Experimental and Theoretical Examination of C-CN and C-H Bond Activations of Acetonitrile Using Zerovalent Nickel
Tülay A. Ateşin; Ting Li; Sébastien Lachaize; William W. Brennessel; Juventino J. García; William D. Jones; Journal of the American Chemical Society 129 (2007) 7562–7569; doi:10.1021/ja0707153

data_4109537
_publ_contact_author_address
'Department of Chemistry, University of Rochester, Rochester, New York 14627'
_publ_contact_author_email       jones@chem.rochester.edu
_publ_contact_author_name        'William D. Jones'
_publ_section_title
;
 Experimental and Theoretical Examination of C-CN and C-H Bond Activations
 of Acetonitrile Using Zerovalent Nickel
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7562
_journal_page_last               7569
_journal_paper_doi               10.1021/ja0707153
_journal_volume                  129
_journal_year                    2007
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C22 H50 B N Ni P2'
_chemical_formula_sum            'C22 H50 B N Ni P2'
_chemical_formula_weight         460.09
_chemical_name_common            jontl04
_chemical_name_systematic        Ni(dippe)(CH3CNBEt3)
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   9.0897(13)
_cell_length_b                   20.487(3)
_cell_length_c                   43.135(6)
_cell_measurement_reflns_used    9820
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      33.25
_cell_measurement_theta_min      2.24
_cell_volume                     8033(2)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'APEX2, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'SHELXTL, Bruker'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97, CNR-IC'
_diffrn_ambient_temperature      100.0(1)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD Platform'
_diffrn_measurement_method       'area detector, \w scans per \f'
_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  0.0470
_diffrn_reflns_av_sigmaI/netI    0.0392
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       65
_diffrn_reflns_limit_l_min       -65
_diffrn_reflns_number            145478
_diffrn_reflns_theta_full        32.57
_diffrn_reflns_theta_max         32.57
_diffrn_reflns_theta_min         1.37
_exptl_absorpt_coefficient_mu    0.852
_exptl_absorpt_correction_T_max  0.8217
_exptl_absorpt_correction_T_min  0.7723
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.141
_exptl_crystal_description       block
_exptl_crystal_F_000             3024
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.559
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details
'Flack H D (1983), 13166 Friedel pairs, Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.440(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     767
_refine_ls_number_reflns         29006
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0397
_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^)+(0.0287P)^2^+3.1744P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0814
_refine_ls_wR_factor_ref         0.0843
_reflns_number_gt                25499
_reflns_number_total             29006
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0707153si20070202_122302_2.cif
_cod_data_source_block           jontl04
_cod_database_code               4109537