Decarbonylative Coupling of Fluorobenzoyl Chlorides with Hexamethyldisilane in the Presence of a Palladium Complex Catalyst: Extremely Facile Decarbonylation of Pentafluorobenzoyl‒Pd Complex Relevant to C6F5SiMe3 Formation
Kashiwabara, Taigo; Tanaka, Masato; Organometallics 25 (2006) 4648–4652; doi:10.1021/om060479p

data_4074225
_publ_section_title
;
 Decarbonylative Coupling of Fluorobenzoyl Chlorides with
 Hexamethyldisilane in the Presence of a Palladium Complex
 Catalyst: Extremely Facile Decarbonylation of
 Pentafluorobenzoyl--Pd Complex Relevant to C6F5SiMe3 Formation
;
_journal_coden_ASTM              ORGND7
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              4648
_journal_page_last               4652
_journal_paper_doi               10.1021/om060479p
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C42 H30 Cl F5 P2 Pd'
_chemical_formula_sum            'C42 H30 Cl F5 P2 Pd'
_chemical_formula_weight         802.52
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.019(2)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
_cell_length_a                   23.287(4)
_cell_length_b                   11.9507(17)
_cell_length_c                   25.667(4)
_cell_measurement_reflns_used    16207
_cell_measurement_temperature    113.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     7143.0(19)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.7.0'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR97
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 1.336
_diffrn_measured_fraction_theta_max 1.336
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.035
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            51316
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    0.695
_exptl_absorpt_correction_T_max  0.933
_exptl_absorpt_correction_T_min  0.857
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3240.00
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         4.89
_refine_diff_density_min         -2.28
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     979
_refine_ls_number_reflns         51316
_refine_ls_R_factor_gt           0.0597
_refine_ls_shift/su_max          0.0070
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
'w = 1/[0.0010Fo^2^ + 2.0000\s(Fo^2^) + 0.5000]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0773
_reflns_number_gt                41680
_reflns_number_total             51316
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om060479psi20060531_063108.cif
_cod_data_source_block           '__ksw511'
_cod_original_cell_volume        7143.1(18)
_cod_original_formula_sum        'C84 H60 Cl2 F10 P2 Pd2 '
_cod_database_code               4074225