Competing C-F Activation Pathways in the Reaction of Pt(0) with Fluoropyridines: Phosphine-Assistance versus Oxidative Addition
Ainara Nova; Stefan Erhardt; Naseralla A. Jasim; Robin N. Perutz; Stuart A. Macgregor; John E. McGrady; Adrian C. Whitwood; Journal of the American Chemical Society 130 (2008) 15499–15511; doi:10.1021/ja8046238

data_4108666
_publ_section_title
;
 Competing C-F Activation Pathways in the Reaction of Pt(0) with
 Fluoropyridines: Phosphine-Assistance versus Oxidative Addition
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15499
_journal_page_last               15511
_journal_paper_doi               10.1021/ja8046238
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C42 H67 F6 N P2 Pt'
_chemical_formula_sum            'C42 H67 F6 N P2 Pt'
_chemical_formula_weight         957.00
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                113.4450(10)
_cell_angle_beta                 105.6340(10)
_cell_angle_gamma                90.0720(10)
_cell_formula_units_Z            4
_cell_length_a                   11.9912(2)
_cell_length_b                   18.4427(2)
_cell_length_c                   22.0438(2)
_cell_measurement_reflns_used    81165
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.910
_cell_volume                     4274.46(10)
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type
'Bruker-Nonius Roper CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_av_sigmaI/netI    0.0454
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            94369
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         2.91
_exptl_absorpt_coefficient_mu    3.413
_exptl_absorpt_correction_T_max  0.843
_exptl_absorpt_correction_T_min  0.754
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/2 (Sheldrick, G.M., 2007)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_description       block
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.127
_refine_diff_density_min         -1.722
_refine_diff_density_rms         0.186
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1029
_refine_ls_number_reflns         19626
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0352
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0219P)^2^+9.0905P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0749
_refine_ls_wR_factor_ref         0.0778
_reflns_number_gt                17968
_reflns_number_total             19626
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8046238_si_003_3.cif
_cod_data_source_block           rnp0801
_cod_database_code               4108666