#------------------------------------------------------------------------------
#$Date: 2025-04-05 06:22:48 +0300 (Sat, 05 Apr 2025) $
#$Revision: 298943 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/75/7717535.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_7717535
loop_
_publ_author_name
'Pandey, Shivendra Kumar'
'Kumar, Sandeep'
'Singh, Swati'
'Patel, Anand Kumar'
'Gond, Mannu Kumar'
'Acharya, Arbind'
'Bharty, Manoj Kumar'
_publ_section_title
;
 Synthesis, structural characterisation, and anticancer potential of mono
 and dinuclear Pd(II) complexes of N-(2-pyridyl)thiourea.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1139
_journal_page_last               1149
_journal_paper_doi               10.1039/d4dt02614d
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C8 H11 N3 S'
_chemical_formula_sum            'C8 H11 N3 S'
_chemical_formula_weight         181.25
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-09-12 deposited with the CCDC.	2024-11-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.131(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7076(14)
_cell_length_b                   11.1525(16)
_cell_length_c                   8.4121(14)
_cell_measurement_reflns_used    1016
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      71.3970
_cell_measurement_theta_min      6.1350
_cell_volume                     908.4(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.0938
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0749
_diffrn_reflns_av_unetI/netI     0.0822
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3087
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.005
_diffrn_reflns_theta_min         4.567
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.737
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48780
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_description       Block
_exptl_crystal_F_000             384
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.775
_refine_diff_density_min         -0.567
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     111
_refine_ls_number_reflns         1709
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.1122
_refine_ls_R_factor_gt           0.0957
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2564
_refine_ls_wR_factor_ref         0.3020
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1256
_reflns_number_total             1709
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt02614d2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
;

2025-04-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel

 Adding full bibliography for 7717535--7717537.cif.
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_moiety     'C16 H22 N6 S2'
_cod_original_formula_sum        'C16 H22 N6 S2'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     362.51
_cod_database_code               7717535
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S -0.05783(10) 0.55606(10) 0.26307(14) 0.0594(6) Uani 1 1 d . . . . .
N2 N 0.1959(3) 0.4750(3) 0.3205(4) 0.0501(9) Uani 1 1 d . . . . .
H2 H 0.155079 0.435066 0.390920 0.060 Uiso 1 1 calc R U . . .
N1 N 0.4086(3) 0.5149(3) 0.2190(4) 0.0498(8) Uani 1 1 d . . . . .
N3 N 0.1707(3) 0.6214(3) 0.1283(4) 0.0528(9) Uani 1 1 d . . . . .
H3 H 0.258504 0.615602 0.122395 0.063 Uiso 1 1 calc R U . . .
C4 C 0.3935(3) 0.3549(3) 0.4094(4) 0.0433(9) Uani 1 1 d . . . . .
C6 C 0.3359(4) 0.4494(3) 0.3147(4) 0.0417(9) Uani 1 1 d . . . . .
C7 C 0.1120(4) 0.5535(3) 0.2323(5) 0.0480(10) Uani 1 1 d . . . . .
C3 C 0.5324(4) 0.3340(3) 0.4008(5) 0.0514(10) Uani 1 1 d . . . . .
H3A H 0.575077 0.273549 0.462460 0.062 Uiso 1 1 calc R U . . .
C1 C 0.5432(4) 0.4892(4) 0.2140(5) 0.0539(10) Uani 1 1 d . . . . .
H1 H 0.594318 0.534155 0.146074 0.065 Uiso 1 1 calc R U . . .
C2 C 0.6095(4) 0.4017(4) 0.3019(6) 0.0578(11) Uani 1 1 d . . . . .
H2A H 0.703411 0.387734 0.295763 0.069 Uiso 1 1 calc R U . . .
C5 C 0.3066(4) 0.2790(4) 0.5115(5) 0.0568(11) Uani 1 1 d . . . . .
H5A H 0.267944 0.328599 0.590300 0.085 Uiso 1 1 calc R U . . .
H5B H 0.363158 0.217953 0.563555 0.085 Uiso 1 1 calc R U . . .
H5C H 0.233488 0.242185 0.445901 0.085 Uiso 1 1 calc R U . . .
C8 C 0.0946(5) 0.7059(4) 0.0227(6) 0.0649(12) Uani 1 1 d . . . . .
H8A H 0.155457 0.738926 -0.051006 0.097 Uiso 1 1 calc R U . . .
H8B H 0.058505 0.769278 0.084662 0.097 Uiso 1 1 calc R U . . .
H8C H 0.019807 0.664944 -0.035229 0.097 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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
C7 N2 C6 130.7(4) . . ?
C7 N2 H2 114.6 . . ?
C6 N2 H2 114.6 . . ?
C6 N1 C1 117.6(3) . . ?
C7 N3 C8 123.5(4) . . ?
C7 N3 H3 118.3 . . ?
C8 N3 H3 118.3 . . ?
C3 C4 C6 116.5(3) . . ?
C3 C4 C5 121.8(3) . . ?
C6 C4 C5 121.7(3) . . ?
N1 C6 N2 118.1(3) . . ?
N1 C6 C4 123.1(4) . . ?
N2 C6 C4 118.7(3) . . ?
N3 C7 N2 117.1(4) . . ?
N3 C7 S1 124.5(3) . . ?
N2 C7 S1 118.3(3) . . ?
C4 C3 C2 121.0(3) . . ?
C4 C3 H3A 119.5 . . ?
C2 C3 H3A 119.5 . . ?
N1 C1 C2 124.1(4) . . ?
N1 C1 H1 117.9 . . ?
C2 C1 H1 117.9 . . ?
C1 C2 C3 117.6(4) . . ?
C1 C2 H2A 121.2 . . ?
C3 C2 H2A 121.2 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N3 C8 H8A 109.5 . . ?
N3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 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
S1 C7 1.687(4) . ?
N2 C7 1.377(5) . ?
N2 C6 1.393(5) . ?
N2 H2 0.8600 . ?
N1 C6 1.327(5) . ?
N1 C1 1.341(5) . ?
N3 C7 1.317(6) . ?
N3 C8 1.459(5) . ?
N3 H3 0.8600 . ?
C4 C3 1.375(5) . ?
C4 C6 1.412(5) . ?
C4 C5 1.506(5) . ?
C3 C2 1.382(6) . ?
C3 H3A 0.9300 . ?
C1 C2 1.359(6) . ?
C1 H1 0.9300 . ?
C2 H2A 0.9300 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H3 N1 0.86 1.97 2.660(5) 136.6 . yes
C2 H2A S1 0.93 3.01 3.695(4) 131.7 1_655 yes
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
C1 N1 C6 N2 -179.8(4) . . . . ?
C1 N1 C6 C4 -0.4(5) . . . . ?
C7 N2 C6 N1 5.8(6) . . . . ?
C7 N2 C6 C4 -173.6(4) . . . . ?
C3 C4 C6 N1 1.3(5) . . . . ?
C5 C4 C6 N1 -177.4(4) . . . . ?
C3 C4 C6 N2 -179.3(3) . . . . ?
C5 C4 C6 N2 2.0(5) . . . . ?
C8 N3 C7 N2 177.9(4) . . . . ?
C8 N3 C7 S1 -1.7(6) . . . . ?
C6 N2 C7 N3 -3.4(6) . . . . ?
C6 N2 C7 S1 176.2(3) . . . . ?
C6 C4 C3 C2 -1.1(6) . . . . ?
C5 C4 C3 C2 177.6(4) . . . . ?
C6 N1 C1 C2 -0.8(6) . . . . ?
N1 C1 C2 C3 0.9(7) . . . . ?
C4 C3 C2 C1 0.1(6) . . . . ?
