Mechanism of the Catalytic Hydrodefluorination of Pentafluoropyridine by Group Six Triangular Cluster Hydrides Containing Phosphines: A Combined Experimental and Theoretical Study
Beltrán, Tomás F.; Feliz, Marta; Llusar, Rosa; Mata, Jose A.; Safont, Vicent S.; Organometallics 30 (2011) 290–297; doi:10.1021/om1009878

data_4063388
_publ_contact_author_address
;Universitat Jaume I
Avda. Sos Baynat s/n
12071 Castell\'on
Spain
;
_publ_contact_author_email       rosa.llusar@qfa.uji.es
_publ_contact_author_name        'Rosa Llusar'
_publ_contact_author_phone       964728086
_publ_section_title
;
 Mechanism of the Catalytic Hydrodefluorination of Pentafluoropyridine by
 Group Six Triangular Cluster Hydrides Containing Phosphines: A Combined
 Experimental and Theoretical Study
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              290
_journal_page_last               297
_journal_paper_doi               10.1021/om1009878
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C18 H48 F3 P6 S4 W3, C24 H20 B'
_chemical_formula_sum            'C42 H68 B F3 P6 S4 W3'
_chemical_formula_weight         1506.38
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                82.866(8)
_cell_angle_beta                 81.808(7)
_cell_angle_gamma                88.481(7)
_cell_formula_units_Z            2
_cell_length_a                   11.137(4)
_cell_length_b                   14.984(5)
_cell_length_c                   16.850(6)
_cell_measurement_temperature    293(2)
_cell_volume                     2761.5(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.804
_diffrn_measured_fraction_theta_max 0.804
_diffrn_measurement_device_type  CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0550
_diffrn_reflns_av_sigmaI/netI    0.1439
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -14
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_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.23
_exptl_absorpt_coefficient_mu    6.596
_exptl_absorpt_correction_T_max  0.5584
_exptl_absorpt_correction_T_min  0.3521
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.812
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.718
_refine_diff_density_min         -1.635
_refine_diff_density_rms         0.233
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     522
_refine_ls_number_reflns         10199
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1341
_refine_ls_R_factor_gt           0.0594
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0038P)^2^+21.0750P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0817
_refine_ls_wR_factor_ref         0.1009
_reflns_number_gt                5865
_reflns_number_total             10199
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om1009878_si_001.cif
_cod_data_source_block           str1070m
_cod_original_cell_volume        2761.5(16)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4063388