γ-Agostic Species as Key Intermediates in the Vinyl Addition Polymerization of Norbornene with Cationic (allyl)Pd Catalysts: Synthesis and Mechanistic Insights
Marc D. Walter; Rebecca A. Moorhouse; Stephanie A. Urbin; Peter S. White; Maurice Brookhart; Journal of the American Chemical Society 131 (2009) 9055–9069; doi:10.1021/ja9025598

data_4104611
_publ_section_title
;
 \g-Agostic Species as Key Intermediates in the Vinyl Addition
 Polymerization of Norbornene with Cationic (allyl)Pd Catalysts: Synthesis
 and Mechanistic Insights
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9055
_journal_page_last               9069
_journal_paper_doi               10.1021/ja9025598
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C21 H27 N2 Pd, Sb F6'
_chemical_formula_sum            'C21 H27 F6 N2 Pd Sb'
_chemical_formula_weight         649.60
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.169(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.8670(2)
_cell_length_b                   18.4716(3)
_cell_length_c                   13.4204(3)
_cell_measurement_reflns_used    9944
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      24.86
_cell_measurement_theta_min      2.34
_cell_volume                     2444.24(8)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      250(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker-AXS SMART APEX-II CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0298
_diffrn_reflns_av_sigmaI/netI    0.0163
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            33289
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    1.896
_exptl_absorpt_correction_T_max  0.7029
_exptl_absorpt_correction_T_min  0.6486
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            clear
_exptl_crystal_density_diffrn    1.765
_exptl_crystal_description       block
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.972
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         4296
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0650P)^2^+5.8513P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1262
_refine_ls_wR_factor_ref         0.1341
_reflns_number_gt                3609
_reflns_number_total             4296
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9025598_si_002.cif
_cod_data_source_block           c07252
_cod_database_code               4104611