Copper(II) complex enhanced chemodynamic therapy through GSH depletion and autophagy flow blockade
Shen, Wen-Ying; Jia, Chun-Peng; Liao, Li-Yi; Chen, Liu-Lin; Yuan, Chen-Cheng; Gu, Yunqiong; Liu, Yang-Han; Liang, Hong; Chen, Zhen-Feng; Dalton Transactions  (2023) –; doi:10.1039/D2DT04108A

data_7712088
_publ_section_title
;
 Copper(II) complex enhanced chemodynamic therapy through GSH depletion
 and autophagy flow blockade
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT04108A
_journal_year                    2023
_chemical_formula_moiety         'C44 H24 Cl4 Cu F2 N4 O2, 2(C H4 O)'
_chemical_formula_sum            'C46 H32 Cl4 Cu F2 N4 O4'
_chemical_formula_weight         948.09
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-01-07
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-01-07 deposited with the CCDC.	2023-01-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.6220(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.3709(2)
_cell_length_b                   11.58280(10)
_cell_length_c                   15.57890(10)
_cell_measurement_reflns_used    11714
_cell_measurement_temperature    295.29(10)
_cell_measurement_theta_max      77.2040
_cell_measurement_theta_min      2.9020
_cell_volume                     4291.38(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      295.29(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     91.00 132.00   0.50    1.30    --  108.56  15.00  30.00   82
  2  \w    150.00 177.00   0.50    1.30    --  108.56  15.00  30.00   54
  3  \w     83.00 177.00   0.50    1.30    --  108.56   9.00 123.00  188
  4  \w     46.00  71.00   0.50    0.30    --   47.12   9.00 123.00   50
  5  \w    -25.00  27.00   0.50    0.30    --  -47.12   9.00 123.00  104
  6  \w    -48.00 -16.00   0.50    1.30    --  -88.50  45.00  60.00   64
  7  \w    -51.00 -18.00   0.50    1.30    --  -88.50  45.00  90.00   66
  8  \w    -50.00 -15.00   0.50    1.30    --  -88.50  61.00 -60.00   70
  9  \w     36.00  75.00   0.50    1.30    --  108.56 -94.00  30.00   78
 10  \w     46.00  95.00   0.50    0.30    --   47.12-125.00-120.00   98
 11  \w     75.00 111.00   0.50    1.30    --  108.56-125.00-150.00   72
 12  \w     36.00  65.00   0.50    1.30    --  108.56-125.00-150.00   58
 13  \w     49.00 101.00   0.50    1.30    --  108.56 -94.00-150.00  104
 14  \w     75.00 101.00   0.50    1.30    --  108.56 -94.00-120.00   52
 15  \w     41.00  67.00   0.50    1.30    --  108.56 -94.00-120.00   52
 16  \w     79.00 104.00   0.50    1.30    --  108.56 -94.00 120.00   50
 17  \w     38.00  64.00   0.50    1.30    --  108.56 -94.00 120.00   52
 18  \w     37.00  63.00   0.50    1.30    --  108.56 -61.00 120.00   52
 19  \w     43.00  71.00   0.50    1.30    --  108.56 -61.00 150.00   56
 20  \w     44.00  70.00   0.50    1.30    --  108.56 -61.00  90.00   52
 21  \w     73.00 105.00   0.50    1.30    --  108.56 -77.00-120.00   64
 22  \w     38.00  63.00   0.50    1.30    --  108.56 -77.00-120.00   50
 23  \w     36.00  61.00   0.50    1.30    --  108.56 -61.00-120.00   50
 24  \w     -6.00  20.00   0.50    0.30    --   47.12 -19.00-150.00   52
 25  \w    -23.00  27.00   0.50    0.30    --   47.12 -19.00-180.00  100
 26  \w     -3.00  24.00   0.50    0.30    --   47.12  -9.00 -51.00   54
 27  \w   -122.00 -24.00   0.50    0.30    --  -47.12  -9.00 -51.00  196
 28  \w   -148.00 -69.00   0.50    1.30    --  -88.50  -9.00 -51.00  158
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0315942000
_diffrn_orient_matrix_UB_12      -0.0118711000
_diffrn_orient_matrix_UB_13      -0.0966535000
_diffrn_orient_matrix_UB_21      -0.0562787000
_diffrn_orient_matrix_UB_22      -0.0051705000
_diffrn_orient_matrix_UB_23      0.0295005000
_diffrn_orient_matrix_UB_31      -0.0052324000
_diffrn_orient_matrix_UB_32      0.1324278000
_diffrn_orient_matrix_UB_33      -0.0074961000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0202
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15217
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.282
_diffrn_reflns_theta_min         3.717
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.494
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51837
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic reddish red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_description       block
_exptl_crystal_F_000             1932
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.233
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         4347
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0347
_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/[\s^2^(Fo^2^)+(0.0533P)^2^+2.8959P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0993
_refine_ls_wR_factor_ref         0.1005
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4073
_reflns_number_total             4347
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt04108a2.cif
_cod_data_source_block           20201110-czf-jcp-l25a
_cod_database_code               7712088
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C184 H88 Cl16 Cu4 N32 O8 '
_shelx_estimated_absorpt_t_max   0.679
_shelx_estimated_absorpt_t_min   0.659
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(F1) = Uanis(F1')
3. Others
 Sof(H18)=Sof(F1')=1-FVAR(1)
 Sof(F1)=Sof(H22)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C5(H5), C2(H2), C11(H11), C18(H18), C22(H22), C12(H12),
 C14(H14), C13(H13), C21(H21), C19(H19), C20(H20)
4.b Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C)
4.c Idealised tetrahedral OH refined as rotating group:
 O2(H2A)
;
_shelx_res_checksum              29799
_shelx_hkl_checksum              8032
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.810
_oxdiff_exptl_absorpt_empirical_full_min 0.644