A Comprehensive Mechanistic Picture of the Isomerizing Alkoxycarbonylation of Plant Oils
Roesle, Philipp; Caporaso, Lucia; Schnitte, Manuel; Goldbach, Verena; Cavallo, Luigi; Mecking, Stefan; Journal of the American Chemical Society  (2014) 141121132036004–; doi:10.1021/ja508447d

data_4123015
_publ_section_title
;
 A Comprehensive Mechanistic Picture of the Isomerizing
 Alkoxycarbonylation of Plant Oils
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              141121132036004
_journal_paper_doi               10.1021/ja508447d
_journal_year                    2014
_chemical_formula_moiety         'C21 H44 F3 O3 P2 Pd S, C F3 O3 S'
_chemical_formula_sum            'C22 H44 F6 O6 P2 Pd S2'
_chemical_formula_weight         751.03
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.818(5)
_cell_angle_beta                 85.071(5)
_cell_angle_gamma                86.760(5)
_cell_formula_units_Z            2
_cell_length_a                   10.7915(6)
_cell_length_b                   11.2935(6)
_cell_length_c                   12.4906(7)
_cell_measurement_reflns_used    35227
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.37
_cell_measurement_theta_min      1.90
_cell_volume                     1514.22(14)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED32'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_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  0.1033
_diffrn_reflns_av_sigmaI/netI    0.0808
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            24930
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    0.928
_exptl_absorpt_correction_T_max  0.8945
_exptl_absorpt_correction_T_min  0.6556
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED32'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             772
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.789
_refine_diff_density_min         -0.545
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         7211
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0252
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0221P)^2^+0.8565P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0516
_refine_ls_wR_factor_ref         0.0525
_reflns_number_gt                6619
_reflns_number_total             7211
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja508447d_si_005.cif
_cod_data_source_block           d:\dtbpbpdotf
_cod_database_code               4123015