N-Acylamidine Palladium(II) Complexes. Synthesis, Structures, and Catalytic Activity for Suzuki-Miyaura Cross-Coupling Reactions: Experiments and DFT Calculations
Jan K. Eberhardt; Roland Fröhlich; Ernst-Ulrich Würthwein; Journal of Organic Chemistry 68 (2003) 6690–6694; doi:10.1021/jo034455t

data_4022464
_publ_section_title
;
 N-Acylamidine Palladium(II) Complexes. Synthesis, Structures,
 and Catalytic Activity for Suzuki-Miyaura Cross-Coupling
 Reactions: Experiments and DFT Calculations
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              6690
_journal_page_last               6694
_journal_paper_doi               10.1021/jo034455t
_journal_volume                  68
_journal_year                    2003
_chemical_formula_sum            'C19 H22 N2 O'
_chemical_formula_weight         294.39
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   'at N5 from difmap, other geom'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.88(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.315(2)
_cell_length_b                   10.086(1)
_cell_length_c                   17.440(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      46.74
_cell_measurement_theta_min      40.22
_cell_volume                     1736.2(5)
_computing_cell_refinement       'Express (Nonius B.V., 1994)'
_computing_data_collection       'Express (Nonius B.V., 1994)'
_computing_data_reduction        'MolEN (Fair, 1990)'
_computing_molecular_graphics    'Diamond (Brandenburg, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       '\w/2\q 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  0.0211
_diffrn_reflns_av_sigmaI/netI    0.0318
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            3731
_diffrn_reflns_theta_full        74.27
_diffrn_reflns_theta_max         74.27
_diffrn_reflns_theta_min         4.48
_diffrn_standards_decay_%        1.8
_diffrn_standards_interval_count 250
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.547
_exptl_absorpt_correction_T_max  0.9474
_exptl_absorpt_correction_T_min  0.8755
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'via \y scan data'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.126
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       pyramid
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.166
_refine_diff_density_min         -0.193
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    'refined as riding atoms'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         3530
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0851
_refine_ls_R_factor_gt           0.0497
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0730P)^2^+0.3448P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1289
_refine_ls_wR_factor_ref         0.1493
_reflns_number_gt                2425
_reflns_number_total             3530
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo034455tsi20030709_093252.cif
_cod_data_source_block           wue1646
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4022464