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_7712086
_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'
_chemical_formula_sum            'C44 H24 Cl4 Cu F2 N4 O2'
_chemical_formula_weight         884.01
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-01-07
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-01-07 deposited with the CCDC.	2023-01-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.2100(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.06330(10)
_cell_length_b                   19.92460(10)
_cell_length_c                   10.12960(10)
_cell_measurement_reflns_used    13650
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      77.7510
_cell_measurement_theta_min      4.4290
_cell_volume                     1906.01(3)
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293(2)
_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 0.981
_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     97.00 178.00   0.50    0.60    --  110.00  45.00   0.00  162
  2  \w    122.00 177.00   0.50    0.60    --  110.00  45.00  30.00  110
  3  \w     95.00 121.00   0.50    0.60    --  110.00  15.00 150.00   52
  4  \w    103.00 178.00   0.50    0.60    --  110.00  45.00 -30.00  150
  5  \w    100.00 133.00   0.50    0.60    --  110.00  77.00-180.00   66
  6  \w    -26.00  28.00   0.50    0.16    --  -47.12  19.00-120.00  108
  7  \w    -69.00 -19.00   0.50    0.16    --  -47.12 102.00  45.00  100
  8  \w    -72.00 -47.00   0.50    0.60    --  -88.50 102.00  45.00   50
  9  \w      8.00  82.00   0.50    0.16    --   47.12-102.00 -58.00  148
 10  \w     39.00 106.00   0.50    0.60    --  110.00-102.00 -58.00  134
 11  \w     51.00 101.00   0.50    0.60    --  110.00 -94.00 -30.00  100
 12  \w     44.00  70.00   0.50    0.60    --  110.00 -94.00  30.00   52
 13  \w     73.00  99.00   0.50    0.60    --  110.00 -94.00  30.00   52
 14  \w     57.00  91.00   0.50    0.60    --  110.00 -94.00   0.00   68
 15  \w     74.00  99.00   0.50    0.60    --  110.00 -77.00 -30.00   50
 16  \w     56.00  82.00   0.50    0.60    --  110.00 -77.00  30.00   52
 17  \w     38.00  71.00   0.50    0.60    --  110.00 -61.00   0.00   66
 18  \w     40.00  69.00   0.50    0.60    --  110.00 -61.00  60.00   58
 19  \w     46.00  72.00   0.50    0.60    --  110.00 -77.00 -30.00   52
 20  \w     78.00 104.00   0.50    0.60    --  110.00 -77.00 -90.00   52
 21  \w     38.00  70.00   0.50    0.60    --  110.00 -61.00-150.00   64
 22  \w     42.00  68.00   0.50    0.60    --  110.00 -61.00-180.00   52
 23  \w     40.00  70.00   0.50    0.60    --  110.00 -61.00  30.00   60
 24  \w     43.00  71.00   0.50    0.60    --  110.00 -61.00  90.00   56
 25  \w     38.00  71.00   0.50    0.60    --  110.00 -61.00 150.00   66
 26  \w    -25.00  20.00   0.50    0.16    --   47.12 -19.00  30.00   90
 27  \w    103.00 154.00   0.50    0.60    --  110.00 125.00  60.00  102
 28  \w    109.00 144.00   0.50    0.60    --  110.00 102.00  45.00   70
 29  \w    -80.00 -54.00   0.50    0.16    --  -47.12 -57.00   0.00   52
 30  \w   -149.00 -98.00   0.50    0.60    --  -88.50-102.00 -58.00  102
 31  \w   -118.00 -84.00   0.50    0.16    --  -47.12-125.00   0.00   68
 32  \w   -117.00 -74.00   0.50    0.16    --  -47.12-125.00  30.00   86
 33  \w   -118.00 -88.00   0.50    0.16    --  -47.12-125.00 150.00   60
 34  \w     94.00 120.00   0.50    0.16    --   46.87  77.00-180.00   52
 35  \w     54.00  80.00   0.50    0.60    --  110.00 -77.00 120.00   52
 36  \w     44.00  70.00   0.50    0.60    --  110.00 -61.00  60.00   52
;
_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      0.0496377000
_diffrn_orient_matrix_UB_12      -0.0736514000
_diffrn_orient_matrix_UB_13      0.0165175000
_diffrn_orient_matrix_UB_21      0.0547590000
_diffrn_orient_matrix_UB_22      0.0085169000
_diffrn_orient_matrix_UB_23      -0.1234466000
_diffrn_orient_matrix_UB_31      0.1454132000
_diffrn_orient_matrix_UB_32      0.0220003000
_diffrn_orient_matrix_UB_33      0.1036676000
_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  0.0363
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            17093
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.030
_diffrn_reflns_theta_min         4.438
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.851
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63743
_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    1.540
_exptl_crystal_description       block
_exptl_crystal_F_000             894
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.293
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       0.00075(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         3988
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0343
_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/[\s^2^(Fo^2^)+(0.0515P)^2^+0.7255P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0956
_refine_ls_wR_factor_ref         0.0968
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3735
_reflns_number_total             3988
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt04108a2.cif
_cod_data_source_block           20201109-czf-swy-l26
_cod_database_code               7712086
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C84 H44 Cl8 Cu2 F4 N12 O4 '
_shelx_estimated_absorpt_t_max   0.655
_shelx_estimated_absorpt_t_min   0.596
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C22(H22), C7(H7), C6(H6), C5(H5), C11(H11), C4(H4), C20(H20),
 C19(H19), C14(H14), C12(H12), C13(H13)
;
_shelx_res_checksum              7756
_shelx_hkl_checksum              46364
_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 1.316
_oxdiff_exptl_absorpt_empirical_full_min 0.621