 C8 -2.8(9) 11_565 . . . ?
Cu3 N2 C4 C3 174.3(5) . . . . ?
Cu3 N2 C5 C6 -173.8(6) . . . . ?
Cu2 O1 N1 Cu2 173.83(16) . . . 3_566 ?
Cu2 O1 N1 C1 1.9(4) . . . . ?
Cu2 O2 C1 N1 4.5(6) . . . . ?
Cu2 O2 C1 C2 -175.0(3) . . . . ?
Cu2 N4 C10 C9 179.1(6) 13_564 . . . ?
Cu2 N4 C11 C12 -178.3(6) 13_564 . . . ?
Cu2 N1 C1 O2 -169.3(4) 3_566 . . . ?
Cu2 N1 C1 C2 10.2(9) 3_566 . . . ?
O4 N3 C7 O3 -3.6(8) . . . . ?
O4 N3 C7 C8 176.3(4) . . . . ?
O1 N1 C1 O2 -4.3(6) . . . . ?
O1 N1 C1 C2 175.2(4) . . . . ?
N4 C10 C9 C8 0.4(11) . . . . ?
N4 C11 C12 C8 -2.1(13) . . . . ?
C2 C3 C4 N2 -3.8(10) . . . . ?
C2 C6 C5 N2 2.3(12) . . . . ?
C7 C8 C9 C10 176.9(6) . . . . ?
C7 C8 C12 C11 -176.0(7) . . . . ?
C1 C2 C3 C4 -176.8(5) . . . . ?
C1 C2 C6 C5 177.5(6) . . . . ?
C10 N4 C11 C12 0.8(11) . . . . ?
C9 C8 C7 O3 -29.8(9) . . . . ?
C9 C8 C7 N3 150.3(6) . . . . ?
C9 C8 C12 C11 2.5(12) . . . . ?
C3 C2 C1 O2 -175.8(5) . . . . ?
C3 C2 C1 N1 4.7(8) . . . . ?
C3 C2 C6 C5 -2.4(10) . . . . ?
C6 C2 C1 O2 4.4(7) . . . . ?
C6 C2 C1 N1 -175.1(5) . . . . ?
C6 C2 C3 C4 3.1(9) . . . . ?
C11 N4 C10 C9 0.1(10) . . . . ?
C12 C8 C7 O3 148.7(7) . . . . ?
C12 C8 C7 N3 -31.2(9) . . . . ?
C12 C8 C9 C10 -1.7(11) . . . . ?
C4 N2 C5 C6 -2.7(12) . . . . ?
C5 N2 C4 C3 3.5(10) . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 1094 electrons were 
found in a volume of 4366Å³ in 1 void per unit cell. 
This is consistent with the presence of 27.4[H2O] per Formula Unit 
which account for 1095 electrons per unit cell.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.230 -0.364 -0.079 4361.1 1094.4 '109.5 H2O'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.95(4)
2 0.05(4)

####################################################################### 
# 
# 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_SUM-33
_database_code_depnum_ccdc_archive 'CCDC 2410554'
loop_
_audit_author_name
_audit_author_address
'Chong Liu'
;Sichuan University
China
;
_audit_update_record             
;
2025-01-25 deposited with the CCDC.	2025-02-09 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT430_SUM-33              
;
PROBLEM: Short Inter D...A Contact  O2       ..N2       .       2.87 Ang.
RESPONSE: O2 and N2 are two neighboring atoms coordinated to the same Cu center, there is no problem with the structure.
;
# Added during the CSD deposition process: Saturday 14 December 2024 05:14 AM
# end Validation Reply Form

_audit_creation_date             2024-03-03
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        SUM-33
_chemical_formula_moiety         'C6 H4 Cu N2 O2'
_chemical_formula_sum            'C6 H4 Cu N2 O2'
_chemical_formula_weight         199.65
_chemical_absolute_configuration ad
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   11.5203(4)
_cell_length_b                   15.0467(5)
_cell_length_c                   4.4357(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     768.90(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8950
_cell_measurement_temperature    223.00
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.23
_shelx_estimated_absorpt_T_max   0.788
_shelx_estimated_absorpt_T_min   0.731
_exptl_absorpt_coefficient_mu    2.786
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6004
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1308 before and 0.0666 after correction.
The Ratio of minimum to maximum transmission is 0.8053.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.725
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             396
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            24274
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.535
_diffrn_reflns_theta_min         2.226
_diffrn_ambient_temperature      223.00
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE TXS PHOTON II'
_diffrn_measurement_method       'ω and φ shutterless scans'
_diffrn_measurement_specimen_support 'nylon loop'
_diffrn_radiation_monochromator  'Helios Multi-layer Optic'
_diffrn_radiation_probe          X-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   TXS
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_type              'Rotaing Anode'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.771
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                1641
_reflns_number_total             1769
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2019)'
_computing_data_collection       'APEX5 V2023.9-2 (Bruker, 2023)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.226
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details 
;
 Flack x determined using 686 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.020(13)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         1769
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0228
_refine_ls_R_factor_gt           0.0209
_refine_ls_restrained_S_all      1.125
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0284P)²+0.2026P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0557
_refine_ls_wR_factor_ref         0.0568
_refine_special_details          SQUEEZE
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.50167(2) 0.58700(2) 0.9337(3) 0.01651(12) Uani 1 1 d . . . . .
O1 O 0.41133(17) 0.67828(13) 0.7549(5) 0.0240(5) Uani 1 1 d . . . . .
O2 O 0.43319(15) 0.51633(11) 0.6201(5) 0.0174(4) Uani 1 1 d . . . . .
N1 N 0.35637(18) 0.56582(14) 0.4301(6) 0.0217(5) Uani 1 1 d . . . . .
N2 N 0.10665(19) 0.82790(14) 0.1440(6) 0.0208(5) Uani 1 1 d . . . . .
C1 C 0.3516(2) 0.64704(17) 0.5295(6) 0.0185(6) Uani 1 1 d . . . . .
C2 C 0.2678(2) 0.70866(17) 0.3849(7) 0.0195(6) Uani 1 1 d . . . . .
C3 C 0.2690(3) 0.7979(2) 0.4626(10) 0.0399(9) Uani 1 1 d . . . . .
H3 H 0.324304 0.819640 0.599907 0.048 Uiso 1 1 calc R U . . .
C4 C 0.1884(3) 0.85445(19) 0.3368(9) 0.0356(8) Uani 1 1 d . . . . .
H4 H 0.191214 0.914915 0.389528 0.043 Uiso 1 1 calc R U . . .
C5 C 0.1829(3) 0.68096(19) 0.1877(8) 0.0347(8) Uani 1 1 d . . . . .
H5 H 0.178708 0.620905 0.130398 0.042 Uiso 1 1 calc R U . . .
C6 C 0.1039(3) 0.74119(19) 0.0743(9) 0.0348(8) Uani 1 1 d . . . . .
H6 H 0.045846 0.720645 -0.057221 0.042 Uiso 1 1 calc 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 O1 1.897(2) . ?
Cu1 O2 1.9140(19) 2_665 ?
Cu1 O2 1.920(2) . ?
Cu1 N2 1.993(2) 3_566 ?
O1 C1 1.302(3) . ?
O2 N1 1.431(3) . ?
N1 C1 1.300(3) . ?
N2 C4 1.333(4) . ?
N2 C6 1.341(3) . ?
C1 C2 1.484(4) . ?
C2 C3 1.387(4) . ?
C2 C5 1.377(4) . ?
C3 H3 0.9400 . ?
C3 C4 1.377(4) . ?
C4 H4 0.9400 . ?
C5 H5 0.9400 . ?
C5 C6 1.379(4) . ?
C6 H6 0.9400 . ?

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 O2 169.66(8) . 2_665 ?
O1 Cu1 O2 82.69(9) . . ?
O1 Cu1 N2 93.63(9) . 3_566 ?
O2 Cu1 O2 91.39(5) 2_665 . ?
O2 Cu1 N2 160.74(11) . 3_566 ?
O2 Cu1 N2 94.69(9) 2_665 3_566 ?
C1 O1 Cu1 110.46(16) . . ?
Cu1 O2 Cu1 126.98(9) 2_664 . ?
N1 O2 Cu1 113.11(14) . . ?
N1 O2 Cu1 114.25(15) . 2_664 ?
C1 N1 O2 108.4(2) . . ?
C4 N2 Cu1 122.44(18) . 3_464 ?
C4 N2 C6 117.1(2) . . ?
C6 N2 Cu1 120.2(2) . 3_464 ?
O1 C1 C2 116.8(2) . . ?
N1 C1 O1 125.3(2) . . ?
N1 C1 C2 117.9(2) . . ?
C3 C2 C1 119.4(2) . . ?
C5 C2 C1 123.2(2) . . ?
C5 C2 C3 117.3(2) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 C2 119.4(3) . . ?
C4 C3 H3 120.3 . . ?
N2 C4 C3 123.4(3) . . ?
N2 C4 H4 118.3 . . ?
C3 C4 H4 118.3 . . ?
C2 C5 H5 120.0 . . ?
C2 C5 C6 120.1(3) . . ?
C6 C5 H5 120.0 . . ?
N2 C6 C5 122.7(3) . . ?
N2 C6 H6 118.7 . . ?
C5 C6 H6 118.7 . . ?

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 N1 -2.9(3) . . . . ?
Cu1 O1 C1 C2 174.3(2) . . . . ?
Cu1 O2 N1 C1 -1.6(3) . . . . ?
Cu1 O2 N1 C1 -157.07(18) 2_664 . . . ?
Cu1 N2 C4 C3 -173.6(3) 3_464 . . . ?
Cu1 N2 C6 C5 172.7(3) 3_464 . . . ?
O1 C1 C2 C3 9.5(4) . . . . ?
O1 C1 C2 C5 -166.4(3) . . . . ?
O2 Cu1 O1 C1 1.19(18) . . . . ?
O2 Cu1 O1 C1 -54.3(7) 2_665 . . . ?
O2 N1 C1 O1 3.0(4) . . . . ?
O2 N1 C1 C2 -174.1(2) . . . . ?
N1 C1 C2 C3 -173.1(3) . . . . ?
N1 C1 C2 C5 10.9(4) . . . . ?
N2 Cu1 O1 C1 162.20(18) 3_566 . . . ?
C1 C2 C3 C4 -177.6(4) . . . . ?
C1 C2 C5 C6 176.5(3) . . . . ?
C2 C3 C4 N2 1.0(7) . . . . ?
C2 C5 C6 N2 1.1(6) . . . . ?
C3 C2 C5 C6 0.4(5) . . . . ?
C4 N2 C6 C5 -1.6(6) . . . . ?
C5 C2 C3 C4 -1.4(5) . . . . ?
C6 N2 C4 C3 0.5(6) . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 60 electrons were 
found in a volume of 180Å³ in 1 void per unit cell. 
This is consistent with the presence of 0.333[C3H7NO] per Formula Unit 
which account for 53 electrons per unit cell.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.500 -0.044 90.1 29.9 '0.667 DMF'
2 0.500 1.000 -0.876 90.1 29.9 '0.667 DMF'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_site                            XU
####################################################################### 
# 
# 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_SUM-23B
_database_code_depnum_ccdc_archive 'CCDC 2410553'
loop_
_audit_author_name
_audit_author_address
'Chong Liu'
;Sichuan University
China
;
_audit_update_record             
;
2025-01-25 deposited with the CCDC.	2025-02-09 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT341_SUM-23B             
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............      0.031 Ang.
RESPONSE: Weak high angle diffraction combined with poor data/parameters ratio leads to the observed low C-C precision.
;
# Added during the CSD deposition process: Monday 16 December 2024 10:43 AM
# end Validation Reply Form

_audit_creation_date             2024-12-14
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        SUM-23B
_chemical_formula_moiety         'C24 H16 Cu5 N8 O8'
_chemical_formula_sum            'C24 H16 Cu5 N8 O8'
_chemical_formula_weight         862.15
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0137 0.0067 '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 -2.7974 3.6876 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0241 0.0134 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0389 0.0241 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           120
_space_group_name_H-M_alt        'I -4 c 2'
_space_group_name_Hall           'I -4 -2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'x, -y, z+1/2'
'-x, y, z+1/2'
'y, x, -z+1/2'
'-y, -x, -z+1/2'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1'
'-x+1/2, y+1/2, z+1'
'y+1/2, x+1/2, -z+1'
'-y+1/2, -x+1/2, -z+1'

_cell_length_a                   23.9056(8)
_cell_length_b                   23.9056(8)
_cell_length_c                   14.4066(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8233.1(8)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    4064
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      52.230
_cell_measurement_theta_min      3.216
_shelx_estimated_absorpt_T_max   0.335
_shelx_estimated_absorpt_T_min   0.263
_exptl_absorpt_coefficient_mu    14.002
_exptl_absorpt_correction_T_max  0.7518
_exptl_absorpt_correction_T_min  0.5353
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1313 before and 0.0932 after correction.
The Ratio of minimum to maximum transmission is 0.7120.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3400
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1208
_diffrn_reflns_av_unetI/netI     0.1140
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16571
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         53.898
_diffrn_reflns_theta_min         2.274
_diffrn_ambient_temperature      193.0
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_measurement_specimen_support 'nylon loop'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_source                   ?
_diffrn_source_current           2.23
_diffrn_source_power             0.1554533
_diffrn_source_voltage           69.71
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.817
_reflns_Friedel_fraction_full    0.948
_reflns_Friedel_fraction_max     0.949
_reflns_number_gt                1891
_reflns_number_total             3653
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'APEX4 V2022.1-1 (Bruker, 2022)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.539
_refine_diff_density_min         -0.671
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.22(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         3653
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1483
_refine_ls_R_factor_gt           0.0803
_refine_ls_restrained_S_all      0.991
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1469P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2011
_refine_ls_wR_factor_ref         0.2425
_refine_special_details          
'Refined as a 2-component inversion twin.,SQUEEZE'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.78(2)
 0.22(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C3(H3), C4(H4), C6(H6), C10(H10), C5(H5), C11(H11), C9(H9)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 1.000000 0.500000 0.250000 0.083(3) Uani 1 4 d S T P . .
Cu4 Cu 0.500000 0.500000 0.500000 0.080(2) Uani 1 4 d S T P . .
Cu3 Cu 0.62614(11) 0.53471(11) 0.4649(3) 0.0810(13) Uani 1 1 d . . . . .
Cu2 Cu 0.88101(11) 0.55953(12) 0.2128(3) 0.0984(17) Uani 1 1 d . . . . .
O1 O 0.9342(5) 0.4566(5) 0.2424(14) 0.084(5) Uani 1 1 d . . . . .
O4 O 0.5558(5) 0.5564(5) 0.5044(13) 0.080(5) Uani 1 1 d . . . . .
O3 O 0.6248(5) 0.6054(5) 0.4048(13) 0.081(5) Uani 1 1 d . . . . .
N1 N 0.8847(5) 0.4822(6) 0.2592(17) 0.077(6) Uani 1 1 d . . . . .
O2 O 0.8664(5) 0.3963(5) 0.3298(15) 0.097(6) Uani 1 1 d . . . . .
N2 N 0.6969(6) 0.5094(6) 0.4155(17) 0.086(7) Uani 1 1 d . . . . .
N3 N 0.5408(8) 0.6100(6) 0.4772(15) 0.082(6) Uani 1 1 d . . . . .
N4 N 0.5679(6) 0.8012(7) 0.3259(18) 0.086(7) Uani 1 1 d . . . . .
C12 C 0.5204(8) 0.7171(7) 0.381(2) 0.084(8) Uani 1 1 d . . . . .
H12 H 0.487061 0.698843 0.400514 0.101 Uiso 1 1 calc R U . . .
C3 C 0.7944(8) 0.5230(8) 0.378(2) 0.087(8) Uani 1 1 d . . . . .
H3 H 0.825688 0.547443 0.374231 0.104 Uiso 1 1 calc R U . . .
C2 C 0.7984(7) 0.4698(7) 0.3478(19) 0.080(8) Uani 1 1 d . . . . .
C7 C 0.5779(7) 0.6318(8) 0.418(2) 0.080(8) Uani 1 1 d . . . . .
C1 C 0.8526(8) 0.4492(8) 0.315(2) 0.103(11) Uani 1 1 d . . . . .
C4 C 0.7426(8) 0.5419(9) 0.4147(19) 0.082(7) Uani 1 1 d . . . . .
H4 H 0.740372 0.578611 0.439681 0.098 Uiso 1 1 calc R U . . .
C6 C 0.7510(8) 0.4363(9) 0.347(2) 0.096(10) Uani 1 1 d . . . . .
H6 H 0.752359 0.399452 0.322026 0.116 Uiso 1 1 calc R U . . .
C8 C 0.5701(9) 0.6886(8) 0.383(2) 0.101(10) Uani 1 1 d . . . . .
C10 C 0.6136(8) 0.7753(9) 0.330(2) 0.100(10) Uani 1 1 d . . . . .
H10 H 0.646693 0.794207 0.310823 0.120 Uiso 1 1 calc R U . . .
C5 C 0.7025(8) 0.4575(11) 0.381(2) 0.091(8) Uani 1 1 d . . . . .
H5 H 0.670416 0.434041 0.381249 0.110 Uiso 1 1 calc R U . . .
C11 C 0.5180(10) 0.7718(9) 0.352(2) 0.104(10) Uani 1 1 d . . . . .
H11 H 0.482948 0.790339 0.349747 0.125 Uiso 1 1 calc R U . . .
C9 C 0.6180(10) 0.7181(11) 0.361(3) 0.135(15) Uani 1 1 d . . . . .
H9 H 0.653670 0.700840 0.366241 0.162 Uiso 1 1 calc 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 O1 1.887(12) 2_765 ?
Cu1 O1 1.887(12) 11_565 ?
Cu1 O1 1.887(12) 12_645 ?
Cu1 O1 1.887(12) . ?
Cu4 O4 1.898(11) 4_656 ?
Cu4 O4 1.898(11) . ?
Cu4 O4 1.898(11) 3_566 ?
Cu4 O4 1.898(11) 2_665 ?
Cu3 O4 1.849(13) . ?
Cu3 O3 1.899(14) . ?
Cu3 N2 1.933(15) . ?
Cu3 N3 2.026(16) 3_566 ?
Cu2 O1 1.925(12) 11_565 ?
Cu2 N1 1.969(15) . ?
Cu2 O2 1.910(13) 11_565 ?
Cu2 N4 1.998(16) 7 ?
O1 N1 1.354(17) . ?
O4 N3 1.39(2) . ?
O3 C7 1.301(19) . ?
N1 C1 1.37(3) . ?
O2 C1 1.32(2) . ?
N2 C4 1.34(2) . ?
N2 C5 1.34(3) . ?
N3 C7 1.34(3) . ?
N4 C10 1.26(2) . ?
N4 C11 1.44(3) . ?
C12 H12 0.9500 . ?
C12 C8 1.37(3) . ?
C12 C11 1.37(3) . ?
C3 H3 0.9500 . ?
C3 C2 1.35(3) . ?
C3 C4 1.42(3) . ?
C2 C1 1.46(3) . ?
C2 C6 1.39(3) . ?
C7 C8 1.46(3) . ?
C4 H4 0.9500 . ?
C6 H6 0.9500 . ?
C6 C5 1.36(3) . ?
C8 C9 1.38(3) . ?
C10 H10 0.9500 . ?
C10 C9 1.44(3) . ?
C5 H5 0.9500 . ?
C11 H11 0.9500 . ?
C9 H9 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 O1 90.20(8) 2_765 12_645 ?
O1 Cu1 O1 90.19(7) 12_645 . ?
O1 Cu1 O1 173.3(12) 2_765 . ?
O1 Cu1 O1 90.20(7) 2_765 11_565 ?
O1 Cu1 O1 173.3(12) 12_645 11_565 ?
O1 Cu1 O1 90.20(8) 11_565 . ?
O4 Cu4 O4 90.06(4) 2_665 4_656 ?
O4 Cu4 O4 90.06(4) 3_566 . ?
O4 Cu4 O4 176.2(12) 2_665 . ?
O4 Cu4 O4 90.06(4) 2_665 3_566 ?
O4 Cu4 O4 176.2(12) 4_656 3_566 ?
O4 Cu4 O4 90.06(4) 4_656 . ?
O4 Cu3 O3 82.8(6) . . ?
O4 Cu3 N2 175.6(9) . . ?
O4 Cu3 N3 87.2(6) . 3_566 ?
O3 Cu3 N2 97.2(7) . . ?
O3 Cu3 N3 167.9(6) . 3_566 ?
N2 Cu3 N3 92.3(7) . 3_566 ?
O1 Cu2 N1 85.2(6) 11_565 . ?
O1 Cu2 N4 169.3(6) 11_565 7 ?
N1 Cu2 N4 103.4(6) . 7 ?
O2 Cu2 O1 81.7(6) 11_565 11_565 ?
O2 Cu2 N1 166.4(6) 11_565 . ?
O2 Cu2 N4 90.0(7) 11_565 7 ?
Cu1 O1 Cu2 115.6(6) . 12_645 ?
N1 O1 Cu1 118.0(9) . . ?
N1 O1 Cu2 115.5(10) . 12_645 ?
Cu3 O4 Cu4 115.4(7) . . ?
N3 O4 Cu4 117.7(11) . . ?
N3 O4 Cu3 114.0(10) . . ?
C7 O3 Cu3 112.4(14) . . ?
O1 N1 Cu2 113.7(11) . . ?
O1 N1 C1 109.7(14) . . ?
C1 N1 Cu2 135.9(13) . . ?
C1 O2 Cu2 111.3(13) . 12_645 ?
C4 N2 Cu3 122.4(15) . . ?
C4 N2 C5 116.8(18) . . ?
C5 N2 Cu3 120.7(13) . . ?
O4 N3 Cu3 106.8(10) . 4_656 ?
C7 N3 Cu3 141.3(15) . 4_656 ?
C7 N3 O4 111.7(15) . . ?
C10 N4 Cu2 124.7(14) . 7 ?
C10 N4 C11 118.0(18) . . ?
C11 N4 Cu2 117.3(13) . 7 ?
C8 C12 H12 119.5 . . ?
C8 C12 C11 121(2) . . ?
C11 C12 H12 119.5 . . ?
C2 C3 H3 120.6 . . ?
C2 C3 C4 118.8(18) . . ?
C4 C3 H3 120.6 . . ?
C3 C2 C1 118.8(17) . . ?
C3 C2 C6 119(2) . . ?
C6 C2 C1 122(2) . . ?
O3 C7 N3 118(2) . . ?
O3 C7 C8 120.8(18) . . ?
N3 C7 C8 119.8(17) . . ?
N1 C1 C2 119.6(18) . . ?
O2 C1 N1 120.3(18) . . ?
O2 C1 C2 119.5(18) . . ?
N2 C4 C3 122(2) . . ?
N2 C4 H4 119.0 . . ?
C3 C4 H4 119.0 . . ?
C2 C6 H6 120.8 . . ?
C5 C6 C2 118(2) . . ?
C5 C6 H6 120.8 . . ?
C12 C8 C7 125(2) . . ?
C12 C8 C9 117(2) . . ?
C9 C8 C7 117(2) . . ?
N4 C10 H10 118.6 . . ?
N4 C10 C9 122.9(19) . . ?
C9 C10 H10 118.6 . . ?
N2 C5 C6 124(2) . . ?
N2 C5 H5 117.8 . . ?
C6 C5 H5 117.8 . . ?
N4 C11 H11 119.6 . . ?
C12 C11 N4 121(2) . . ?
C12 C11 H11 119.6 . . ?
C8 C9 C10 120(2) . . ?
C8 C9 H9 120.2 . . ?
C10 C9 H9 120.2 . . ?

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 N1 Cu2 37(2) . . . . ?
Cu1 O1 N1 C1 -135.4(19) . . . . ?
Cu4 O4 N3 Cu3 43.7(18) . . . 4_656 ?
Cu4 O4 N3 C7 -131.9(18) . . . . ?
Cu3 O4 N3 Cu3 -176.3(9) . . . 4_656 ?
Cu3 O4 N3 C7 8(3) . . . . ?
Cu3 O3 C7 N3 7(3) . . . . ?
Cu3 O3 C7 C8 175(2) . . . . ?
Cu3 N2 C4 C3 -179.6(19) . . . . ?
Cu3 N2 C5 C6 -179(2) . . . . ?
Cu3 N3 C7 O3 176.7(19) 4_656 . . . ?
Cu3 N3 C7 C8 8(4) 4_656 . . . ?
Cu2 O1 N1 Cu2 179.5(9) 12_645 . . . ?
Cu2 O1 N1 C1 7(3) 12_645 . . . ?
Cu2 N1 C1 O2 177(2) . . . . ?
Cu2 N1 C1 C2 7(5) . . . . ?
Cu2 O2 C1 N1 13(4) 12_645 . . . ?
Cu2 O2 C1 C2 -177(2) 12_645 . . . ?
Cu2 N4 C10 C9 178(3) 7 . . . ?
Cu2 N4 C11 C12 -179(2) 7 . . . ?
O1 Cu1 O1 Cu2 -153.0(15) 11_565 . . 12_645 ?
O1 Cu1 O1 Cu2 20.3(4) 12_645 . . 12_645 ?
O1 Cu1 O1 N1 163(2) 12_645 . . . ?
O1 Cu1 O1 N1 -10.2(13) 11_565 . . . ?
O1 N1 C1 O2 -13(4) . . . . ?
O1 N1 C1 C2 176(2) . . . . ?
O4 Cu4 O4 Cu3 19.0(4) 3_566 . . . ?
O4 Cu4 O4 Cu3 -157.2(15) 4_656 . . . ?
O4 Cu4 O4 N3 -17.8(10) 4_656 . . . ?
O4 Cu4 O4 N3 158.4(19) 3_566 . . . ?
O4 Cu3 O3 C7 -1.7(17) . . . . ?
O4 N3 C7 O3 -10(3) . . . . ?
O4 N3 C7 C8 -178(2) . . . . ?
O3 Cu3 O4 Cu4 137.3(11) . . . . ?
O3 Cu3 O4 N3 -3.6(15) . . . . ?
O3 C7 C8 C12 170(3) . . . . ?
O3 C7 C8 C9 -18(4) . . . . ?
N2 Cu3 O3 C7 173.8(17) . . . . ?
N3 Cu3 O4 Cu4 -35.8(11) 3_566 . . . ?
N3 Cu3 O4 N3 -176.7(12) 3_566 . . . ?
N3 Cu3 O3 C7 33(5) 3_566 . . . ?
N3 C7 C8 C12 -21(5) . . . . ?
N3 C7 C8 C9 150(3) . . . . ?
N4 C10 C9 C8 4(6) . . . . ?
C12 C8 C9 C10 -5(5) . . . . ?
C3 C2 C1 N1 -44(4) . . . . ?
C3 C2 C1 O2 146(3) . . . . ?
C3 C2 C6 C5 -4(4) . . . . ?
C2 C3 C4 N2 -4(4) . . . . ?
C2 C6 C5 N2 1(5) . . . . ?
C7 C8 C9 C10 -178(3) . . . . ?
C1 C2 C6 C5 177(3) . . . . ?
C4 N2 C5 C6 0(4) . . . . ?
C4 C3 C2 C1 -176(3) . . . . ?
C4 C3 C2 C6 5(4) . . . . ?
C6 C2 C1 N1 135(3) . . . . ?
C6 C2 C1 O2 -35(5) . . . . ?
C8 C12 C11 N4 -2(4) . . . . ?
C10 N4 C11 C12 0(5) . . . . ?
C5 N2 C4 C3 1(4) . . . . ?
C11 N4 C10 C9 -1(5) . . . . ?
C11 C12 C8 C7 176(3) . . . . ?
C11 C12 C8 C9 5(5) . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 1302 electrons were 
found in a volume of 3806Å³ in 1 void per unit cell. 
This is consistent with the presence of 16.3[H2O] per Formula Unit 
which account for 1303 electrons per unit cell.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.838 -0.148 -0.700 3806.1 1302.3 '130.3 H2O'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.78(2)
2 0.22(2)

