Unexpected Intermediates and Products in the C-F Bond Activation of Tetrafluorobenzenes with a Bis(triethylphosphine)Nickel Synthon: Direct Evidence of a Rapid and Reversible C-H Bond Activation by Ni(0)
Samuel A. Johnson; Carla W. Huff; Ferheen Mustafa; Mark Saliba; Journal of the American Chemical Society 130 (2008) 17278–17280; doi:10.1021/ja8081395

data_4108908
_publ_section_title
;
 Unexpected Intermediates and Products in the C-F Bond Activation of
 Tetrafluorobenzenes with a Bis(triethylphosphine)Nickel Synthon: Direct
 Evidence of a Rapid and Reversible C-H Bond Activation by Ni(0)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17278
_journal_page_last               17280
_journal_paper_doi               10.1021/ja8081395
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C26 H40 Ni P2'
_chemical_formula_sum            'C26 H40 Ni P2'
_chemical_formula_weight         473.23
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2007-01-18T17:21:11-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 94.9400(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2828(15)
_cell_length_b                   13.3695(14)
_cell_length_c                   13.3018(14)
_cell_measurement_reflns_used    9099
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.14
_cell_measurement_theta_min      2.16
_cell_volume                     2530.6(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            27568
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    0.903
_exptl_absorpt_correction_T_max  0.826
_exptl_absorpt_correction_T_min  0.7196
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, BRUKER 2001'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_description       block
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.313
_refine_diff_density_min         -0.224
_refine_diff_density_rms         0.05
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.05
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         5772
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.05
_refine_ls_R_factor_all          0.0319
_refine_ls_R_factor_gt           0.0278
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+0.6545P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.071
_refine_ls_wR_factor_ref         0.0736
_reflns_number_gt                5177
_reflns_number_total             5772
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8081395_si_002_1.cif
_cod_data_source_block           fm1m
_cod_database_code               4108908