Bimetallic Nickel Aluminun Mediated Para-Selective Alkenylation of Pyridine: Direct Observation of η2,η1-Pyridine Ni(0)-Al(III) Intermediates Prior to C-H Bond Activation
Chung-Chih Tsai; Wei-Chih Shih; Cyong-Hui Fang; Chia-Yi Li; Tiow-Gan Ong; Glenn P. A. Yap; Journal of the American Chemical Society 132 (2010) 11887–11889; doi:10.1021/ja1061246

data_4102977
_publ_section_title
;
 Bimetallic Nickel Aluminun Mediated Para-Selective Alkenylation of
 Pyridine: Direct Observation of \h2,\h1-Pyridine Ni(0)-Al(III)
 Intermediates Prior to C-H Bond Activation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11887
_journal_page_last               11889
_journal_paper_doi               10.1021/ja1061246
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C48 H76 Al N7 Ni O'
_chemical_formula_weight         852.85
_chemical_name_systematic
;
 ?
;
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.805(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.7429(5)
_cell_length_b                   13.5697(4)
_cell_length_c                   18.3723(5)
_cell_measurement_reflns_used    9832
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.03
_cell_measurement_theta_min      2.70
_cell_volume                     4887.4(2)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2001)'
_computing_publication_material  'SHELXTL (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 836.6
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker AXS APEX diffractometer'
_diffrn_measurement_method       \w
_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  0.0467
_diffrn_reflns_av_sigmaI/netI    0.0406
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            60922
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         1.87
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.456
_exptl_absorpt_correction_T_max  0.8946
_exptl_absorpt_correction_T_min  0.8754
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2003)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.159
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.469
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     572
_refine_ls_number_reflns         10774
_refine_ls_number_restraints     131
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0389
_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^)+(0.0464P)^2^+2.3792P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0913
_refine_ls_wR_factor_ref         0.1018
_reflns_number_gt                8285
_reflns_number_total             10774
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1061246_si_001.cif
_cod_data_source_block           i12041
_cod_database_code               4102977