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_7713636
_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         '2(C20 H28 Au1.5 N7 O2 Zn2), Cl O4, H2 O'
_chemical_formula_sum            'C40 H58 Au3 Cl N14 O9 Zn4'
_chemical_formula_weight         1766.83
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-04-06
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-04-06 deposited with the CCDC.	2023-07-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 148.11(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   53.912(9)
_cell_length_b                   12.3116(3)
_cell_length_c                   31.451(5)
_cell_measurement_reflns_used    11270
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4940
_cell_measurement_theta_min      2.4400
_cell_volume                     11028(13)
_computing_cell_refinement       'CrysAlisPro 1.171.42.76a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.76a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.76a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_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 0.990
_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    -78.00 -51.00   0.50   85.00    --   -4.89 -28.00  90.00   54
  2  \w    -17.00  69.00   0.50   85.00    --   -4.89  28.00-108.00  172
  3  \w    -22.00  25.00   0.50   85.00    --   -4.89 -99.00  90.00   94
  4  \w    -26.00   4.00   0.50   85.00    --   -4.89 -28.00  90.00   60
  5  \w    -21.00   4.00   0.50   85.00    --    5.44 -19.00  60.00   50
;
_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      -0.0205463000
_diffrn_orient_matrix_UB_12      -0.0161143000
_diffrn_orient_matrix_UB_13      -0.0188263000
_diffrn_orient_matrix_UB_21      -0.0130268000
_diffrn_orient_matrix_UB_22      0.0027301000
_diffrn_orient_matrix_UB_23      -0.0381464000
_diffrn_orient_matrix_UB_31      0.0053548000
_diffrn_orient_matrix_UB_32      -0.0552457000
_diffrn_orient_matrix_UB_33      0.0036017000
_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  0.0464
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       54
_diffrn_reflns_limit_h_min       -66
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            36771
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.102
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    9.770
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.916
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.76a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
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    2.128
_exptl_crystal_description       needle
_exptl_crystal_F_000             6736
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.826
_refine_diff_density_min         -0.745
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     679
_refine_ls_number_reflns         10727
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0320
_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^)+(0.0277P)^2^+4.0903P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0642
_refine_ls_wR_factor_ref         0.0692
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8194
_reflns_number_total             10727
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01749d2.cif
_cod_data_source_block           znaudmenclo4
_cod_original_cell_volume        11028(7)
_cod_database_code               7713636
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C20 H10 N3 O4 Zn1 Au1'
_shelx_estimated_absorpt_t_max   0.696
_shelx_estimated_absorpt_t_min   0.245
_reflns_odcompleteness_completeness 98.60
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Others
 Fixed Sof: Au4(0.5) Au2(0.5)
 Fixed U12: Au4(-0) Au2(0)
 Fixed U23: Au4(0) Au2(0)
 Fixed Uiso: H3(0.077) H11(0.071) H17(0.064) H32(0.077) H5(0.078) H12A(0.099)
 H12B(0.099) H23(0.087) H27(0.086) H9A(0.141) H9B(0.141) H9C(0.141) H15A(0.114)
 H15B(0.114) H15C(0.114) H13A(0.1) H13B(0.1) H33A(0.106) H33B(0.106)
 H33C(0.106) H33D(0.106) H7A(0.086) H7B(0.086) H14A(0.148) H14B(0.148)
 H14C(0.148) H29A(0.143) H29B(0.143) H36A(0.107) H36B(0.107) H36C(0.107)
 H30A(0.21) H30B(0.21) H30C(0.21) H31A(0.207) H31B(0.207) H31C(0.207)
 H25(0.102) H28A(0.123) H28B(0.123) H16A(0.166) H16B(0.166) H16C(0.166)
 H60A(0.203) H60B(0.203) H60C(0.203) H8A(0.107) H8B(0.107) H10A(0.174)
 H10B(0.174) H10C(0.174) H35A(0.192) H35B(0.192) H35C(0.192) H34A(0.085)
 H34B(0.085) H34C(0.065) H34D(0.065) H36D(0.107) H36E(0.107) H36F(0.107)
 H9D(0.157) H9E(0.157)
 Fixed X: Au4(0.5) Au2(0.5) H3(0.406471) H11(0.450275) H17(0.473546)
 H32(0.261627) H5(0.388702) H12A(0.500928) H12B(0.538915) H23(0.244746)
 H27(0.274876) H9A(0.626882) H9B(0.635367) H9C(0.585136) H15A(0.647316)
 H15B(0.64966) H15C(0.612204) H13A(0.549557) H13B(0.581216) H33A(0.319889)
 H33B(0.264732) H33C(0.300858) H33D(0.260032) H7A(0.524458) H7B(0.571085)
 H14A(0.64368) H14B(0.602022) H14C(0.641578) H29A(0.339468) H29B(0.369243)
 H36A(0.384492) H36B(0.400631) H36C(0.380027) H30A(0.393876) H30B(0.398731)
 H30C(0.415355) H31A(0.281487) H31B(0.319227) H31C(0.313596) H25(0.254634)
 H28A(0.299639) H28B(0.27049) H16A(0.326041) H16B(0.322187) H16C(0.343517)
 H60A(0.199259) H60B(0.250634) H60C(0.227791) H8A(0.54771) H8B(0.589913)
 H10A(0.662036) H10B(0.636069) H10C(0.663254) H35A(0.32476) H35B(0.274846)
 H35C(0.302166) H34A(0.258657) H34B(0.293062) H34C(0.311523) H34D(0.352369)
 H36D(0.395189) H36E(0.368708) H36F(0.378793)
 Fixed Y: H3(-0.13348) H11(0.308312) H17(-0.215409) H32(0.882549) H5(0.185232)
 H12A(0.447158) H12B(0.401561) H23(0.790753) H27(0.355768) H9A(-0.245638) H9B(-
 0.119866) H9C(-0.165571) H15A(0.376973) H15B(0.256027) H15C(0.290948)
 H13A(0.448807) H13B(0.487576) H33A(0.983922) H33B(0.985171) H33C(0.997707)
 H33D(0.961981) H7A(-0.322852) H7B(-0.278699) H14A(0.427982) H14B(0.388956)
 H14C(0.307106) H29A(0.183268) H29B(0.255183) H36A(0.947627) H36B(0.843028)
 H36C(0.833448) H30A(0.255195) H30B(0.38152) H30C(0.323534) H31A(0.341679)
 H31B(0.381674) H31C(0.257274) H25(0.472605) H28A(0.225534) H28B(0.25539) H16A(-
 0.054409) H16B(0.070343) H16C(-0.007882) H60A(0.605203) H60B(0.599331)
 H60C(0.712303) H8A(-0.274222) H8B(-0.337481) H10A(-0.242501) H10B(-0.177604)
 H10C(-0.115199) H35A(0.771367) H35B(0.794825) H35C(0.88673) H34A(0.906154)
 H34B(1.004833) H34C(1.013515) H34D(0.968609) H36D(0.861113) H36E(0.962159)
 H36F(0.954741)
 Fixed Z: Au4(0.25) Au2(0.25) H3(0.341559) H11(0.396573) H17(0.416607) H32(-
 0.120936) H5(0.320772) H12A(0.450735) H12B(0.537441) H23(-0.209219) H27(-
 0.119355) H9A(0.505039) H9B(0.518604) H9C(0.435738) H15A(0.668655)
 H15B(0.656622) H15C(0.635978) H13A(0.467524) H13B(0.551448) H33A(0.024103)
 H33B(-0.058446) H33C(-0.016892) H33D(-0.045883) H7A(0.459425) H7B(0.547726)
 H14A(0.590717) H14B(0.501313) H14C(0.572103) H29A(0.082215) H29B(0.094404)
 H36A(0.213171) H36B(0.212281) H36C(0.228362) H30A(0.213845) H30B(0.225365)
 H30C(0.207816) H31A(0.039183) H31B(0.126842) H31C(0.109311) H25(-0.205806)
 H28A(-0.040952) H28B(-0.042543) H16A(0.234956) H16B(0.238704) H16C(0.304008)
 H60A(-0.335568) H60B(-0.278533) H60C(-0.301737) H8A(0.427429) H8B(0.509188)
 H10A(0.627687) H10B(0.625759) H10C(0.629522) H35A(0.155048) H35B(0.063507)
 H35C(0.127313) H34A(-0.002836) H34B(0.052241) H34C(0.070754) H34D(0.102298)
 H36D(0.216207) H36E(0.196237) H36F(0.162)
;
_shelx_res_checksum              51533
_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 1.421
_oxdiff_exptl_absorpt_empirical_full_min 0.660