#------------------------------------------------------------------------------
#$Date: 2023-03-30 02:17:18 +0300 (Thu, 30 Mar 2023) $
#$Revision: 282130 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/27/7712704.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7712704
loop_
_publ_author_name
'Jiang, Ming'
'Pang, Jinhui'
'Jia, Xiaoying'
'Chu, Yong'
'Li, Wenjuan'
'Liang, Hong'
'Yang, Feng'
_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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -51.00  38.00   1.00    3.00    --   17.77 -57.00-120.00   89
  2  ω     -1.00  73.00   1.00    3.00    --   17.77-121.00-148.00   74
  3  ω    -90.00  10.00   1.00    3.00    --  -19.57 -77.00 -60.00  100
  4  ω    -88.00   2.00   1.00    3.00    --  -19.57 -57.00  30.00   90
  5  ω    -93.00  25.00   1.00    3.00    --  -19.57 -19.00  90.00  118
  6  ω     -4.00  87.00   1.00    3.00    --   17.77  57.00 -90.00   91
  7  ω    -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       'ω 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/[σ²(Fo²)+(0.0430P)²+0.0625P] where P=(Fo²+2Fc²)/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
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.23915(3) 0.38378(2) 0.67197(2) 0.03039(11) Uani 1 1 d D . .
S1 S 0.29289(10) 0.16830(6) 0.52338(6) 0.04394(18) Uani 1 1 d . . .
Cl1 Cl 0.07220(9) 0.29554(6) 0.82803(7) 0.04876(18) Uani 1 1 d . . .
O1 O 0.4889(2) 0.46731(16) 0.78106(15) 0.0342(3) Uani 1 1 d D . .
H1 H 0.562(2) 0.525(2) 0.747(2) 0.051 Uiso 1 1 d D . .
N2 N 0.2613(2) 0.45345(17) 0.47881(17) 0.0277(4) Uani 1 1 d . . .
N3 N 0.3057(2) 0.36979(17) 0.36050(17) 0.0294(4) Uani 1 1 d . . .
N1 N 0.1651(2) 0.59910(18) 0.71253(18) 0.0312(4) Uani 1 1 d . . .
N4 N 0.3483(2) 0.14275(18) 0.25659(18) 0.0349(4) Uani 1 1 d . . .
C009 C 0.1906(3) 0.6695(2) 0.6076(2) 0.0304(5) Uani 1 1 d . . .
C00A C 0.2384(3) 0.5835(2) 0.4784(2) 0.0314(5) Uani 1 1 d . . .
H00A H 0.2517 0.6219 0.3990 0.038 Uiso 1 1 calc R . .
C00B C 0.3173(3) 0.2332(2) 0.3730(2) 0.0291(5) Uani 1 1 d . . .
C00C C 0.1697(3) 0.8125(2) 0.6200(3) 0.0402(6) Uani 1 1 d . . .
H00C H 0.1851 0.8579 0.5452 0.048 Uiso 1 1 calc R . .
C00D C 0.1252(3) 0.8870(3) 0.7466(3) 0.0461(6) Uani 1 1 d . . .
H00D H 0.1135 0.9842 0.7589 0.055 Uiso 1 1 calc R . .
C00E C 0.1189(3) 0.6714(2) 0.8321(2) 0.0385(5) Uani 1 1 d . . .
H00E H 0.0994 0.6231 0.9044 0.046 Uiso 1 1 calc R . .
C00F C 0.5917(4) 0.3923(3) 0.8615(3) 0.0480(6) Uani 1 1 d D . .
H00B H 0.6511 0.3269 0.8000 0.072 Uiso 1 1 calc R . .
H00F H 0.5131 0.3389 0.9121 0.072 Uiso 1 1 calc R . .
H00G H 0.6804 0.4605 0.9267 0.072 Uiso 1 1 calc R . .
C00G C 0.0988(3) 0.8153(3) 0.8529(3) 0.0435(6) Uani 1 1 d . . .
H00H H 0.0677 0.8629 0.9382 0.052 Uiso 1 1 calc R . .
C00H C 0.3694(4) -0.0063(2) 0.2553(3) 0.0478(6) Uani 1 1 d . . .
H00I H 0.4319 -0.0115 0.3432 0.072 Uiso 1 1 calc R . .
H00J H 0.4376 -0.0406 0.1802 0.072 Uiso 1 1 calc R . .
H00K H 0.2526 -0.0651 0.2418 0.072 Uiso 1 1 calc R . .
C00I C 0.3632(4) 0.1884(3) 0.1244(2) 0.0439(6) Uani 1 1 d . . .
H00L H 0.2858 0.2590 0.1174 0.066 Uiso 1 1 calc R . .
H00M H 0.3276 0.1063 0.0478 0.066 Uiso 1 1 calc R . .
H00N H 0.4859 0.2298 0.1206 0.066 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 Zn1 S1 101.85(2) . . ?
O1 Zn1 S1 102.87(5) . . ?
O1 Zn1 Cl1 105.33(5) . . ?
O1 Zn1 N2 102.23(6) . . ?
O1 Zn1 N1 89.59(6) . . ?
N2 Zn1 S1 79.31(5) . . ?
N2 Zn1 Cl1 151.33(5) . . ?
N2 Zn1 N1 75.38(6) . . ?
N1 Zn1 S1 153.67(5) . . ?
N1 Zn1 Cl1 96.94(5) . . ?
C00B S1 Zn1 98.31(7) . . ?
Zn1 O1 H1 118.7(12) . . ?
C00F O1 Zn1 124.74(14) . . ?
C00F O1 H1 108.8(12) . . ?
N3 N2 Zn1 123.66(12) . . ?
C00A N2 Zn1 117.02(14) . . ?
C00A N2 N3 119.25(17) . . ?
C00B N3 N2 113.18(16) . . ?
C009 N1 Zn1 113.92(14) . . ?
C00E N1 Zn1 127.38(15) . . ?
C00E N1 C009 118.22(18) . . ?
C00B N4 C00H 122.05(18) . . ?
C00B N4 C00I 121.87(18) . . ?
C00I N4 C00H 116.08(18) . . ?
N1 C009 C00A 115.56(18) . . ?
N1 C009 C00C 122.3(2) . . ?
C00C C009 C00A 122.1(2) . . ?
N2 C00A C009 117.45(19) . . ?
N2 C00A H00A 121.3 . . ?
C009 C00A H00A 121.3 . . ?
N3 C00B S1 125.28(16) . . ?
N4 C00B S1 118.81(15) . . ?
N4 C00B N3 115.90(18) . . ?
C009 C00C H00C 120.7 . . ?
C009 C00C C00D 118.6(2) . . ?
C00D C00C H00C 120.7 . . ?
C00C C00D H00D 120.5 . . ?
C00G C00D C00C 119.0(2) . . ?
C00G C00D H00D 120.5 . . ?
N1 C00E H00E 118.7 . . ?
N1 C00E C00G 122.6(2) . . ?
C00G C00E H00E 118.7 . . ?
O1 C00F H00B 109.5 . . ?
O1 C00F H00F 109.5 . . ?
O1 C00F H00G 109.5 . . ?
H00B C00F H00F 109.5 . . ?
H00B C00F H00G 109.5 . . ?
H00F C00F H00G 109.5 . . ?
C00D C00G C00E 119.2(2) . . ?
C00D C00G H00H 120.4 . . ?
C00E C00G H00H 120.4 . . ?
N4 C00H H00I 109.5 . . ?
N4 C00H H00J 109.5 . . ?
N4 C00H H00K 109.5 . . ?
H00I C00H H00J 109.5 . . ?
H00I C00H H00K 109.5 . . ?
H00J C00H H00K 109.5 . . ?
N4 C00I H00L 109.5 . . ?
N4 C00I H00M 109.5 . . ?
N4 C00I H00N 109.5 . . ?
H00L C00I H00M 109.5 . . ?
H00L C00I H00N 109.5 . . ?
H00M C00I H00N 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 S1 2.3761(6) . ?
Zn1 Cl1 2.2700(6) . ?
Zn1 O1 2.0558(15) . ?
Zn1 N2 2.1371(17) . ?
Zn1 N1 2.1762(17) . ?
S1 C00B 1.721(2) . ?
O1 H1 0.862(9) . ?
O1 C00F 1.419(3) . ?
N2 N3 1.362(2) . ?
N2 C00A 1.280(3) . ?
N3 C00B 1.351(3) . ?
N1 C009 1.349(3) . ?
N1 C00E 1.332(3) . ?
N4 C00B 1.343(3) . ?
N4 C00H 1.454(3) . ?
N4 C00I 1.453(3) . ?
C009 C00A 1.463(3) . ?
C009 C00C 1.380(3) . ?
C00A H00A 0.9300 . ?
C00C H00C 0.9300 . ?
C00C C00D 1.390(3) . ?
C00D H00D 0.9300 . ?
C00D C00G 1.369(4) . ?
C00E H00E 0.9300 . ?
C00E C00G 1.382(3) . ?
C00F H00B 0.9600 . ?
C00F H00F 0.9600 . ?
C00F H00G 0.9600 . ?
C00G H00H 0.9300 . ?
C00H H00I 0.9600 . ?
C00H H00J 0.9600 . ?
C00H H00K 0.9600 . ?
C00I H00L 0.9600 . ?
C00I H00M 0.9600 . ?
C00I H00N 0.9600 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Zn1 S1 C00B N3 0.05(19) . . . . ?
Zn1 S1 C00B N4 -179.01(15) . . . . ?
Zn1 N2 N3 C00B 6.0(2) . . . . ?
Zn1 N2 C00A C009 -3.0(3) . . . . ?
Zn1 N1 C009 C00A 8.2(2) . . . . ?
Zn1 N1 C009 C00C -172.98(18) . . . . ?
Zn1 N1 C00E C00G 170.64(17) . . . . ?
S1 Zn1 O1 C00F -55.81(17) . . . . ?
S1 Zn1 N2 N3 -4.86(14) . . . . ?
S1 Zn1 N2 C00A 178.17(16) . . . . ?
S1 Zn1 N1 C009 -23.7(2) . . . . ?
S1 Zn1 N1 C00E 164.42(14) . . . . ?
Cl1 Zn1 S1 C00B 152.84(8) . . . . ?
Cl1 Zn1 O1 C00F 50.51(17) . . . . ?
Cl1 Zn1 N2 N3 -100.03(16) . . . . ?
Cl1 Zn1 N2 C00A 83.00(18) . . . . ?
Cl1 Zn1 N1 C009 -159.14(14) . . . . ?
Cl1 Zn1 N1 C00E 29.01(19) . . . . ?
O1 Zn1 S1 C00B -98.19(8) . . . . ?
O1 Zn1 N2 N3 96.15(14) . . . . ?
O1 Zn1 N2 C00A -80.82(16) . . . . ?
O1 Zn1 N1 C009 95.46(15) . . . . ?
O1 Zn1 N1 C00E -76.39(18) . . . . ?
N2 Zn1 S1 C00B 2.07(8) . . . . ?
N2 Zn1 O1 C00F -137.46(17) . . . . ?
N2 Zn1 N1 C009 -7.30(14) . . . . ?
N2 Zn1 N1 C00E -179.15(19) . . . . ?
N2 N3 C00B S1 -3.6(3) . . . . ?
N2 N3 C00B N4 175.52(16) . . . . ?
N3 N2 C00A C009 179.91(16) . . . . ?
N1 Zn1 S1 C00B 18.25(14) . . . . ?
N1 Zn1 O1 C00F 147.59(17) . . . . ?
N1 Zn1 N2 N3 -177.52(16) . . . . ?
N1 Zn1 N2 C00A 5.51(16) . . . . ?
N1 C009 C00A N2 -3.7(3) . . . . ?
N1 C009 C00C C00D 1.7(4) . . . . ?
N1 C00E C00G C00D 0.7(4) . . . . ?
C009 N1 C00E C00G -0.9(3) . . . . ?
C009 C00C C00D C00G -1.8(4) . . . . ?
C00A N2 N3 C00B -177.06(18) . . . . ?
C00A C009 C00C C00D -179.6(2) . . . . ?
C00C C009 C00A N2 177.5(2) . . . . ?
C00C C00D C00G C00E 0.7(4) . . . . ?
C00E N1 C009 C00A -179.11(19) . . . . ?
C00E N1 C009 C00C -0.3(3) . . . . ?
C00H N4 C00B S1 -2.7(3) . . . . ?
C00H N4 C00B N3 178.16(19) . . . . ?
C00I N4 C00B S1 177.50(17) . . . . ?
C00I N4 C00B N3 -1.7(3) . . . . ?
