Cu(I)-based Fenton-like agent inducing mitochondrial damage for photo-assisted enhanced chemodynamic therapy
Hong, Zhao-Guo; Zhong, Jingjing; Ding, Dang-Dang; Gong, Si-Hui; Zhang, Liangliang; Zhao, Shulin; Shen, Xing-Can; Liang, Hong; Huang, Fu-Ping; Dalton Transactions  (2023) –; doi:10.1039/D3DT00317E

data_7712751
_publ_section_title
;
 Cu(I)-based Fenton-like agent inducing mitochondrial damage for
 photo-assisted enhanced chemodynamic therapy
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00317E
_journal_year                    2023
_chemical_formula_moiety         'C96 H88 Cu2 N6 O2 P4, 2(N O3), 2(C H4 O)'
_chemical_formula_sum            'C98 H96 Cu2 N8 O10 P4'
_chemical_formula_weight         1796.79
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-11-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-07-22 deposited with the CCDC.	2023-04-06 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 103.7750(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.22620(10)
_cell_length_b                   21.26880(10)
_cell_length_c                   15.15300(10)
_cell_measurement_reflns_used    31738
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.8140
_cell_measurement_theta_min      3.1950
_cell_volume                     4453.04(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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    -26.00   0.00   0.50    1.00    --  -47.12  19.00 -90.00   52
  2  \w    -23.00   3.00   0.50    1.00    --  -47.12  19.00-180.00   52
  3  \w    -59.00  -7.00   0.50    1.00    --  -47.12 109.00-117.00  104
  4  \w    -51.00 -16.00   0.50    3.00    --  -88.50  45.00  30.00   70
  5  \w    -51.00 -26.00   0.50    3.00    --  -88.50  45.00  90.00   50
  6  \w    -26.00  27.00   0.50    1.00    --  -47.12  19.00 150.00  106
  7  \w     23.00  87.00   0.50    1.00    --   47.12-109.00 145.00  128
  8  \w     73.00  98.00   0.50    3.00    --  110.00-109.00 145.00   50
  9  \w     81.00 106.00   0.50    3.00    --  110.00 -77.00 150.00   50
 10  \w     62.00  90.00   0.50    3.00    --  110.00 -94.00 150.00   56
 11  \w     41.00  67.00   0.50    3.00    --  110.00 -61.00 150.00   52
 12  \w     38.00  71.00   0.50    3.00    --  110.00 -77.00 150.00   66
 13  \w     39.00 102.00   0.50    3.00    --  110.00 -77.00  90.00  126
 14  \w     95.00 134.00   0.50    3.00    --  110.00  15.00  90.00   78
 15  \w    138.00 169.00   0.50    3.00    --  110.00  15.00  90.00   62
 16  \w    129.00 155.00   0.50    3.00    --  110.00 125.00  30.00   52
 17  \w    127.00 153.00   0.50    3.00    --  110.00 109.00-117.00   52
 18  \w     92.00 157.00   0.50    3.00    --  110.00  15.00-150.00  130
 19  \w     92.00 178.00   0.50    3.00    --  110.00  15.00 -90.00  172
 20  \w     93.00 177.00   0.50    3.00    --  110.00  15.00  60.00  168
 21  \w     81.00 107.00   0.50    3.00    --  110.00-112.00-137.20   52
 22  \w     81.00 111.00   0.50    3.00    --  110.00-125.00-180.00   60
 23  \w     75.00 110.00   0.50    3.00    --  110.00-125.00-150.00   70
 24  \w     64.00 104.00   0.50    3.00    --  110.00-100.00-131.73   80
 25  \w     47.00  75.00   0.50    3.00    --  110.00-112.00-137.20   56
 26  \w     44.00  74.00   0.50    3.00    --  110.00 -94.00-120.00   60
 27  \w     46.00  71.00   0.50    3.00    --  110.00 -61.00-180.00   50
 28  \w     44.00  69.00   0.50    3.00    --  110.00 -61.00-150.00   50
 29  \w     38.00  65.00   0.50    3.00    --  110.00 -61.00 -90.00   54
 30  \w     40.00  69.00   0.50    3.00    --  110.00 -61.00 -30.00   58
 31  \w     42.00  70.00   0.50    3.00    --  110.00 -61.00  30.00   56
 32  \w     41.00  70.00   0.50    3.00    --  110.00 -61.00   0.00   58
 33  \w     44.00  69.00   0.50    3.00    --  110.00 -61.00 -60.00   50
 34  \w     38.00  92.00   0.50    3.00    --  110.00 -94.00 -90.00  108
 35  \w     39.00  75.00   0.50    3.00    --  110.00-125.00-180.00   72
 36  \w     38.00  63.00   0.50    3.00    --  110.00 -61.00  60.00   50
 37  \w   -120.00 -61.00   0.50    1.00    --  -47.12 -37.00-180.00  118
 38  \w   -112.00 -73.00   0.50    1.00    --  -47.12-125.00 -60.00   78
 39  \w   -119.00 -78.00   0.50    1.00    --  -47.12-125.00-120.00   82
 40  \w   -118.00 -79.00   0.50    1.00    --  -47.12-125.00 -90.00   78
 41  \w   -145.00-120.00   0.50    3.00    --  -88.50-109.00 145.00   50
 42  \w    -73.00 -48.00   0.50    3.00    --  -88.50 109.00-117.00   50
;
_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      -0.0122962000
_diffrn_orient_matrix_UB_12      -0.0684235000
_diffrn_orient_matrix_UB_13      0.0286519000
_diffrn_orient_matrix_UB_21      -0.0466094000
_diffrn_orient_matrix_UB_22      -0.0172047000
_diffrn_orient_matrix_UB_23      -0.0995786000
_diffrn_orient_matrix_UB_31      0.1005066000
_diffrn_orient_matrix_UB_32      -0.0163130000
_diffrn_orient_matrix_UB_33      -0.0151021000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            44875
_diffrn_reflns_theta_full        77.95
_diffrn_reflns_theta_max         77.95
_diffrn_reflns_theta_min         3.65
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.786
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.80a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1876
_refine_diff_density_max         1.905
_refine_diff_density_min         -0.697
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     554
_refine_ls_number_reflns         9374
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0519
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0782P)^2^+7.1536P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1443
_refine_ls_wR_factor_ref         0.1462
_reflns_number_gt                8806
_reflns_number_total             9374
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d3dt00317e2.cif
_cod_data_source_block           20201102-hfp-hzg-n-rg-cu
_cod_database_code               7712751
_chemical_oxdiff_formula         'C196 H184 Cu4 N16 O20 P8 '
_diffrn_oxdiff_digest_frames
;
01128302f35f4d4ccc4e7462d335747965000285177
;
_diffrn_oxdiff_digest_hkl
;
016b8e42c3d8ba2e6a96c16b1419656d5c14cc
;
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C14(H14),
 C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23),
  C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32),
 C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39), C40(H40), C41(H41),
  C42(H42), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C49(H49A,H49B,H49C)
2.c Idealised tetrahedral OH refined as rotating group:
 O5(H5A)
;
_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 1.372
_oxdiff_exptl_absorpt_empirical_full_min 0.777