Palladium catalysed cross-dehydrogenative-coupling of 1,3,5-trialkoxybenzenes with simple arenes
Thomas E. Storr; Faridah Namata; Michael F. Greaney; Chem.Commun. 50 (2014) 13275–; doi:10.1039/C4cc06271J

data_7115855
_publ_section_title
;
 Palladium catalysed cross-dehydrogenative-coupling of
 1,3,5-trialkoxybenzenes with simple arenes
;
_journal_name_full               Chem.Commun.
_journal_page_first              13275
_journal_paper_doi               10.1039/C4cc06271J
_journal_volume                  50
_journal_year                    2014
_chemical_formula_sum            'C17 H20 O3'
_chemical_formula_weight         272.33
_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                74.6760(10)
_cell_angle_beta                 77.4230(10)
_cell_angle_gamma                79.3020(10)
_cell_formula_units_Z            2
_cell_length_a                   8.1003(2)
_cell_length_b                   9.2891(2)
_cell_length_c                   10.3849(2)
_cell_measurement_reflns_used    2546
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      70.12
_cell_measurement_theta_min      4.49
_cell_volume                     728.70(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_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      150(2)
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5413
_diffrn_reflns_theta_full        66.60
_diffrn_reflns_theta_max         70.11
_diffrn_reflns_theta_min         4.49
_exptl_absorpt_coefficient_mu    0.673
_exptl_absorpt_correction_T_max  0.9057
_exptl_absorpt_correction_T_min  0.781862
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             292
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.244
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         2620
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0440
_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^)+(0.1257P)^2^+0.0727P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1362
_refine_ls_wR_factor_ref         0.1788
_reflns_number_gt                2228
_reflns_number_total             2620
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc06271j2.cif
_cod_data_source_block           s3834ma
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7115855