Mitochondria-mediated anti-proliferation of triple-negative breast cancer cells by Pd(II)-, Pt(II)-, and Au(III)-NHC complexes of NCN pincers.
Sahu, Priyanka; Jana, Narayan Ch; Das, Ananya; Chatterjee, Nabanita; Gach-Janczak, Katarzyna; Dinda, Joydev; Dalton transactions (Cambridge, England : 2003) 54 (2025) 10003–10021; doi:10.1039/d5dt00471c

data_7718846
_publ_section_title
;
 Mitochondria-mediated anti-proliferation of triple-negative breast cancer
 cells by Pd(II)-, Pt(II)-, and Au(III)-NHC complexes of NCN pincers.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10003
_journal_page_last               10021
_journal_paper_doi               10.1039/d5dt00471c
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety
'C21 H20 Cl N6 Pd, F6 P, C1.5 H3.75 O0.375, 0.25(C2 H3 N)'
_chemical_formula_sum            'C23 H24.5 Cl F6 N6.25 O0.38 P Pd'
_chemical_formula_weight         681.31
_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             2025-04-08
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-05-06 deposited with the CCDC.	2025-05-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.749(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.0097(10)
_cell_length_b                   7.9195(3)
_cell_length_c                   28.7829(12)
_cell_measurement_reflns_used    23014
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      32.2910
_cell_measurement_theta_min      1.8300
_cell_volume                     5118.0(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.845
_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     24.00  76.00   0.50   47.88    --    7.63-158.00 144.00  104
  2  \w      0.00  54.00   0.50   47.88    --    7.63-118.00 -61.00  108
  3  \w    -59.00  11.00   0.50   47.88    --    7.63 -37.00-150.00  140
  4  \w    -42.00  15.00   0.50   47.88    --   -8.26 -77.00 -60.00  114
  5  \w    -42.00  12.00   0.50   47.88    --   -8.26 -77.00   0.00  108
  6  \w     -8.00  54.00   0.50   47.88    --   -8.26  37.00 150.00  124
  7  \w    -41.00  15.00   0.50   47.88    --   -8.26 -77.00-180.00  112
  8  \w    -42.00  15.00   0.50   47.88    --   -8.26 -77.00  90.00  114
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0516
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.845
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            36608
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.845
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.959
_diffrn_reflns_theta_min         2.727
_exptl_absorpt_coefficient_mu    0.965
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.35523
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light white'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.768
_exptl_crystal_description       block
_exptl_crystal_F_000             2730
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.232
_refine_diff_density_min         -0.685
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         7478
_refine_ls_number_restraints     202
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0339
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0359P)^2^+15.3346P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0834
_refine_ls_wR_factor_ref         0.0849
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6880
_reflns_number_total             7478
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00471c2.cif
_cod_data_source_block           complex-2
_cod_depositor_comments
'Adding full bibliography for 7718845--7718846.cif.'
_cod_original_formula_sum        'C23 H24.50 Cl F6 N6.25 O0.38 P Pd'
_cod_database_code               7718846
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.910
_shelx_estimated_absorpt_t_min   0.830
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 P1B-F3 \\sim P1B-F3A
 with sigma of 0.02
 P1B-F1 \\sim P1B-F6A
 with sigma of 0.02
 P1B-F5 \\sim P1B-F5A
 with sigma of 0.02
 P1B-F2 \\sim P1B-F2A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C25) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(N7) \\sim Ueq, Uanis(O1)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C22) \\sim Ueq, Uanis(C23) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(F2A) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(P1B)
\\sim Ueq, Uanis(F3A) \\sim Ueq, Uanis(F1B) \\sim Ueq, Uanis(F1) \\sim Ueq,
Uanis(F5A) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F4A) \\sim Ueq, Uanis(F6A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F1A) \\sim Ueq, Uanis(F1B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(P1A) \\sim Ueq, Uanis(P1B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(F1) \\sim Ueq, Uanis(F5A) \\sim Ueq, Uanis(F4A) \\sim Ueq, Uanis(F5)
\\sim Ueq, Uanis(F6A) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F2A) \\sim Ueq,
Uanis(F2) \\sim Ueq, Uanis(F3A) \\sim Ueq, Uanis(F1A) \\sim Ueq, Uanis(F1B)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C25, C24, N7, O1
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O1, C22, C23
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F2A, F2, F3, F6A, P1B, F5, F3A, F5A, F1, F4A, F1B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 P1A, P1B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F4
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Fixed Sof: P1B(0.75) F3(0.75) F1(0.75) F1B(0.75) F5(0.75) F2(0.75) O1(0.375)
 N7(0.25) C24(0.25) C25(0.25) H25A(0.25) H25B(0.25) H25C(0.25) C22(0.75)
 H22A(0.75) H22B(0.75) C23(0.75) H23A(0.75) H23B(0.75) H23C(0.75) F3A(0.25)
 F2A(0.25) F4A(0.25) F6A(0.75) F5A(0.25) F1A(0.25) P1A(0.25) F4(0.25)
6.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C13(H13A,H13B), C22(H22A,H22B)
6.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C11(H11), C12(H12), C18(H18), C20(H20), C5(H5), C2(H2), C3(H3),
 C19(H19), C4(H4)
6.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C15(H15A,H15B,H15C), C25(H25A,H25B,H25C), C23(H23A,H23B,H23C)
;
_shelx_res_checksum              80895
_shelx_hkl_checksum              18225
_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
;