Synthesis, characterisation, crystal structures and biological studies of palladium(ii) complexes containing 5-(2-hydroxy-3-methoxy-phenyl)-2,4-dihydro[1,2,4]triazole-3-thione derivatives
Shanmugapriya, A.; Dallemer, F.; Prabhakaran, R.; New Journal of Chemistry 42 (2018) 18850–; doi:10.1039/C8NJ03714K

data_7057823
_publ_section_title
;
 Synthesis, characterisation, crystal structures and biological studies of
 palladium(ii) complexes containing
 5-(2-hydroxy-3-methoxy-phenyl)-2,4-dihydro[1,2,4]triazole-3-thione
 derivatives
;
_journal_issue                   23
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              18850
_journal_paper_doi               10.1039/C8NJ03714K
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         'C20 H23 N6 O4 Pd S2, Cl'
_chemical_formula_sum            'C20 H23 Cl N6 O4 Pd S2'
_chemical_formula_weight         617.41
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-08-31
_audit_creation_method
;
Olex2 1.2
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221)
;
_audit_update_record
;
2018-07-25 deposited with the CCDC.
2018-10-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.137(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.0019(3)
_cell_length_b                   10.3208(3)
_cell_length_c                   25.8409(9)
_cell_measurement_reflns_used    10154
_cell_measurement_temperature    293
_cell_measurement_theta_max      23.7360
_cell_measurement_theta_min      3.7560
_cell_volume                     2394.54(14)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3048
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.922
_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    -55.00  73.00   1.00   20.00    --   -8.68  19.00-180.00  128
  2  \w    -20.00  51.00   1.00   20.00    --    9.31 -99.00  30.00   71
  3  \w    -67.00  36.00   1.00   20.00    --    9.31 -38.00  60.00  103
  4  \w    -24.00  88.00   1.00   20.00    --    9.31  77.00-180.00  112
  5  \w    -20.00  33.00   1.00   20.00    --   -8.68 -99.00-120.00   53
  6  \w    -20.00  33.00   1.00   20.00    --   -8.68 -99.00  30.00   53
  7  \w    -20.00  33.00   1.00   20.00    --   -8.68 -99.00 -30.00   53
  8  \w     -4.00  62.00   1.00   20.00    --    9.31-118.00-163.00   66
  9  \w    -20.00  51.00   1.00   20.00    --    9.31 -99.00 -60.00   71
 10  \w    -67.00  36.00   1.00   20.00    --    9.31 -38.00-150.00  103
 11  \w    -38.00  59.00   1.00   20.00    --   -8.68  57.00  60.00   97
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0316636000
_diffrn_orient_matrix_UB_12      0.0515110000
_diffrn_orient_matrix_UB_13      0.0136680000
_diffrn_orient_matrix_UB_21      0.0149641000
_diffrn_orient_matrix_UB_22      -0.0340123000
_diffrn_orient_matrix_UB_23      0.0236533000
_diffrn_orient_matrix_UB_31      0.0708055000
_diffrn_orient_matrix_UB_32      0.0302285000
_diffrn_orient_matrix_UB_33      0.0033352000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0724
_diffrn_reflns_av_unetI/netI     0.0500
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.922
_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       31
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            52248
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.397
_diffrn_reflns_theta_min         3.473
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.102
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84551
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_description       prism
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.460
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         5543
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0403
_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^)+(0.0193P)^2^+2.1002P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0647
_refine_ls_wR_factor_ref         0.0729
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4049
_reflns_number_total             5543
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj03714k2.cif
_cod_data_source_block           apl18dp
_cod_depositor_comments
'Adding full bibliography for 7057823--7057824.cif.'
_cod_original_cell_volume        2394.52(14)
_cod_database_code               7057823
_shelxl_version_number           2014/6
_reflns_odcompleteness_completeness 99.56
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.66
_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
2.a Aromatic/amide H refined with riding coordinates:
 N2(H2), N3(H3), N5(H5), C1(H1), C5(H5A), C6(H6), C7(H7), C16(H16), C17(H17),
 C18(H18)
2.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C)
2.c Idealised tetrahedral OH refined as rotating group:
 O4(H4)
;
_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 1.264
_oxdiff_exptl_absorpt_empirical_full_min 0.868