Synthesis and Reactivity of a Mono-σ-Aryl Palladium(IV) Fluoride Complex
Nicholas D. Ball; Melanie S. Sanford; Journal of the American Chemical Society 131 (2009) 3796–3797; doi:10.1021/ja8054595

data_4104046
_publ_section_title
;
 Synthesis and Reactivity of a Mono-\s-Aryl Palladium(IV) Fluoride Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3796
_journal_page_last               3797
_journal_paper_doi               10.1021/ja8054595
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C24 H29 F5 N2 Pd, 2(C3 H6 O)'
_chemical_formula_sum            'C30 H41 F5 N2 O2 Pd'
_chemical_formula_weight         663.05
_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                73.6720(10)
_cell_angle_beta                 77.1800(10)
_cell_angle_gamma                69.5870(10)
_cell_formula_units_Z            2
_cell_length_a                   9.6894(7)
_cell_length_b                   12.7681(9)
_cell_length_c                   13.8914(10)
_cell_measurement_reflns_used    9998
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.26
_cell_volume                     1530.97(19)
_computing_cell_refinement       'Bruker SAINT'
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0261
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            44156
_diffrn_reflns_theta_full        28.36
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    0.665
_exptl_absorpt_correction_T_max  0.9010
_exptl_absorpt_correction_T_min  0.8356
_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            colorless
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             684
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.715
_refine_diff_density_min         -2.979
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     438
_refine_ls_number_reflns         7631
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0448
_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^)+(0.0297P)^2^+3.9241P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1019
_refine_ls_wR_factor_ref         0.1088
_reflns_number_gt                6810
_reflns_number_total             7631
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8054595_si_003.cif
_cod_data_source_block           nb255
_cod_database_code               4104046