Physical properties and cytotoxicity of Cu(ii) and Zn(ii) complexes with a TMS-substituted indolo[2,3-c]quinoline-derived Schiff base
Wittmann, Christopher; Besleaga, Iuliana; Mahmoudi, Soheil; Palamarciuc, Oleg; Balan-Porcarasu, Mihaela; Dascalu, Mihaela; Shova, Sergiu; Cazacu, Maria; Kiricsi, Mónika; Igaz, Nóra; Dömötör, Orsolya; Enyedy, Eva A.; Dvoranová, Dana; Rapta, Peter; Arion, Vladimir B.; Dalton Transactions 54 (2025) 7882–7898; doi:10.1039/D5DT00314H

data_7718476
_publ_section_title
;
 Physical properties and cytotoxicity of Cu(ii) and Zn(ii) complexes with
 a TMS-substituted indolo[2,3-c]quinoline-derived Schiff base
;
_journal_issue                   19
_journal_name_full               'Dalton Transactions'
_journal_page_first              7882
_journal_page_last               7898
_journal_paper_doi               10.1039/D5DT00314H
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C22 H17 Cl2 N5 Zn, 1.5(C2 H6 O S)'
_chemical_formula_sum            'C25 H26 Cl2 N5 O1.5 S1.5 Zn'
_chemical_formula_weight         604.87
_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             2025-01-22
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-01-22 deposited with the CCDC.	2025-04-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.352(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3995(5)
_cell_length_b                   14.5451(3)
_cell_length_c                   14.9042(4)
_cell_measurement_reflns_used    5307
_cell_measurement_temperature    299.18(10)
_cell_measurement_theta_max      69.0590
_cell_measurement_theta_min      3.5360
_cell_volume                     2686.53(16)
_computing_cell_refinement       'CrysAlisPro 1.171.43.137a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.137a 64-bit (release 10-09-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.137a (Rigaku OD, 2024)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      299.18(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.919
_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    -17.00  10.00   0.50   30.00    --  -47.51  77.00-123.00   54
  2  \w   -117.00 -25.00   0.50   30.00    --  -47.51 -77.00 110.00  184
  3  \w    -69.00 -30.00   0.50   30.00    --  -47.51  77.00-123.00   78
  4  \w     16.00  43.00   0.50   30.00    --   47.51 -77.00 110.00   54
  5  \w   -161.00-135.00   0.50   40.00    --  -91.75 -77.00 110.00   52
  6  \w    -82.00 -20.00   0.50   40.00    --  -91.75  77.00-123.00  124
  7  \w     87.00 178.00   0.50   40.00    --  106.68  77.00-123.00  182
  8  \w     51.00 105.00   0.50   40.00    --  106.68 -77.00 110.00  108
  9  \w    -22.00  26.00   0.50   30.00    --  -47.51  19.00-120.00   96
 10  \w    -27.00  22.00   0.50   30.00    --   47.51 -19.00-120.00   98
 11  \w     48.00  73.00   0.50   30.00    --   47.51  77.00-123.00   50
 12  \w    -53.00 -19.00   0.50   40.00    --  -91.75  61.00  30.00   68
 13  \w    -49.00 -23.00   0.50   40.00    --  -91.75  45.00   0.00   52
 14  \w    -74.00 -25.00   0.50   40.00    --  -91.75 125.00 150.00   98
 15  \w    -51.00 -21.00   0.50   40.00    --  -91.75  45.00  90.00   60
 16  \w    -46.00 -20.00   0.50   40.00    --  -91.75  45.00  60.00   52
 17  \w    -50.00 -22.00   0.50   40.00    --  -91.75  45.00-180.00   56
 18  \w    -49.00 -21.00   0.50   40.00    --  -91.75  45.00  30.00   56
 19  \w     35.00  65.00   0.50   40.00    --  106.68 -61.00 120.00   60
 20  \w     84.00 165.00   0.50   40.00    --  106.68  77.00-180.00  162
 21  \w     40.00  65.00   0.50   40.00    --  106.68 -61.00-120.00   50
 22  \w    102.00 177.00   0.50   40.00    --  106.68  15.00 150.00  150
 23  \w     95.00 169.00   0.50   40.00    --  106.68  15.00-180.00  148
;
_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      -0.0106526000
_diffrn_orient_matrix_UB_12      -0.0877265000
_diffrn_orient_matrix_UB_13      0.0535943000
_diffrn_orient_matrix_UB_21      -0.1237296000
_diffrn_orient_matrix_UB_22      0.0097696000
_diffrn_orient_matrix_UB_23      -0.0438419000
_diffrn_orient_matrix_UB_31      -0.0048676000
_diffrn_orient_matrix_UB_32      -0.0585465000
_diffrn_orient_matrix_UB_33      -0.0877465000
_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  0.0499
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.919
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17121
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.919
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.360
_diffrn_reflns_theta_min         3.567
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.439
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62004
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.137a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_description       plate
_exptl_crystal_F_000             1244
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.868
_refine_diff_density_min         -0.702
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       0.00040(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         5233
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0957
_refine_ls_R_factor_gt           0.0615
_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^)+(0.0930P)^2^+2.3841P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1582
_refine_ls_wR_factor_ref         0.1809
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3478
_reflns_number_total             5233
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00314h2.cif
_cod_data_source_block           shs_856_olpa_autored
_cod_depositor_comments
'Adding full bibliography for 7718475--7718477.cif.'
_cod_original_cell_volume        2686.52(14)
_cod_original_formula_sum        'C25 H26 Cl2 N5 O1.50 S1.50 Zn'
_cod_database_code               7718476
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C20H20N6O2S1Cl2Zn1
_chemical_oxdiff_usercomment     OlPa_136
_shelx_estimated_absorpt_t_max   0.957
_shelx_estimated_absorpt_t_min   0.809
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 S2X-C42 \\sim S2-C42
 with sigma of 0.01
 S2-O2A \\sim S2X-O2B
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(S2) = Uanis(S2X)
Uanis(O2A) = Uanis(O2B)
4. Others
 Sof(H42D)=Sof(H42E)=Sof(H42F)=1-FVAR(1)
 Sof(S2)=Sof(O2A)=0.5*(1-FVAR(2))
 Sof(S2X)=Sof(O2B)=0.5*FVAR(2)
 Sof(H42A)=Sof(H42B)=Sof(H42C)=FVAR(1)
5.a Riding coordinates:
 N7(H7), N12(H12), C21(H21A,H21B,H21C), C41(H41A,H41B,H41C), C40(H40A,H40B,
 H40C), C42(H42D,H42E,H42F), C42(H42A,H42B,H42C)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C8(H8), C9(H9), C10(H10), C11(H11), C17(H17),
 C18(H18), C19(H19), C20(H20)
;
_shelx_res_checksum              84762
_shelx_hkl_checksum              64805
_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 1.514
_oxdiff_exptl_absorpt_empirical_full_min 0.639