Palladium(II)-Catalyzed Direct Carboxylation of Alkenyl C-H Bonds with CO2
Kota Sasano; Jun Takaya; Nobuharu Iwasawa; Journal of the American Chemical Society 135 (2013) 10954–10957; doi:10.1021/ja405503y

data_4120222
_publ_section_title
;
 Palladium(II)-Catalyzed Direct Carboxylation of Alkenyl C-H Bonds with
 CO2
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10954
_journal_page_last               10957
_journal_paper_doi               10.1021/ja405503y
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C26 H18 N2 O Pd'
_chemical_formula_weight         480.82
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 92.712(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   28.977(6)
_cell_length_b                   7.7766(13)
_cell_length_c                   17.185(3)
_cell_measurement_reflns_used    5457
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.4855
_cell_measurement_theta_min      3.1065
_cell_volume                     3868.2(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0339
_diffrn_reflns_av_sigmaI/netI    0.0253
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            23013
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.36
_exptl_absorpt_coefficient_mu    0.981
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9298
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.651
_exptl_crystal_description       prism
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.657
_refine_diff_density_min         -0.891
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         4427
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0367
_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^)+(0.0367P)^2^+12.0393P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0807
_refine_ls_wR_factor_ref         0.0837
_reflns_number_gt                3982
_reflns_number_total             4427
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja405503y_si_002.cif
_cod_data_source_block           crystalclear
_cod_database_code               4120222