Palladium(III)-Catalyzed Fluorination of Arylboronic Acid Derivatives
Anthony R. Mazzotti; Michael G. Campbell; Pingping Tang; Jennifer M. Murphy; Tobias Ritter; Journal of the American Chemical Society 135 (2013) 14012–14015; doi:10.1021/ja405919z

data_4120826
_publ_section_title
;
 Palladium(III)-Catalyzed Fluorination of Arylboronic Acid Derivatives
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14012
_journal_page_last               14015
_journal_paper_doi               10.1021/ja405919z
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C17 H14 B2 F8 N4 Pd'
_chemical_formula_weight         554.34
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 113.793(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.490(4)
_cell_length_b                   11.504(3)
_cell_length_c                   13.834(4)
_cell_measurement_reflns_used    4554
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      25.04
_cell_measurement_theta_min      2.39
_cell_volume                     1964.4(10)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_data_collection       'APEX2 v2009.3.0 (Bruker-AXS, 2009)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0394
_diffrn_reflns_av_sigmaI/netI    0.0337
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15857
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    1.032
_exptl_absorpt_correction_T_max  0.8202
_exptl_absorpt_correction_T_min  0.7471
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.874
_exptl_crystal_description       block
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.263
_refine_diff_density_min         -1.028
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         3717
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0501
_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^)+(0.0660P)^2^+8.5203P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1312
_refine_ls_wR_factor_ref         0.1398
_reflns_number_gt                3105
_reflns_number_total             3717
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja405919z_si_002.cif
_cod_data_source_block           mgc
_cod_database_code               4120826