Mechanistic Features of Isomerizing Alkoxycarbonylation of Methyl Oleate
Philipp Roesle; Christoph J. Dürr; Heiko M. Möller; Luigi Cavallo; Lucia Caporaso; Stefan Mecking; Journal of the American Chemical Society 134 (2012) 17696–17703; doi:10.1021/ja307411p

data_4118809
_publ_contact_author_address
;Chair of Chemical Materials Science
Department of Chemistry
University of Konstanz
78464 Konstanz
Germany
;
_publ_contact_author_email       stefan.mecking@uni-konstanz.de
_publ_contact_author_fax         00497531885152
_publ_contact_author_name        'Pofessor Stefan Mecking'
_publ_contact_author_phone       00497531882593
_publ_section_title
;
 Mechanistic Features of Isomerizing Alkoxycarbonylation of Methyl Oleate
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17696
_journal_page_last               17703
_journal_paper_doi               10.1021/ja307411p
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C20 H42 F3 O3 P2 Pd S, C F3 O3  S'
_chemical_formula_sum            'C21 H42 F6 O6 P2 Pd S2'
_chemical_formula_weight         737.01
_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   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 116.419(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.1681(6)
_cell_length_b                   16.4128(7)
_cell_length_c                   22.4646(8)
_cell_measurement_reflns_used    62659
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.15
_cell_measurement_theta_min      1.60
_cell_volume                     5999.1(4)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_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 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0532
_diffrn_reflns_av_sigmaI/netI    0.0292
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            76320
_diffrn_reflns_theta_full        25.77
_diffrn_reflns_theta_max         25.77
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    0.936
_exptl_absorpt_correction_T_max  0.8879
_exptl_absorpt_correction_T_min  0.7371
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED32'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_description       platelet
_exptl_crystal_F_000             3024
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.263
_exptl_crystal_size_min          0.110
_refine_diff_density_max         2.035
_refine_diff_density_min         -1.248
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.330
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     709
_refine_ls_number_reflns         11310
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.330
_refine_ls_R_factor_all          0.0806
_refine_ls_R_factor_gt           0.0727
_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^)+(0.0000P)^2^+88.7993P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1620
_refine_ls_wR_factor_ref         0.1646
_reflns_number_gt                10162
_reflns_number_total             11310
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja307411p_si_002.cif
_cod_data_source_block           d:\dtbpppdotf\gs11_001
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4118809