N,N'-Dimethylpiperazinium-2,3-dithione Triiodide, [Me2Pipdt]I3, as a Powerful New Oxidation Agent toward Metallic Platinum. Synthesis and X-ray Structures of the Reagent and the Product [Pt(Me2Pipdt)2](I3)2
Francesco Bigoli; Paola Deplano; Maria Laura Mercuri; Maria Angela Pellinghelli; Gloria Pintus; Angela Serpe; Emanuele F. Trogu; Journal of the American Chemical Society 123 (2001) 1788–1789; doi:10.1021/ja0056015

data_4115448
_publ_contact_author
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     Prof. Paola Deplano       
     Dipartimento di Chimica Inorganica ed Analitica
     Cittadella Universitaria di Monserrato
     Universit\`a degli Studi di Cagliari
     090042 Monserrato, Cagliari
     Italy
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_publ_contact_author_email       deplano@vaxca1.unica.it
_publ_contact_author_fax         '[int.code]039(0)70 6754499'
_publ_contact_author_phone       '[int.code]039(0)70 6754680'
_publ_section_title
;
 N,N'-Dimethylpiperazinium-2,3-dithione Triiodide, [Me2Pipdt]I3, as a
 Powerful New Oxidation Agent toward Metallic Platinum. Synthesis and
 X-ray Structures of the Reagent and the Product [Pt(Me2Pipdt)2](I3)2
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1788
_journal_page_last               1789
_journal_paper_doi               10.1021/ja0056015
_journal_volume                  123
_journal_year                    2001
_chemical_formula_sum            'C12 H20 I6 N4 Pt S4'
_chemical_formula_weight         1305.04
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.99(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.072(6)
_cell_length_b                   13.303(5)
_cell_length_c                   12.611(5)
_cell_measurement_reflns_used    32
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      9
_cell_volume                     1447.5(13)
_computing_cell_refinement       'local programs'
_computing_data_collection       'Siemens AED local upgrade'
_computing_data_reduction        'local programs'
_computing_molecular_graphics    ORTEP
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type  'Siemens AED diffractometer'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0618
_diffrn_reflns_av_sigmaI/netI    0.1519
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3281
_diffrn_reflns_theta_full        27.04
_diffrn_reflns_theta_max         27.04
_diffrn_reflns_theta_min         3.06
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 100
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    11.542
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6526
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.994
_exptl_crystal_description       prism
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.230
_refine_diff_density_min         -1.194
_refine_diff_density_rms         0.230
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.676
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         3150
_refine_ls_number_restraints     00
_refine_ls_restrained_S_all      0.676
_refine_ls_R_factor_all          0.1365
_refine_ls_R_factor_gt           0.0506
_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^)+(0.0851P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1248
_refine_ls_wR_factor_ref         0.1393
_reflns_number_gt                1001
_reflns_number_total             3150
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0056015_2.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0851P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0851P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_cell_volume        1447.5(12)
_cod_database_code               4115448