Homo- and heterometallic complexes of Zn(II), {Zn(II)Au(I)}, and {Zn(II)Ag(I)} with pentadentate Schiff base ligands as promising anticancer agents
Zhivkova, Tania; Culita, Daniela; Abudalleh, Abedulkadir; Dyakova, Lora; Mocanu, Teodora; Madalan, Augustin M.; Georgieva, Milena; Miloshev, George; Hanganu, Anamaria; Marinescu, Gabriela; Alexandrova, Radostina; Dalton Transactions  (2023) –; doi:10.1039/D3DT01749D

data_7713635
_publ_section_title
;
 Homo- and heterometallic complexes of Zn(II), {Zn(II)Au(I)}, and
 {Zn(II)Ag(I)} with pentadentate Schiff base ligands as promising
 anticancer agents
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01749D
_journal_year                    2023
_chemical_formula_moiety         'C19 H28 Ag N6 O2 Zn2, Cl O4'
_chemical_formula_sum            'C19 H28 Ag Cl N6 O6 Zn2'
_chemical_formula_weight         710.53
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-04-06 deposited with the CCDC.	2023-07-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.756(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.9935(8)
_cell_length_b                   15.8675(8)
_cell_length_c                   10.9844(5)
_cell_measurement_reflns_used    8644
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.9020
_cell_measurement_theta_min      2.3910
_cell_volume                     2695.6(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_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)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_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 0.991
_diffrn_measured_fraction_theta_max 0.987
_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    -10.00  28.00   0.50   12.00    --   -4.82 -99.00 -30.00   76
  2  \w    -14.00  58.00   0.50   12.00    --   -4.82  37.00  60.00  144
  3  \w    -12.00  63.00   0.50   12.00    --    5.36  77.00 120.00  150
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0415826000
_diffrn_orient_matrix_UB_12      0.0082367000
_diffrn_orient_matrix_UB_13      0.0398862000
_diffrn_orient_matrix_UB_21      0.0095495000
_diffrn_orient_matrix_UB_22      -0.0437134000
_diffrn_orient_matrix_UB_23      0.0020544000
_diffrn_orient_matrix_UB_31      0.0167953000
_diffrn_orient_matrix_UB_32      0.0044616000
_diffrn_orient_matrix_UB_33      -0.0535184000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            15664
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.307
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.627
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30761
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.73a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.751
_exptl_crystal_description       needle
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.699
_refine_diff_density_min         -0.615
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         5229
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0392
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0682P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1105
_refine_ls_wR_factor_ref         0.1163
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4216
_reflns_number_total             5229
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01749d2.cif
_cod_data_source_block           zn_ag_dmen1_auto
_cod_database_code               7713635
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.649
_shelx_estimated_absorpt_t_min   0.487
_reflns_odcompleteness_completeness 98.53
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H2-O2
 0.98 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C16B \\sim C16A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
C15B \\sim C15A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
4. Others
 Sof(H13C)=Sof(H13D)=Sof(C14B)=Sof(H14C)=Sof(H14D)=Sof(C15B)=Sof(H15D)=
 Sof(H15E)=Sof(H15F)=Sof(C16B)=Sof(H16D)=Sof(H16E)=Sof(H16F)=1-FVAR(1)
 Sof(H13A)=Sof(H13B)=Sof(C14A)=Sof(H14A)=Sof(H14B)=Sof(C15A)=Sof(H15A)=
 Sof(H15B)=Sof(H15C)=Sof(C16A)=Sof(H16A)=Sof(H16B)=Sof(H16C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C8(H8A,H8B), C13(H13A,H13B), C13(H13C,H13D), C14A(H14A,H14B),
 C14B(H14C,H14D)
5.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C12(H12), C3(H3), C5(H5)
5.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C15A(H15A,H15B,
 H15C), C16A(H16A,H16B,H16C), C15B(H15D,H15E,H15F), C16B(H16D,H16E,H16F)
;
_shelx_res_checksum              68262
_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 2.061
_oxdiff_exptl_absorpt_empirical_full_min 0.373