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_4120827
_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            'C30 H22 B3 F12 N6 Pd'
_chemical_formula_weight         833.37
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 99.8300(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.0771(6)
_cell_length_b                   17.6720(7)
_cell_length_c                   15.6002(6)
_cell_measurement_reflns_used    30928
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      25.706
_cell_measurement_theta_min      2.305
_cell_volume                     4095.5(3)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0250
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7791
_diffrn_reflns_theta_full        25.72
_diffrn_reflns_theta_max         25.72
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    0.535
_exptl_absorpt_correction_T_max  0.8621
_exptl_absorpt_correction_T_min  0.5871
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_description       needle
_exptl_crystal_F_000             1652
_exptl_crystal_size_max          1.0
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.29
_refine_diff_density_max         3.061
_refine_diff_density_min         -2.050
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     513
_refine_ls_number_reflns         7791
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0867
_refine_ls_R_factor_gt           0.0767
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0960P)^2^+29.5516P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2027
_refine_ls_wR_factor_ref         0.2090
_reflns_number_gt                6585
_reflns_number_total             7791
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja405919z_si_003.cif
_cod_data_source_block           mgc4
_cod_database_code               4120827