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_7712705
_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         'C13 H12 Cl2 N4 S Zn'
_chemical_formula_sum            'C13 H12 Cl2 N4 S Zn'
_chemical_formula_weight         392.634
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_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                82.285(8)
_cell_angle_beta                 82.036(7)
_cell_angle_gamma                89.835(8)
_cell_formula_units_Z            2
_cell_length_a                   7.2908(6)
_cell_length_b                   9.6604(10)
_cell_length_c                   10.9647(10)
_cell_measurement_reflns_used    1325
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      20.8340
_cell_measurement_theta_min      3.5440
_cell_volume                     757.80(12)
_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  'olex2.refine 1.3 (Bourhis et al., 2015)'
_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 0.9978
_diffrn_measured_fraction_theta_max 0.9978
_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    -15.00  63.00   1.00    2.00    --   17.93-105.00 138.00   78
  2  \w    -90.00  10.00   1.00    2.00    --  -19.72 -77.00-120.00  100
  3  \w    -89.00   2.00   1.00    2.00    --  -19.72 -57.00 -30.00   91
  4  \w    -45.00  53.00   1.00    2.00    --  -19.72  38.00-120.00   98
  5  \w    -93.00  24.00   1.00    2.00    --  -19.72 -19.00  30.00  117
  6  \w    -65.00 -10.00   1.00    2.00    --  -19.72 105.00-121.00   55
  7  \w    -41.00  49.00   1.00    2.00    --  -19.72  57.00   0.00   90
;
_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      0.0019335000
_diffrn_orient_matrix_UB_12      -0.0279602000
_diffrn_orient_matrix_UB_13      0.0630136000
_diffrn_orient_matrix_UB_21      0.0481802000
_diffrn_orient_matrix_UB_22      0.0606373000
_diffrn_orient_matrix_UB_23      0.0091063000
_diffrn_orient_matrix_UB_31      -0.0855999000
_diffrn_orient_matrix_UB_32      0.0321358000
_diffrn_orient_matrix_UB_33      0.0170977000
_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  0.0773
_diffrn_reflns_av_unetI/netI     0.1186
_diffrn_reflns_Laue_measured_fraction_full 0.9978
_diffrn_reflns_Laue_measured_fraction_max 0.9978
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9926
_diffrn_reflns_point_group_measured_fraction_full 0.9978
_diffrn_reflns_point_group_measured_fraction_max 0.9978
_diffrn_reflns_theta_full        24.9997
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.51
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.108
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52024
_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 yellowish yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             397.591
_exptl_crystal_preparation       'heated 343 k'
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.6742
_refine_diff_density_min         -0.7075
_refine_diff_density_rms         0.1647
_refine_ls_d_res_high            0.8409
_refine_ls_d_res_low             5.8087
_refine_ls_goodness_of_fit_ref   1.0123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    24
_refine_ls_number_parameters     190
_refine_ls_number_reflns         2675
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0123
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_gt           0.0505
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0330P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0896
_refine_ls_wR_factor_ref         0.1147
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              8
_reflns_limit_h_min              -8
_reflns_limit_k_max              11
_reflns_limit_k_min              -11
_reflns_limit_l_max              13
_reflns_limit_l_min              0
_reflns_number_gt                1780
_reflns_number_total             2675
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3dt00148b2.cif
_cod_data_source_block           20191230-PJH-ZN-N6AAA
_cod_database_code               7712705
_reflns_odcompleteness_completeness 99.81
_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 N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N4(H4), N3(H3), C009(H009), C00D(H00D), C00E(H00E), C00F(H00F), C00G(H00G),
 C00H(H00H), C00I(H00I), C00J(H00J), C00K(H00K), C00L(H00L)
;
_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 2.486
_oxdiff_exptl_absorpt_empirical_full_min 0.478