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_7057824
_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         '2(C30 H26 N6 O4 Pd S2), Cl'
_chemical_formula_sum            'C60 H52 Cl N12 O8 Pd2 S4'
_chemical_formula_weight         1445.62
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-04-13
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2018-07-25 deposited with the CCDC.
2018-10-09 downloaded from the CCDC.
;
_cell_angle_alpha                74.7310(10)
_cell_angle_beta                 87.4550(10)
_cell_angle_gamma                84.5360(10)
_cell_formula_units_Z            2
_cell_length_a                   12.88650(10)
_cell_length_b                   13.4398(2)
_cell_length_c                   19.0250(3)
_cell_measurement_reflns_used    70651
_cell_measurement_temperature    293
_cell_measurement_theta_max      28.4730
_cell_measurement_theta_min      3.7240
_cell_volume                     3163.58(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.18b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.18b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.18b (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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3048
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -24.00  85.00   1.00    7.00    --    8.41  77.00 -60.00  109
  2  \w    -20.00  82.00   1.00    7.00    --    8.41  57.00-180.00  102
  3  \w     -5.00  60.00   1.00    7.00    --    8.41-117.00 -58.07   65
  4  \w    -16.00  83.00   1.00    7.00    --    8.41  38.00 120.00   99
  5  \w    -63.00  40.00   1.00    7.00    --   10.00 -64.00 157.35  103
  6  \w    -65.00  42.00   1.00    7.00    --   10.00 -73.00  19.72  107
  7  \w    -18.00  53.00   1.00    7.00    --   10.00-102.00  79.61   71
  8  \w    -78.00 -35.00   1.00    7.00    --   -7.55 147.00 138.87   43
  9  \w    -20.00  33.00   1.00    7.00    --   -7.55 -99.00 -60.00   53
 10  \w    -81.00 -37.00   1.00    7.00    --   -7.55 151.00 113.76   44
 11  \w    -20.00  49.00   1.00    7.00    --    8.41 -99.00  60.00   69
 12  \w     14.00  80.00   1.00    7.00    --    8.41-149.00  21.83   66
 13  \w    -14.00  55.00   1.00    7.00    --   10.00-106.00 151.47   69
 14  \w    -20.00  33.00   1.00    7.00    --   -7.55 -99.00-180.00   53
 15  \w    -49.00  72.00   1.00    7.00    --   -7.55  19.00 -30.00  121
 16  \w    -16.00  83.00   1.00    7.00    --    8.41  38.00   0.00   99
 17  \w    -80.00  97.00   1.00    7.00    --    8.41   0.00-180.00  177
 18  \w    -80.00  97.00   1.00    7.00    --    8.41   0.00-150.00  177
 19  \w    -16.00  83.00   1.00    7.00    --    8.41  38.00-150.00   99
 20  \w    -80.00  97.00   1.00    7.00    --    8.41   0.00 -90.00  177
 21  \w    -80.00  95.00   1.00    7.00    --    8.41   0.00 -60.00  175
 22  \w    -80.00  97.00   1.00    7.00    --    8.41   0.00-120.00  177
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0300975000
_diffrn_orient_matrix_UB_12      -0.0420830000
_diffrn_orient_matrix_UB_13      0.0228599000
_diffrn_orient_matrix_UB_21      -0.0413433000
_diffrn_orient_matrix_UB_22      -0.0066191000
_diffrn_orient_matrix_UB_23      0.0262463000
_diffrn_orient_matrix_UB_31      -0.0210582000
_diffrn_orient_matrix_UB_32      -0.0346516000
_diffrn_orient_matrix_UB_33      -0.0168145000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_unetI/netI     0.0130
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            172190
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.712
_diffrn_reflns_theta_max         24.712
_diffrn_reflns_theta_min         3.177
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.806
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71271
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.18b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_description       prism
_exptl_crystal_F_000             1466
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.922
_refine_diff_density_min         -0.602
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     778
_refine_ls_number_reflns         10769
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0331
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0412P)^2^+3.1287P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0827
_refine_ls_wR_factor_ref         0.0871
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9659
_reflns_number_total             10769
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj03714k2.cif
_cod_data_source_block           apl16dp
_cod_depositor_comments
'Adding full bibliography for 7057823--7057824.cif.'
_cod_database_code               7057824
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         'c57 h52 n6 o4 p2 s2 Pd1'
_diffrn_oxdiff_ac3_digest_frames
;
01d360f5c38ceca04c26bb0d3076aeed2c000274adb
;
_diffrn_oxdiff_ac3_digest_hkl
;
014f3cce4c805ff07219b9470741e41fa59d54
;
_reflns_odcompleteness_completeness 99.80
_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. Uiso/Uaniso restraints and constraints
C39 \\sim C44 \\sim C43 \\sim C42 \\sim C41 \\sim C40: within 1.7A with sigma
of 0.005 and sigma for terminal atoms of 0.01
3.a Aromatic/amide H refined with riding coordinates:
 N3(H3A), N4(H4), C1(H1), C3(H3B), C4(H4A), C5(H5), C11(H11), C12(H12),
 C13(H13), C14(H14), C15(H15), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23),
  C25(H25), C26(H26), C27(H27), N8(H8), N9(H9), N10(H10), C30(H30), C32(H32),
 C33(H33), C34(H34), C48(H48), C50(H50), C51(H51), C52(H52), C54(H54), C55(H55),
  C56(H56)
3.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C29(H29A,H29B,H29C), C37(H37A,H37B,H37C), C59(H59A,H59B,H59C)
3.c Idealised tetrahedral OH refined as rotating group:
 O3(H3), O7(H7)
;
_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 1.464
_oxdiff_exptl_absorpt_empirical_full_min 0.777