Oxidant/complexing properties of the methimazole (MeImHS)/iodine system towards palladium and gold metals. Crystal structure of the complex cation [PdII(MeImHS)4]2+ balanced by a tetraiodide/iodide mixture
Isaia, Francesco; Aragoni, Maria Carla; Arca, Massimiliano; Caltagirone, Claudia; Castellano, Carlo; Demartin, Francesco; Garau, Alessandra; Lippolis, Vito; Pivetta, Tiziana; New Journal of Chemistry 44 (2020) 2652–2660; doi:10.1039/C9NJ05872A

data_7059230
_publ_section_title
;
 Oxidant/complexing properties of the methimazole (MeImHS)/iodine system
 towards palladium and gold metals. Crystal structure of the complex
 cation [PdII(MeImHS)4]2+ balanced by a tetraiodide/iodide mixture
;
_journal_issue                   6
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2652
_journal_page_last               2660
_journal_paper_doi               10.1039/C9NJ05872A
_journal_volume                  44
_journal_year                    2020
_chemical_formula_sum            'C16 H24 I3.46 N8 Pd S4'
_chemical_formula_weight         1002.14
_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
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-11-07 deposited with the CCDC.	2020-01-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.62(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.7210(17)
_cell_length_b                   12.844(3)
_cell_length_c                   14.190(3)
_cell_measurement_reflns_used    5757
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      24.90
_cell_measurement_theta_min      2.56
_cell_volume                     1567.1(6)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'APEX II CCD diffractometer'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_unetI/netI     0.0216
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10812
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.274
_diffrn_reflns_theta_min         2.152
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    4.287
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.124
_exptl_crystal_description       prism
_exptl_crystal_F_000             939
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   1.000
_exptl_transmission_factor_min   0.842
_refine_diff_density_max         1.666
_refine_diff_density_min         -1.091
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         2824
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0478
_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/[\s^2^(Fo^2^)+(0.0704P)^2^+11.1450P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1393
_refine_ls_wR_factor_ref         0.1476
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2273
_reflns_number_total             2824
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj05872a2.cif
_cod_data_source_block           '[Pd(MeImHS)4]I4'
_cod_depositor_comments
;Adding full bibliography for 7059230.cif.

 Adding full bibliography for 7059230.cif.
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7059230
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              26088