Formation and Characterization of the Hexanuclear Platinum Cluster [Pt~6~(μ-P-t-Bu~2~)~4~(CO)~6~](CF~3~SO~3~)~2~ through Structural, Electrochemical and Computational Analyses
Fabrizia Fabrizi de Biani; Andrea Ienco; Franco Laschi; Piero Leoni; Fabio Marchetti; Lorella Marchetti; Carlo Mealli; Piero Zanello; Journal of the American Chemical Society 127 (2005) 3076–3089; doi:10.1021/ja043626o

data_4111484
_publ_contact_author_address
;
       Dipartimento di Chimica e Chimica Industriale
       Universit\`a di Pisa
       Via Risorgimento,  35
       56126  Pisa
       Italy
;
_publ_contact_author_email       leoni@dcci.unipi.it
_publ_contact_author_fax         '+39 050 2219260'
_publ_contact_author_name        '  Prof. P. Leoni'
_publ_contact_author_phone       '+39 050 2219217'
_publ_section_title
;
 Formation and Characterization of the Hexanuclear Platinum Cluster
 [Pt~6~(\m-P-t-Bu~2~)~4~(CO)~6~](CF~3~SO~3~)~2~ through Structural,
 Electrochemical and Computational Analyses
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3076
_journal_page_last               3089
_journal_paper_doi               10.1021/ja043626o
_journal_volume                  127
_journal_year                    2005
_chemical_formula_moiety         'C27 H54 O3 P3 Pt3, C F3 O3 S'
_chemical_formula_sum            'C28 H54 F3 O6 P3 Pt3 S'
_chemical_formula_weight         1253.95
_chemical_name_systematic
;
tris-(\m-2-Di-t-butylphosphido)-tricarbonyl-triangulo-tri-platinum(i,i,ii)
  trifluoromethanesulfonate
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.912(5)
_cell_length_b                   17.308(4)
_cell_length_c                   9.0440(18)
_cell_measurement_reflns_used    44
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.481
_cell_measurement_theta_min      5.238
_cell_volume                     4056.1(15)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'WINGX-1.64 (Farrugia, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '2\q/\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0908
_diffrn_reflns_av_sigmaI/netI    0.0732
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       1
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4695
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.35
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    10.539
_exptl_absorpt_correction_T_max  0.1851
_exptl_absorpt_correction_T_min  0.07125
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'Deep red (r.l.) violet(t.l.)'
_exptl_crystal_density_diffrn    2.053
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2368
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.885
_refine_diff_density_min         -1.245
_refine_diff_density_rms         0.253
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         3699
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1100
_refine_ls_R_factor_gt           0.0556
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0483P)^2^+46.0506P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1120
_refine_ls_wR_factor_ref         0.1364
_reflns_number_gt                2283
_reflns_number_total             3699
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja043626osi20041104_115038.cif
_cod_data_source_block           plafosco
_cod_original_cell_volume        4056.1(14)
_cod_database_code               4111484