Mechanism of C-F Reductive Elimination from Palladium(IV) Fluorides
Takeru Furuya; Diego Benitez; Ekaterina Tkatchouk; Alexandra E. Strom; Pingping Tang; William A. Goddard; Tobias Ritter; Journal of the American Chemical Society 132 (2010) 3793–3807; doi:10.1021/ja909371t

data_4102119
_publ_section_title
;
 Mechanism of C-F Reductive Elimination from Palladium(IV) Fluorides
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3793
_journal_page_last               3807
_journal_paper_doi               10.1021/ja909371t
_journal_volume                  132
_journal_year                    2010
_chemical_compound_source        'chemical synthesis'
_chemical_formula_iupac
;
[Pd F2 (C17 H12 N3 O4 S) (C13 H8 N)] . (C2 H3 N)
;
_chemical_formula_moiety         'C30 H20 F2 N4 O4 Pd S, C2 H3 N'
_chemical_formula_structural
;
(Pd F2 (C17 H12 N3 O4 S) (C13 H8 N)) (C2 H3 N)
;
_chemical_formula_sum            'C32 H23 F2 N5 O4 Pd S'
_chemical_formula_weight         718.01
_chemical_name_common            TF04054
_chemical_name_systematic
; 
(Benzo[h]quinolinato){(2-nitrophenyl-sulfonyl)[(2-(pyridine-2-yl)phenyl]
amido}-difluoropalladium(IV) Acetonitrile Solvate
;
_chemical_temperature_decomposition 416
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 99.197(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.0089(3)
_cell_length_b                   13.3937(4)
_cell_length_c                   21.0503(7)
_cell_measurement_reflns_used    1442
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      17.95
_cell_measurement_theta_min      2.42
_cell_volume                     2785.65(15)
_computing_cell_refinement       'SAINT V7.34A (Bruker AXS, 2006b)'
_computing_data_collection       'APEX2 v2.1-0 (Bruker AXS, 2006a)'
_computing_data_reduction
;
SAINT V7.34A (Bruker AXS, 2006b), SADABS (Bruker AXS, 2004)
;
_computing_molecular_graphics    'SHELXTL v6.12 (Bruker AXS, 2001)'
_computing_publication_material  'SHELXTL v6.12 (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXTL v6.12 (Bruker AXS, 2001)'
_computing_structure_solution    'SHELXTL v6.12 (Bruker AXS, 2001)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 836.6
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       '\w scans, 2147 0.5\% rotations'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1469
_diffrn_reflns_av_sigmaI/netI    0.0690
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            34170
_diffrn_reflns_theta_full        22.49
_diffrn_reflns_theta_max         22.49
_diffrn_reflns_theta_min         1.81
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.805
_exptl_absorpt_correction_T_max  0.9802
_exptl_absorpt_correction_T_min  0.9421
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2004)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.712
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.392
_refine_diff_density_min         -0.505
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         3643
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0234P)^2^+3.0772P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0829
_reflns_number_gt                2584
_reflns_number_total             3643
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja909371t_si_002.cif
_cod_data_source_block           compound_3
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4102119