Unprecedented Tris-Phosphido-Bridged Triangular Clusters with 42 Valence Electrons. Chemical, Electrochemical and Computational Studies of their Formation and Stability
Tiziana Funaioli; Piero Leoni; Lorella Marchetti; Alberto Albinati; Silvia Rizzato; Fabrizia Fabrizi de Biani; Andrea Ienco; Gabriele Manca; Carlo Mealli; Inorganic Chemistry 52 (2013) 4635–4647; doi:10.1021/ic400251y

data_4334520
_publ_contact_author_address
;     
Dipartimento di Chimica e Chimica Industriale
Universita' di Pisa
Via Risorgimento 35. I-56126 Pisa (Italy)
;
_publ_contact_author_email       leoni@dcci.unipi.it
_publ_contact_author_name        'P. Leoni'
_publ_section_title
;
 Unprecedented Tris-Phosphido-Bridged Triangular Clusters with 42 Valence
 Electrons. Chemical, Electrochemical and Computational Studies of their
 Formation and Stability
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4635
_journal_page_last               4647
_journal_paper_doi               10.1021/ic400251y
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C24 H54 Br3 P3 Pt3'
_chemical_formula_weight         1260.53
_chemical_name_common
;
 Pt3(mu-PBut2)3Br3
;
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_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                120.00
_cell_formula_units_Z            2
_cell_length_a                   11.9553(8)
_cell_length_b                   11.9553
_cell_length_c                   14.6560(10)
_cell_measurement_reflns_used    9894
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.839
_cell_measurement_theta_min      2.408
_cell_volume                     1814.12(17)
_computing_cell_refinement       'SAINTPLUS  (Bruker AXS, 1999)'
_computing_data_collection       'SMART      (Bruker AXS, 2001)'
_computing_data_reduction        'SAINTPLUS  (Bruker AXS, 1999)'
_computing_molecular_graphics
;     
 ORTEP for Windows v1.074 (L.J. Farrugia 1997)
 Mercury CSD 3.0.1 (Build RC6), CCDC, Cambridge (2011)
;
_computing_publication_material
'WinGX v1.64.05(L.J. Farrugia, J. Appl. Cryst.,1999,32, 837)'
_computing_structure_refinement  'SHELXL-97 (Acta Cryst.,2008,A64,112)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0277
_diffrn_reflns_av_sigmaI/netI    0.0129
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22824
_diffrn_reflns_theta_full        29.35
_diffrn_reflns_theta_max         29.35
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    14.987
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6150
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Sadabs 2.01 (Bruker AXS, 1999)'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    2.308
_exptl_crystal_description       cubic
_exptl_crystal_F_000             1164
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.416
_refine_diff_density_min         -1.391
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       0.00026(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     56
_refine_ls_number_reflns         1678
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0207
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0144P)^2^+4.4571P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0431
_refine_ls_wR_factor_ref         0.0452
_reflns_number_gt                1485
_reflns_number_total             1678
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400251y_si_001_2.cif
_cod_data_source_block           Pt3Br3
_cod_database_code               4334520