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_7712703
_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_absolute_configuration ad
_chemical_formula_moiety         'C16 H18 N8 S2 Zn'
_chemical_formula_sum            'C16 H18 N8 S2 Zn'
_chemical_formula_weight         451.903
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_Int_Tables_number      19
_atom_sites_solution_primary     dual
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4043(8)
_cell_length_b                   12.9146(14)
_cell_length_c                   16.6007(15)
_cell_measurement_reflns_used    2852
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      25.9690
_cell_measurement_theta_min      3.8250
_cell_volume                     2016.2(3)
_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    'SHELXT 2014/4 (Sheldrick, 2014)'
_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 0.9957
_diffrn_measured_fraction_theta_max 0.9960
_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     34.00  94.00   1.00    1.50    --   17.93-178.00  30.00   60
  2  \w     35.00  94.00   1.00    1.50    --   17.93 178.00 120.00   59
  3  \w    -96.00 -34.00   1.00    1.50    --  -19.72 178.00  60.00   62
  4  \w    -12.00  24.00   1.00    1.50    --   17.93  77.00 -30.00   36
;
_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      0.0173412000
_diffrn_orient_matrix_UB_12      -0.0421331000
_diffrn_orient_matrix_UB_13      0.0256444000
_diffrn_orient_matrix_UB_21      0.0513485000
_diffrn_orient_matrix_UB_22      -0.0171369000
_diffrn_orient_matrix_UB_23      -0.0283783000
_diffrn_orient_matrix_UB_31      0.0524264000
_diffrn_orient_matrix_UB_32      0.0306782000
_diffrn_orient_matrix_UB_33      0.0191685000
_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  0.0383
_diffrn_reflns_av_unetI/netI     0.0541
_diffrn_reflns_Laue_measured_fraction_full 0.9957
_diffrn_reflns_Laue_measured_fraction_max 0.9960
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            8841
_diffrn_reflns_point_group_measured_fraction_full 0.9202
_diffrn_reflns_point_group_measured_fraction_max 0.9111
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.63
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.444
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43242
_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    1.489
_exptl_crystal_description       plate
_exptl_crystal_F_000             930.530
_exptl_crystal_preparation       'heated 343k'
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.2951
_refine_diff_density_min         -0.4792
_refine_diff_density_rms         0.0679
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   0.003(14)
_refine_ls_d_res_high            0.8107
_refine_ls_d_res_low             5.6062
_refine_ls_goodness_of_fit_ref   0.9901
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    32
_refine_ls_number_parameters     246
_refine_ls_number_reflns         3619
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.9901
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0345
_refine_ls_shift/su_max          0.0008
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0446P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0798
_refine_ls_wR_factor_ref         0.0856
_reflns_Friedel_coverage         0.798
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              15
_reflns_limit_k_min              -15
_reflns_limit_l_max              20
_reflns_limit_l_min              -20
_reflns_number_gt                3282
_reflns_number_total             3619
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3dt00148b2.cif
_cod_data_source_block           20200629-YF-PJH-ZNN1
_cod_original_sg_symbol_Hall     ' P 2ac 2ab'
_cod_database_code               7712703
_reflns_odcompleteness_completeness 99.49
_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
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N009(H009), N4(H4), C00C(H00C), C00G(H00G), C00H(H00H), C00I(H00I),
 C00J(H00J), C00K(H00K), C00L(H00L), C00M(H00M), C00P(H00P), C00Q(H00Q)
2.b Idealised Me refined as rotating group:
 C00O(H00a,H00b,H00d), C00R(H00e,H00f,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 1.553
_oxdiff_exptl_absorpt_empirical_full_min 0.643