A triphenylphosphine coordinated Cu(i) Fenton-like agent with ferrocene moieties for enhanced chemodynamic therapy
Zhong, Jingjing; Hong, Zhaoguo; Huang, Sudi; Zhong, Qiongqiong; Zhang, Liangliang; Zhao, Shulin; Liang, Hong; Huang, Fu-Ping; Dalton Transactions  (2022) –; doi:10.1039/D2DT03088H

data_7711754
_publ_section_title
;
 A triphenylphosphine coordinated Cu(i) Fenton-like agent with ferrocene
 moieties for enhanced chemodynamic therapy
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT03088H
_journal_year                    2022
_chemical_formula_moiety         'C48 H41 Cu Fe N2 O P2, N O3'
_chemical_formula_sum            'C48 H41 Cu Fe N3 O4 P2'
_chemical_formula_weight         905.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-11-30
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2022-09-05 deposited with the CCDC.	2022-11-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.2340(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7163(2)
_cell_length_b                   20.0068(3)
_cell_length_c                   16.7064(2)
_cell_measurement_reflns_used    16955
_cell_measurement_temperature    295.76(10)
_cell_measurement_theta_max      76.3150
_cell_measurement_theta_min      2.1880
_cell_volume                     4328.65(11)
_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 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      295.76(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.966
_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    113.00 138.00   0.50    0.78    --  108.56 124.00-137.00   50
  2  \w    102.00 128.00   0.50    0.78    --  108.56 125.00 -30.00   52
  3  \w    152.00 178.00   0.50    0.78    --  108.56 125.00 -30.00   52
  4  \w    112.00 178.00   0.50    0.78    --  108.56  45.00  30.00  132
  5  \w    -27.00  28.00   0.50    0.19    --  -47.12  19.00  90.00  110
  6  \w    -47.00 -17.00   0.50    0.78    --  -88.50  45.00 -30.00   60
  7  \w    -50.00 -16.00   0.50    0.78    --  -88.50  45.00   0.00   68
  8  \w    -49.00 -19.00   0.50    0.78    --  -88.50  45.00  30.00   60
  9  \w    -49.00 -16.00   0.50    0.78    --  -88.50  45.00  90.00   66
 10  \w    -51.00 -16.00   0.50    0.78    --  -88.50  45.00  60.00   70
 11  \w    -27.00  24.00   0.50    0.19    --  -47.12  19.00-180.00  102
 12  \w    -83.00 -38.00   0.50    0.19    --  -47.12 124.00-137.00   90
 13  \w    -74.00 -49.00   0.50    0.78    --  -88.50 124.00-137.00   50
 14  \w    -87.00 -62.00   0.50    0.78    --  -88.50 146.00  27.00   50
 15  \w   -142.00 -81.00   0.50    0.78    --  -88.50-146.00 -22.00  122
 16  \w   -115.00 -89.00   0.50    0.19    --  -47.12-125.00-180.00   52
 17  \w   -118.00 -92.00   0.50    0.19    --  -47.12-146.00 -22.00   52
 18  \w   -141.00-116.00   0.50    0.78    --  -88.50-124.00 143.00   50
 19  \w   -138.00 -84.00   0.50    0.78    --  -88.50 -94.00 150.00  108
 20  \w    -98.00 -73.00   0.50    0.78    --  -88.50 -30.00  30.00   50
 21  \w   -150.00-123.00   0.50    0.78    --  -88.50 -30.00  30.00   54
 22  \w   -118.00 -68.00   0.50    0.19    --  -47.12 -57.00-180.00  100
 23  \w    -65.00 -39.00   0.50    0.19    --  -47.12 -57.00-180.00   52
 24  \w     53.00  78.00   0.50    0.19    --   47.12-146.00 -22.00   50
 25  \w     36.00 111.00   0.50    0.78    --  108.56-125.00-180.00  150
 26  \w     46.00 126.00   0.50    0.78    --  108.56-146.00 -22.00  160
 27  \w     70.00  97.00   0.50    0.78    --  108.56 -94.00-180.00   54
 28  \w     48.00 103.00   0.50    0.78    --  108.56 -94.00 -30.00  110
 29  \w     40.00  65.00   0.50    0.19    --   47.12-124.00 143.00   50
 30  \w     36.00 108.00   0.50    0.78    --  108.56-124.00 143.00  144
 31  \w     58.00  84.00   0.50    0.78    --  108.56 -94.00 150.00   52
 32  \w     37.00  71.00   0.50    0.78    --  108.56 -61.00 120.00   68
 33  \w     39.00  70.00   0.50    0.78    --  108.56 -61.00 150.00   62
 34  \w     46.00  71.00   0.50    0.78    --  108.56 -61.00 -90.00   50
 35  \w    -21.00  27.00   0.50    0.19    --   47.12 -19.00-150.00   96
 36  \w     38.00  65.00   0.50    0.78    --  108.56 -61.00-180.00   54
;
_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      -0.0066803000
_diffrn_orient_matrix_UB_12      0.0767860000
_diffrn_orient_matrix_UB_13      0.0026913000
_diffrn_orient_matrix_UB_21      0.1174343000
_diffrn_orient_matrix_UB_22      0.0048322000
_diffrn_orient_matrix_UB_23      0.0180835000
_diffrn_orient_matrix_UB_31      -0.0179571000
_diffrn_orient_matrix_UB_32      0.0030611000
_diffrn_orient_matrix_UB_33      -0.0959195000
_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  0.0386
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            38992
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.487
_diffrn_reflns_theta_min         3.568
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.372
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62664
_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            red
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_description       block
_exptl_crystal_F_000             1868
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.768
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         8544
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0474
_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^)+(0.0651P)^2^+2.2072P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1229
_refine_ls_wR_factor_ref         0.1286
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7214
_reflns_number_total             8544
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03088h2.cif
_cod_data_source_block           hfp-zjj-fc-cu
_cod_database_code               7711754
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.541
_shelx_estimated_absorpt_t_min   0.335
_reflns_odcompleteness_completeness 99.66
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O3) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C42)
\\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C29) \\sim Ueq,
Uanis(C30) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C27) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 N2(H2), C2(H2A), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10),
 C11(H11), C12(H12), 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), C37(H37),
  C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C43(H43), C45(H45),
 C46(H46), C47(H47)
;
_shelx_res_checksum              99749
_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 2.224
_oxdiff_exptl_absorpt_empirical_full_min 0.779