Development of zinc(II) 2-pyridinecarboxaldehyde thiosemicarbazone complex with remarkable antitumor and antiangiogenic activities
Jiang, Ming; Pang, Jinhui; Jia, Xiaoying; Chu, Yong; Li, Wenjuan; Liang, Hong; Yang, Feng; Dalton Transactions  (2023) –; doi:10.1039/D3DT00148B

data_7712704
_publ_section_title
;
 Development of zinc(II) 2-pyridinecarboxaldehyde thiosemicarbazone
 complex with remarkable antitumor and antiangiogenic activities
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00148B
_journal_year                    2023
_chemical_formula_moiety         'C10 H15 Cl N4 O S Zn'
_chemical_formula_sum            'C10 H15 Cl N4 O S Zn'
_chemical_formula_weight         340.14
_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
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-03-08
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-03-08 deposited with the CCDC.	2023-03-29 downloaded from the CCDC.
;
_cell_angle_alpha                101.592(4)
_cell_angle_beta                 94.606(4)
_cell_angle_gamma                97.946(4)
_cell_formula_units_Z            2
_cell_length_a                   7.5232(4)
_cell_length_b                   9.5669(4)
_cell_length_c                   9.7810(4)
_cell_measurement_reflns_used    3790
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      28.6030
_cell_measurement_theta_min      3.9630
_cell_volume                     678.74(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9784
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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    -51.00  38.00   1.00    3.00    --   17.77 -57.00-120.00   89
  2  \w     -1.00  73.00   1.00    3.00    --   17.77-121.00-148.00   74
  3  \w    -90.00  10.00   1.00    3.00    --  -19.57 -77.00 -60.00  100
  4  \w    -88.00   2.00   1.00    3.00    --  -19.57 -57.00  30.00   90
  5  \w    -93.00  25.00   1.00    3.00    --  -19.57 -19.00  90.00  118
  6  \w     -4.00  87.00   1.00    3.00    --   17.77  57.00 -90.00   91
  7  \w    -96.00 -34.00   1.00    3.00    --  -19.57 178.00 -60.00   62
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0864681000
_diffrn_orient_matrix_UB_12      -0.0143993000
_diffrn_orient_matrix_UB_13      0.0221199000
_diffrn_orient_matrix_UB_21      -0.0113115000
_diffrn_orient_matrix_UB_22      0.0297167000
_diffrn_orient_matrix_UB_23      0.0706772000
_diffrn_orient_matrix_UB_31      -0.0396425000
_diffrn_orient_matrix_UB_32      -0.0691706000
_diffrn_orient_matrix_UB_33      0.0080297000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7327
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.38
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.153
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41022
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic brownish yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.664
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             348
_exptl_crystal_preparation       'heated 343 k'
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.275
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         2392
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0253
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+0.0625P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0699
_refine_ls_wR_factor_ref         0.0720
_reflns_number_gt                2208
_reflns_number_total             2392
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d3dt00148b2.cif
_cod_data_source_block           pjh-zn-n2
_cod_original_cell_volume        678.74(5)
_cod_database_code               7712704
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O1-H1
 0.85 with sigma of 0.01
 Zn1-H1
 2.657077 with sigma of 0.02
 C00F-H1
 1.882607 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C00A(H00A), C00C(H00C), C00D(H00D), C00E(H00E), C00G(H00H)
3.b Idealised Me refined as rotating group:
 C00F(H00B,H00F,H00G), C00H(H00I,H00J,H00K), C00I(H00L,H00M,H00N)
;
_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 1.567
_oxdiff_exptl_absorpt_empirical_full_min 0.541