Unprecedented palladium(ii) complex containing dipodal 1,3,4-thiadiazole derivatives: synthesis, structure, and biological and thermal investigations
Heidari, Leila; Ghassemzadeh, Mitra; Fenske, Dieter; Fuhr, Olaf; Saeidifar, Maryam; Mohsenzadeh, Farshid; New Journal of Chemistry 44 (2020) 16769–16775; doi:10.1039/D0NJ02918A

data_7060013
_publ_section_title
;
 Unprecedented palladium(ii) complex containing dipodal 1,3,4-thiadiazole
 derivatives: synthesis, structure, and biological and thermal
 investigations
;
_journal_issue                   39
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              16769
_journal_page_last               16775
_journal_paper_doi               10.1039/D0NJ02918A
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C12 H12 Cl2 N6 Pd S4, C3 H7 N O'
_chemical_formula_sum            'C15 H19 Cl2 N7 O Pd S4'
_chemical_formula_weight         618.91
_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   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2019-01-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-05-28 deposited with the CCDC.	2020-09-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.0630(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.13860(10)
_cell_length_b                   23.0128(4)
_cell_length_c                   12.3047(2)
_cell_measurement_reflns_used    30375
_cell_measurement_temperature    180.15
_cell_measurement_theta_max      64.58
_cell_measurement_theta_min      3.14
_cell_volume                     2291.68(6)
_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      180.15
_diffrn_detector                 'Eiger R 4M'
_diffrn_detector_area_resol_mean 13.33
_diffrn_detector_type            DECTRIS
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '1.2 0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34143
_diffrn_reflns_av_R_equivalents  0.0173
_diffrn_reflns_av_unetI/netI     0.0119
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            23896
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        53.597
_diffrn_reflns_theta_max         62.498
_diffrn_reflns_theta_min         3.342
_diffrn_source                   'Metaljet D2'
_diffrn_source_current           2.860
_diffrn_source_power             0.200
_diffrn_source_target            Ga
_diffrn_source_type              'Metaljet D2'
_diffrn_source_voltage           70
_exptl_absorpt_coefficient_mu    8.184
_exptl_absorpt_correction_T_max  0.0690
_exptl_absorpt_correction_T_min  0.0229
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.794
_exptl_crystal_description       needle
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.799
_refine_diff_density_min         -1.028
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         5473
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0279
_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^)+(0.0476P)^2^+1.8570P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0756
_refine_ls_wR_factor_ref         0.0770
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5062
_reflns_number_total             5473
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj02918a2.cif
_cod_data_source_block           pd76
_cod_depositor_comments          'Adding full bibliography for 7060013.cif.'
_cod_database_code               7060013
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.735
_shelx_estimated_absorpt_t_min   0.244
_olex2_refinement_description
;
;
_shelx_res_checksum              21581
_olex2_submission_special_instructions 'No special instructions were received'