Pd-Catalyzed Copolymerization of Methyl Acrylate with Carbon Monoxide: Structures, Properties and Mechanistic Aspects toward Ligand Design
Akifumi Nakamura; Kagehiro Munakata; Shingo Ito; Takuya Kochi; Lung Wa Chung; Keiji Morokuma; Kyoko Nozaki; Journal of the American Chemical Society 133 (2011) 6761–6779; doi:10.1021/ja2003268

data_4106070
_publ_section_title
;
 Pd-Catalyzed Copolymerization of Methyl Acrylate with Carbon Monoxide:
 Structures, Properties and Mechanistic Aspects toward Ligand Design
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6761
_journal_page_last               6779
_journal_paper_doi               10.1021/ja2003268
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C37 H41 F3 O7 P2 Pd S'
_chemical_formula_weight         855.10
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                90.0000
_cell_angle_beta                 96.5948(13)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   9.252(3)
_cell_length_b                   24.067(8)
_cell_length_c                   17.032(6)
_cell_measurement_reflns_used    6678
_cell_measurement_temperature    103.1500
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      3.1929
_cell_volume                     3767(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      103(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'RIGAKU/MSC Meacury 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     0.71070
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_av_sigmaI/netI    0.0424
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14582
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.19
_exptl_absorpt_coefficient_mu    0.695
_exptl_absorpt_correction_T_max  0.9029
_exptl_absorpt_correction_T_min  0.7011
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_description       Block
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.906
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details 'Flack (1983), 3212 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.021(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         7521
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0285
_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^)+(0.0291P)^2^+0.1629P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0619
_refine_ls_wR_factor_ref         0.0635
_reflns_number_gt                7137
_reflns_number_total             7521
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2003268_si_002.cif
_cod_data_source_block           dppepdma
_cod_database_code               4106070