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_7712701
_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         'C28 H26 N8 S2 Zn, C H4 O, H2 O'
_chemical_formula_sum            'C29 H32 N8 O2 S2 Zn'
_chemical_formula_weight         654.11
_chemical_name_systematic        1
_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     dual
_audit_creation_date             2023-03-01
_audit_creation_method
;
Olex2 1.5
(compiled 2023.02.24 svn.rf166f9f3 for OlexSys, GUI svn.r6725)
;
_audit_update_record
;
2023-03-08 deposited with the CCDC.	2023-03-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.745(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.610(4)
_cell_length_b                   18.595(4)
_cell_length_c                   11.731(3)
_cell_measurement_reflns_used    9736
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      26.468
_cell_measurement_theta_min      2.191
_cell_volume                     3051.9(13)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_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 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15179
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.480
_diffrn_reflns_theta_min         1.822
_diffrn_source_current           45.0
_diffrn_source_power             2.25
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.983
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dull dark brown'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_description       plate
_exptl_crystal_F_000             1360
_exptl_crystal_preparation       'heated 343 k'
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.235
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         3154
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0266
_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^)+(0.0367P)^2^+2.4179P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0695
_refine_ls_wR_factor_ref         0.0725
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2883
_reflns_number_total             3154
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00148b2.cif
_cod_data_source_block           bbbb
_cod_original_cell_volume        3052.0(11)
_cod_database_code               7712701
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.891
_shelx_estimated_absorpt_t_min   0.777
_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 O(H) groups, All O(H,H) groups
2. Restrained distances
 O2-C
 1.5 with sigma of 0.02
3. Rigid bond restraints
 S002, Zn01
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0002
4. Others
 Fixed Sof: O2(0.5) H2(0.5) O1(0.5) H1A(0.5) H1B(0.5) C(0.5) HA(0.5) HB(0.5)
 HC(0.5)
5.a Free rotating group:
 O1(H1A,H1B)
5.b Aromatic/amide H refined with riding coordinates:
 N005(H005), C00A(H00A), C00C(H00C), C00D(H00D), C00E(H00E), C00F(H00F),
 C00G(H00G), C00I(H00J), C00J(H00K), C00K(H00L)
5.c Idealised Me refined as rotating group:
 C00H(H00B,H00H,H00I), C(HA,HB,HC)
5.d Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_shelx_res_checksum              37529
_shelx_hkl_checksum              81553
_olex2_submission_special_instructions 'No special instructions were received'