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_7711755
_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         'C88 H74 Cu2 N4 O2 P4, 2(N O3), 2(C H4 O)'
_chemical_formula_sum            'C90 H82 Cu2 N6 O10 P4'
_chemical_formula_weight         1658.57
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-10-20
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-10-25 deposited with the CCDC.	2022-11-14 downloaded from the CCDC.
;
_cell_angle_alpha                80.4720(10)
_cell_angle_beta                 82.9410(10)
_cell_angle_gamma                65.549(2)
_cell_formula_units_Z            1
_cell_length_a                   11.7360(2)
_cell_length_b                   12.9128(3)
_cell_length_c                   15.1245(2)
_cell_measurement_reflns_used    26739
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      76.8350
_cell_measurement_theta_min      2.9580
_cell_volume                     2053.92(7)
_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 2018/3 (Sheldrick, 2015)'
_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 0.989
_diffrn_measured_fraction_theta_max 0.927
_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    -41.10  27.00   0.15    0.14    --  -47.12  37.00  30.00  454
  2  \w    -38.00  26.05   0.15    0.14    --  -47.12  37.00 150.00  427
  3  \w    -43.00 -16.00   0.15    0.55    --  -88.50  45.00  90.00  180
  4  \w    -51.00 -18.00   0.15    0.55    --  -88.50  45.00 150.00  220
  5  \w    -74.00 -47.00   0.15    0.55    --  -88.50 111.00 125.00  180
  6  \w    -80.00 -53.00   0.15    0.14    --  -47.12 111.00 125.00  180
  7  \w    -50.00  -2.00   0.15    0.14    --  -47.12 111.00 125.00  320
  8  \w    -50.00 -23.00   0.15    0.55    --  -88.50  45.00  60.00  180
  9  \w    -71.00 -26.00   0.15    0.55    --  -88.50  61.00  60.00  300
 10  \w    -85.00 -47.05   0.15    0.55    --  -88.50 125.00 150.00  253
 11  \w    -42.00  27.00   0.15    0.14    --  -47.12  37.00 -90.00  460
 12  \w    -50.00 -18.05   0.15    0.55    --  -88.50  45.00-120.00  213
 13  \w    -50.00 -17.00   0.15    0.55    --  -88.50  45.00-150.00  220
 14  \w    -47.00 -14.90   0.15    0.55    --  -88.50 125.00-180.00  214
 15  \w   -107.00 -80.90   0.15    0.55    --  -88.50 -15.00-120.00  174
 16  \w   -108.00 -72.00   0.15    0.55    --  -88.50 -61.00-120.00  240
 17  \w   -113.00 -83.90   0.15    0.14    --  -47.12-125.00-180.00  194
 18  \w   -150.00-112.95   0.15    0.55    --  -88.50 -61.00-120.00  247
 19  \w   -154.00 -82.90   0.15    0.55    --  -88.50 -94.00-180.00  474
 20  \w   -157.00-109.90   0.15    0.55    --  -88.50 -15.00-120.00  314
 21  \w   -163.00 -73.00   0.15    0.55    --  -88.50 -30.00 -60.00  600
 22  \w   -129.00 -96.90   0.15    0.55    --  -88.50-111.00  31.00  214
 23  \w   -126.00 -75.00   0.15    0.55    --  -88.50 -45.00  90.00  340
 24  \w     38.00  63.05   0.15    0.14    --   47.12-111.00  31.00  167
 25  \w     38.00  92.00   0.15    0.14    --   47.12-125.00   0.00  360
 26  \w     46.00  83.05   0.15    0.14    --   47.12-125.00 -60.00  247
 27  \w     75.00 107.10   0.15    0.55    --  108.56-111.00  31.00  214
 28  \w     62.00 106.25   0.15    0.55    --  108.56-125.00  90.00  295
 29  \w     80.00 106.10   0.15    0.55    --  108.56-117.00 140.29  174
 30  \w     84.00 123.00   0.15    0.55    --  108.56-142.00 158.80  260
 31  \w     68.00 105.05   0.15    0.55    --  108.56 -77.00 150.00  247
 32  \w     52.00  77.20   0.15    0.55    --  108.56-142.00 158.80  168
 33  \w     36.00 106.05   0.15    0.55    --  108.56-104.00 105.59  467
 34  \w     41.00  68.00   0.15    0.55    --  108.56 -61.00  30.00  180
 35  \w     42.00  88.05   0.15    0.55    --  108.56 -94.00 -30.00  307
 36  \w     45.00  70.05   0.15    0.55    --  108.56 -61.00 -60.00  167
 37  \w     46.00 100.00   0.15    0.55    --  108.56 -94.00-120.00  360
 38  \w     81.00 108.00   0.15    0.55    --  108.56-109.00 -95.91  180
 39  \w     39.00 108.00   0.15    0.55    --  108.56-125.00-120.00  460
 40  \w     42.00  68.10   0.15    0.55    --  108.56-109.00 -95.91  174
 41  \w     37.00 104.05   0.15    0.55    --  108.56 -94.00 -60.00  447
 42  \w     37.00 111.10   0.15    0.55    --  108.56-125.00-180.00  494
 43  \w     36.00  66.00   0.15    0.55    --  108.56 -61.00-120.00  200
 44  \w     37.00  66.10   0.15    0.55    --  108.56 -61.00   0.00  194
 45  \w     36.00 114.00   0.15    0.55    --  108.56   0.00   0.00  520
 46  \w    124.00 177.25   0.15    0.55    --  108.56   0.00   0.00  355
 47  \w    135.00 160.95   0.15    0.55    --  108.56 111.00 125.00  173
 48  \w    103.00 128.95   0.15    0.55    --  108.56 111.00 125.00  173
 49  \w     45.00  70.05   0.15    0.55    --  108.56 -61.00 120.00  167
;
_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      0.1366659000
_diffrn_orient_matrix_UB_12      -0.0343284000
_diffrn_orient_matrix_UB_13      0.0219858000
_diffrn_orient_matrix_UB_21      -0.0316761000
_diffrn_orient_matrix_UB_22      -0.0382927000
_diffrn_orient_matrix_UB_23      0.0984771000
_diffrn_orient_matrix_UB_31      0.0344843000
_diffrn_orient_matrix_UB_32      -0.1217084000
_diffrn_orient_matrix_UB_33      -0.0229262000
_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  0.0502
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.927
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26739
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.927
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.493
_diffrn_reflns_theta_min         2.968
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.883
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80753
_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 light yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_description       block
_exptl_crystal_F_000             862
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.777
_refine_diff_density_min         -0.579
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     507
_refine_ls_number_reflns         8091
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0491
_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^)+(0.0849P)^2^+0.4489P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1430
_refine_ls_wR_factor_ref         0.1539
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6680
_reflns_number_total             8091
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03088h2.cif
_cod_data_source_block           20201222-hfp-zjj-ph-cu
_cod_database_code               7711755
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C92 H84 Cu2 N4 O10 P4 '
_shelx_estimated_absorpt_t_max   0.820
_shelx_estimated_absorpt_t_min   0.682
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 N2(H2), C0AA(H0AA), C2(H2A), C3(H3), C4(H4), C5(H5), C7(H7), C10(H10),
 C11(H11), C12(H12), C13(H13), C14(H14), C16(H16), C17(H17), C18(H18), C19(H19),
  C20(H20), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C28(H28),
 C29(H29), C30(H30), C31(H31), C32(H32), C34(H34), C35(H35), C36(H36), C37(H37),
  C38(H38), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44)
1.b Idealised Me refined as rotating group:
 C45(H45A,H45B,H45C)
1.c Idealised tetrahedral OH refined as rotating group:
 O5(H5A)
;
_shelx_res_checksum              90118
_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 2.964
_oxdiff_exptl_absorpt_empirical_full_min 0.390