Synthesis of Dibenzofurans via Palladium-Catalyzed Phenol-Directed C-H Activation/C-O Cyclization
Bin Xiao; Tian-Jun Gong; Zhao-Jing Liu; Jing-Hui Liu; Dong-Fen Luo; Jun Xu; Lei Liu; Journal of the American Chemical Society 133 (2011) 9250–9253; doi:10.1021/ja203335u

data_4106307
_publ_section_title
;
 Synthesis of Dibenzofurans via Palladium-Catalyzed Phenol-Directed C-H
 Activation/C-O Cyclization
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9250
_journal_page_last               9253
_journal_paper_doi               10.1021/ja203335u
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C45 H55 Cl3 N2 O3 Pd'
_chemical_formula_weight         884.66
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 93.0240(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.05900(10)
_cell_length_b                   18.4839(2)
_cell_length_c                   23.6246(2)
_cell_measurement_temperature    293(2)
_cell_volume                     4386.39(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_sigmaI/netI    0.0281
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            29454
_diffrn_reflns_theta_full        72.37
_diffrn_reflns_theta_max         72.37
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    5.404
_exptl_absorpt_correction_T_max  0.2940
_exptl_absorpt_correction_T_min  0.2211
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.627
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     502
_refine_ls_number_reflns         8568
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0318
_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^)+(0.0605P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0893
_refine_ls_wR_factor_ref         0.0915
_reflns_number_gt                7087
_reflns_number_total             8568
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja203335u_si_001.cif
_cod_data_source_block           100418
_cod_original_cell_volume        4386.40(7)
_cod_database_code               4106307