Palladium-Catalyzed Coupling Reactions of Tetrafluoroethylene with Arylzinc Compounds
Masato Ohashi; Tadashi Kambara; Tsubasa Hatanaka; Hiroki Saijo; Ryohei Doi; Sensuke Ogoshi; Journal of the American Chemical Society 133 (2011) 3256–3259; doi:10.1021/ja109911p

data_4105746
_publ_contact_author_address
;
 Department of Applied Chemistry,
 Faculty of Engineering, Suita, Osaka-565-0871, Japan
;
_publ_contact_author_email       ohashi@chem.eng.osaka-u.ac.jp
_publ_contact_author_fax         '+81 6 6879 7394'
_publ_contact_author_name        'Assistant Prof. Masato Ohashi'
_publ_contact_author_phone       '+81 6 6879 7393'
_publ_section_title
;
 Palladium-Catalyzed Coupling Reactions of Tetrafluoroethylene with
 Arylzinc Compounds
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3256
_journal_page_last               3259
_journal_paper_doi               10.1021/ja109911p
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         '2(C38 H30 F4 P2 Pd), C7'
_chemical_formula_sum            'C83 H60 F8 P4 Pd2'
_chemical_formula_weight         1545.99
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 91.3190(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   18.0191(9)
_cell_length_b                   9.5138(5)
_cell_length_c                   20.8353(11)
_cell_measurement_reflns_used    32512
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.06
_cell_measurement_theta_min      3.03
_cell_volume                     3570.9(3)
_computing_cell_refinement       'Rigaku/RAPID Diffractometer Control'
_computing_data_collection       'Rigaku/RAPID Diffractometer Control'
_computing_data_reduction        'teXsan: PROCESS (MSC)'
_computing_molecular_graphics    'Ortep-3 (Louis J. Farrugia, 1999)'
_computing_publication_material  'SHELXL-97 and modified'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1999)'
_computing_structure_solution    'PATTY (Bueskens, et al., 1994)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_detector       'imaging plate'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            31619
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.10
_exptl_absorpt_coefficient_mu    0.659
_exptl_absorpt_correction_T_max  0.80
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Higashi, T. (1999). Abscor - empirical Absorption Correction based on
Fourier Series Approximation. Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_description       block
_exptl_crystal_F_000             1564
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.554
_refine_diff_density_min         -0.645
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         6235
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0360
_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^)+(0.0370P)^2^+3.5412P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0788
_refine_ls_wR_factor_ref         0.0832
_reflns_number_gt                5247
_reflns_number_total             6235
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja109911p_si_001_2.cif
_cod_data_source_block           TFE-Pd
_cod_original_sg_symbol_Hall     '-p 2ybc'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4105746