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_4104045
_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
; 
2(C24 H28 F2 N2 Pd), 0.5(C6 H6), 0.5(C6 H6), 0.5(C6 H6)
;
_chemical_formula_sum            'C57 H65 F4 N4 Pd2'
_chemical_formula_weight         1094.93
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'I -2ya'
_symmetry_space_group_name_H-M   'I 1 a 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                 95.1350(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.9592(12)
_cell_length_b                   17.5332(12)
_cell_length_c                   20.2950(14)
_cell_measurement_reflns_used    9918
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      24.92
_cell_measurement_theta_min      2.51
_cell_volume                     6364.9(8)
_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  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_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  0.0652
_diffrn_reflns_av_sigmaI/netI    0.0445
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            70232
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    0.610
_exptl_absorpt_correction_T_max  0.9472
_exptl_absorpt_correction_T_min  0.8625
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  Blessing, R. Acta Cryst. (1995) A51 33-38.
  Sheldrick, G.  SADABS (Version 2007/4) Bruker AXS area
  detector absorption and other corrections, University of
  Gottingen, Germany 2007.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.143
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blade
_exptl_crystal_F_000             2252
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.805
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.139
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     682
_refine_ls_number_reflns         11189
_refine_ls_number_restraints     218
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0552
_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^)+(0.1065P)^2^+3.1299P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1553
_refine_ls_wR_factor_ref         0.1651
_reflns_number_gt                9308
_reflns_number_total             11189
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8054595_si_002.cif
_cod_data_source_block           nb96
_cod_database_code               4104045