P-Chiral Phosphine-Sulfonate/Palladium-Catalyzed Asymmetric Copolymerization of Vinyl Acetate with Carbon Monoxide
Akifumi Nakamura; Takeharu Kageyama; Hiroki Goto; Brad P. Carrow; Shingo Ito; Kyoko Nozaki; Journal of the American Chemical Society 134 (2012) 12366–12369; doi:10.1021/ja3044344

data_4118399
_publ_section_title
;
 P-Chiral Phosphine-Sulfonate/Palladium-Catalyzed Asymmetric
 Copolymerization of Vinyl Acetate with Carbon Monoxide
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12366
_journal_page_last               12369
_journal_paper_doi               10.1021/ja3044344
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C110 H103 F6 O24 P3 Pd3 S3'
_chemical_formula_weight         2431.21
_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                114.526(4)
_cell_angle_beta                 98.0070(15)
_cell_angle_gamma                94.549(3)
_cell_formula_units_Z            2
_cell_length_a                   11.915(3)
_cell_length_b                   21.699(5)
_cell_length_c                   22.520(6)
_cell_measurement_reflns_used    15933
_cell_measurement_temperature    93.1500
_cell_measurement_theta_max      31.2920
_cell_measurement_theta_min      2.7029
_cell_volume                     5184(2)
_computing_cell_refinement       'RIGAKU CrystalClear'
_computing_data_collection       'RIGAKU CrystalClear'
_computing_data_reduction        'RIGAKU CrystalClear'
_computing_molecular_graphics    ORTEP-III
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Rigaku Saturn724 CCD'
_diffrn_measurement_method       'omega scans'
_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  0.0465
_diffrn_reflns_av_sigmaI/netI    0.0793
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            34840
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    0.707
_exptl_absorpt_correction_T_max  0.9655
_exptl_absorpt_correction_T_min  0.9014
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_description       Block
_exptl_crystal_F_000             2480
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.753
_refine_diff_density_min         -0.970
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1354
_refine_ls_number_reflns         17841
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0748
_refine_ls_R_factor_gt           0.0579
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0425P)^2^+10.0511P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1188
_refine_ls_wR_factor_ref         0.1300
_reflns_number_gt                14355
_reflns_number_total             17841
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja3044344_si_004.cif
_cod_data_source_block           phbivac
_cod_database_code               4118399