Aryl-CF3 Bond-Forming Reductive Elimination from Palladium(IV)
Nicholas D. Ball; Jeff W. Kampf; Melanie S. Sanford; Journal of the American Chemical Society 132 (2010) 2878–2879; doi:10.1021/ja100955x

data_4101984
_publ_section_title
;
 Aryl-CF3 Bond-Forming Reductive Elimination from Palladium(IV)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2878
_journal_page_last               2879
_journal_paper_doi               10.1021/ja100955x
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C26 H28 F8 N2 O3 Pd S, C2 H4 Cl2'
_chemical_formula_sum            'C28 H32 Cl2 F8 N2 O3 Pd S'
_chemical_formula_weight         805.92
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 96.779(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.401(3)
_cell_length_b                   12.8736(18)
_cell_length_c                   24.692(3)
_cell_measurement_reflns_used    9992
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      25.40
_cell_measurement_theta_min      2.42
_cell_volume                     6439.6(15)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART-APEX'
_computing_data_reduction        'Bruker SAINT'
_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      85(2)
_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  0.1127
_diffrn_reflns_av_sigmaI/netI    0.0606
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            65770
_diffrn_reflns_theta_full        26.45
_diffrn_reflns_theta_max         26.45
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    0.887
_exptl_absorpt_correction_T_max  0.9570
_exptl_absorpt_correction_T_min  0.8220
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  Blessing, R. Acta Cryst. (1995) A51 33-38.
  Sheldrick, G.  SADABS (Version 2008/1) Bruker AXS area
  detector absorption and other corrections, University of
  Gottingen, Germany 2008.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3248
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.372
_refine_diff_density_min         -1.532
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.159
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         6624
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.159
_refine_ls_R_factor_all          0.0921
_refine_ls_R_factor_gt           0.0674
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0235P)^2^+3.5536P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1202
_refine_ls_wR_factor_ref         0.1274
_reflns_number_gt                5159
_reflns_number_total             6624
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja100955x_si_001.cif
_cod_data_source_block           nb51
_cod_original_cell_volume        6439.7(15)
_cod_database_code               4101984