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_4120223
_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            'C34 H35 Cs O5 Pd'
_chemical_formula_weight         762.93
_chemical_name_systematic
; 
 ? 
;
_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                109.830(5)
_cell_angle_beta                 94.785(6)
_cell_angle_gamma                100.526(2)
_cell_formula_units_Z            2
_cell_length_a                   9.403(4)
_cell_length_b                   12.127(5)
_cell_length_c                   14.748(5)
_cell_measurement_reflns_used    3310
_cell_measurement_temperature    138(2)
_cell_measurement_theta_max      30.4468
_cell_measurement_theta_min      1.8322
_cell_volume                     1536.0(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      138(2)
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_av_sigmaI/netI    0.0725
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9182
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    1.812
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5442
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.649
_exptl_crystal_description       prism
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.207
_exptl_crystal_size_mid          0.051
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.836
_refine_diff_density_min         -3.046
_refine_diff_density_rms         0.306
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         5187
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.1055
_refine_ls_R_factor_gt           0.0802
_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^)+(0.1896P)^2^+1.1912P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2317
_refine_ls_wR_factor_ref         0.2870
_reflns_number_gt                3776
_reflns_number_total             5187
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja405503y_si_003.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        1536.1(10)
_cod_database_code               4120223