#------------------------------------------------------------------------------
#$Date: 2023-03-30 02:17:18 +0300 (Thu, 30 Mar 2023) $
#$Revision: 282130 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/27/7712702.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_7712702
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         'C7 H8 Cl2 N4 S Zn'
_chemical_formula_sum            'C7 H8 Cl2 N4 S Zn'
_chemical_formula_weight         316.50
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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                90.00
_cell_angle_beta                 93.392(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.4725(2)
_cell_length_b                   13.9731(5)
_cell_length_c                   10.8484(4)
_cell_measurement_reflns_used    2733
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      28.2580
_cell_measurement_theta_min      3.9850
_cell_volume                     1130.74(7)
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -55.00  62.00   1.00    2.33    --   17.93 -19.00 150.00  117
  2  ω    -20.00  60.00   1.00    2.33    --   17.93 -99.00 120.00   80
  3  ω    -12.00  88.00   1.00    2.33    --   17.93  77.00  30.00  100
  4  ω    -68.00 -34.00   1.00    2.33    --  -19.72 178.00 -30.00   34
;
_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      -0.0936137000
_diffrn_orient_matrix_UB_12      -0.0056946000
_diffrn_orient_matrix_UB_13      0.0050318000
_diffrn_orient_matrix_UB_21      0.0125883000
_diffrn_orient_matrix_UB_22      -0.0497345000
_diffrn_orient_matrix_UB_23      0.0102779000
_diffrn_orient_matrix_UB_31      0.0110376000
_diffrn_orient_matrix_UB_32      0.0083734000
_diffrn_orient_matrix_UB_33      0.0644924000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6245
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         3.41
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.799
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48178
_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    1.859
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             632
_exptl_crystal_preparation       'heated 343k'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.230
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         1986
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0249
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0389P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0650
_refine_ls_wR_factor_ref         0.0680
_reflns_number_gt                1747
_reflns_number_total             1986
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d3dt00148b2.cif
_cod_data_source_block           pjh-zn-n
_cod_database_code               7712702
_reflns_odcompleteness_completeness 99.71
_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, All N(H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N3(H3), C5(H5), C10(H10), C11(H11), C12(H12), C22(H22)
2.b X=CH2 refined with riding coordinates:
 N4(H4A,H4B)
;
_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 1.652
_oxdiff_exptl_absorpt_empirical_full_min 0.580
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x-1/2, -y-1/2, z-1/2'
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 0.04300(3) 0.33713(2) 0.76433(2) 0.03288(12) Uani 1 1 d . . .
S2 S 0.08957(9) 0.16417(5) 0.74210(6) 0.04166(19) Uani 1 1 d . . .
Cl2 Cl -0.06833(8) 0.35848(5) 0.95516(5) 0.04223(18) Uani 1 1 d . . .
Cl1 Cl 0.34299(8) 0.37584(5) 0.78046(6) 0.04864(19) Uani 1 1 d . . .
C1 C -0.1917(3) 0.45916(18) 0.59335(19) 0.0321(5) Uani 1 1 d . . .
N2 N -0.1643(2) 0.29532(15) 0.62216(15) 0.0309(4) Uani 1 1 d . . .
N3 N -0.2028(3) 0.20207(16) 0.59921(17) 0.0371(5) Uani 1 1 d . . .
H3 H -0.2966 0.1860 0.5541 0.045 Uiso 1 1 calc R . .
N4 N -0.1289(3) 0.04524(16) 0.61987(17) 0.0434(5) Uani 1 1 d . . .
H4A H -0.2214 0.0323 0.5718 0.052 Uiso 1 1 calc R . .
H4B H -0.0615 -0.0003 0.6491 0.052 Uiso 1 1 calc R . .
C5 C -0.2503(3) 0.36200(18) 0.5653(2) 0.0356(6) Uani 1 1 d . . .
H5 H -0.3457 0.3493 0.5087 0.043 Uiso 1 1 calc R . .
N1 N -0.0601(2) 0.46716(14) 0.68384(16) 0.0318(4) Uani 1 1 d . . .
C7 C -0.0904(3) 0.13487(18) 0.64881(19) 0.0313(5) Uani 1 1 d . . .
C10 C -0.0664(4) 0.6360(2) 0.6571(2) 0.0463(7) Uani 1 1 d . . .
H10 H -0.0233 0.6958 0.6820 0.056 Uiso 1 1 calc R . .
C11 C -0.0014(3) 0.5539(2) 0.7145(2) 0.0415(6) Uani 1 1 d . . .
H11 H 0.0877 0.5598 0.7776 0.050 Uiso 1 1 calc R . .
C12 C -0.2601(3) 0.5382(2) 0.5308(2) 0.0435(6) Uani 1 1 d . . .
H12 H -0.3488 0.5310 0.4676 0.052 Uiso 1 1 calc R . .
C22 C -0.1966(3) 0.6275(2) 0.5622(2) 0.0477(7) Uani 1 1 d . . .
H22 H -0.2406 0.6815 0.5203 0.057 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'
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
Cl2 Zn1 S2 106.11(3) . . ?
Cl2 Zn1 Cl1 107.70(3) . . ?
Cl1 Zn1 S2 95.49(3) . . ?
N2 Zn1 S2 76.57(6) . . ?
N2 Zn1 Cl2 112.90(5) . . ?
N2 Zn1 Cl1 139.28(5) . . ?
N1 Zn1 S2 147.72(5) . . ?
N1 Zn1 Cl2 96.70(5) . . ?
N1 Zn1 Cl1 99.03(5) . . ?
N1 Zn1 N2 73.60(7) . . ?
C7 S2 Zn1 100.68(9) . . ?
N1 C1 C5 115.2(2) . . ?
N1 C1 C12 121.6(2) . . ?
C12 C1 C5 123.2(2) . . ?
N3 N2 Zn1 121.18(14) . . ?
C5 N2 Zn1 117.44(17) . . ?
C5 N2 N3 121.34(19) . . ?
N2 N3 H3 120.8 . . ?
C7 N3 N2 118.39(19) . . ?
C7 N3 H3 120.8 . . ?
H4A N4 H4B 120.0 . . ?
C7 N4 H4A 120.0 . . ?
C7 N4 H4B 120.0 . . ?
C1 C5 H5 121.8 . . ?
N2 C5 C1 116.5(2) . . ?
N2 C5 H5 121.8 . . ?
C1 N1 Zn1 117.06(15) . . ?
C11 N1 Zn1 124.66(16) . . ?
C11 N1 C1 118.3(2) . . ?
N3 C7 S2 121.73(19) . . ?
N4 C7 S2 121.92(19) . . ?
N4 C7 N3 116.4(2) . . ?
C11 C10 H10 120.7 . . ?
C11 C10 C22 118.7(3) . . ?
C22 C10 H10 120.7 . . ?
N1 C11 C10 123.0(2) . . ?
N1 C11 H11 118.5 . . ?
C10 C11 H11 118.5 . . ?
C1 C12 H12 120.2 . . ?
C22 C12 C1 119.6(2) . . ?
C22 C12 H12 120.2 . . ?
C10 C22 H22 120.6 . . ?
C12 C22 C10 118.8(2) . . ?
C12 C22 H22 120.6 . . ?
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 S2 2.4556(7) . ?
Zn1 Cl2 2.2958(6) . ?
Zn1 Cl1 2.3026(6) . ?
Zn1 N2 2.1993(18) . ?
Zn1 N1 2.1396(19) . ?
S2 C7 1.685(2) . ?
C1 C5 1.453(3) . ?
C1 N1 1.353(3) . ?
C1 C12 1.379(3) . ?
N2 N3 1.354(3) . ?
N2 C5 1.271(3) . ?
N3 H3 0.8600 . ?
N3 C7 1.350(3) . ?
N4 H4A 0.8600 . ?
N4 H4B 0.8600 . ?
N4 C7 1.319(3) . ?
C5 H5 0.9300 . ?
N1 C11 1.325(3) . ?
C10 H10 0.9300 . ?
C10 C11 1.379(4) . ?
C10 C22 1.380(4) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C12 C22 1.371(4) . ?
C22 H22 0.9300 . ?
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 S2 C7 N3 6.01(19) . . . . ?
Zn1 S2 C7 N4 -174.25(17) . . . . ?
Zn1 N2 N3 C7 -11.9(2) . . . . ?
Zn1 N2 C5 C1 5.0(3) . . . . ?
Zn1 N1 C11 C10 177.34(17) . . . . ?
S2 Zn1 N2 N3 11.70(14) . . . . ?
S2 Zn1 N2 C5 -170.50(17) . . . . ?
S2 Zn1 N1 C1 23.6(2) . . . . ?
S2 Zn1 N1 C11 -154.85(14) . . . . ?
Cl2 Zn1 S2 C7 102.40(8) . . . . ?
Cl2 Zn1 N2 N3 -90.36(15) . . . . ?
Cl2 Zn1 N2 C5 87.44(16) . . . . ?
Cl2 Zn1 N1 C1 -111.59(14) . . . . ?
Cl2 Zn1 N1 C11 70.00(17) . . . . ?
Cl1 Zn1 S2 C7 -147.38(8) . . . . ?
Cl1 Zn1 N2 N3 94.42(16) . . . . ?
Cl1 Zn1 N2 C5 -87.78(18) . . . . ?
Cl1 Zn1 N1 C1 139.22(14) . . . . ?
Cl1 Zn1 N1 C11 -39.19(18) . . . . ?
C1 N1 C11 C10 -1.1(3) . . . . ?
C1 C12 C22 C10 -0.6(4) . . . . ?
N2 Zn1 S2 C7 -7.93(9) . . . . ?
N2 Zn1 N1 C1 0.36(14) . . . . ?
N2 Zn1 N1 C11 -178.05(19) . . . . ?
N2 N3 C7 S2 2.5(3) . . . . ?
N2 N3 C7 N4 -177.23(19) . . . . ?
N3 N2 C5 C1 -177.23(19) . . . . ?
C5 C1 N1 Zn1 1.9(2) . . . . ?
C5 C1 N1 C11 -179.56(19) . . . . ?
C5 C1 C12 C22 -179.5(2) . . . . ?
C5 N2 N3 C7 170.4(2) . . . . ?
N1 Zn1 S2 C7 -30.79(13) . . . . ?
N1 Zn1 N2 N3 179.20(16) . . . . ?
N1 Zn1 N2 C5 -3.00(16) . . . . ?
N1 C1 C5 N2 -4.6(3) . . . . ?
N1 C1 C12 C22 -1.4(3) . . . . ?
C11 C10 C22 C12 1.8(4) . . . . ?
C12 C1 C5 N2 173.6(2) . . . . ?
C12 C1 N1 Zn1 -176.26(16) . . . . ?
C12 C1 N1 C11 2.3(3) . . . . ?
C22 C10 C11 N1 -1.0(4) . . . . ?
