C-H vs C-C Bond Activation of Acetonitrile and Benzonitrile via Oxidative Addition: Rhodium vs Nickel and Cp* vs Tp' (Tp' = Hydrotris(3,5-dimethylpyrazol-1-yl)borate, Cp* = η5-Pentamethylcyclopentadienyl)
Meagan E. Evans; Ting Li; William D. Jones; Journal of the American Chemical Society 132 (2010) 16278–16284; doi:10.1021/ja107927b

data_4103527
_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
;
 C-H vs C-C Bond Activation of Acetonitrile and Benzonitrile via Oxidative
 Addition: Rhodium vs Nickel and Cp* vs Tp' (Tp' =
 Hydrotris(3,5-dimethylpyrazol-1-yl)borate, Cp* =
 \h5-Pentamethylcyclopentadienyl)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16278
_journal_page_last               16284
_journal_paper_doi               10.1021/ja107927b
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C20 H29 N P Rh, 0.5(H2 O)'
_chemical_formula_sum            'C20 H30 N O0.5 P Rh'
_chemical_formula_weight         426.33
_chemical_name_common            jonme12
_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                89.287(3)
_cell_angle_beta                 76.682(3)
_cell_angle_gamma                67.204(3)
_cell_formula_units_Z            2
_cell_length_a                   8.1053(13)
_cell_length_b                   8.7271(13)
_cell_length_c                   15.880(2)
_cell_measurement_reflns_used    4057
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      37.76
_cell_measurement_theta_min      2.81
_cell_volume                     1004.0(3)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2010)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0365
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            31455
_diffrn_reflns_theta_full        36.32
_diffrn_reflns_theta_max         36.32
_diffrn_reflns_theta_min         1.32
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.933
_exptl_absorpt_correction_T_max  0.9125
_exptl_absorpt_correction_T_min  0.7934
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             442
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.890
_refine_diff_density_min         -0.919
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     233
_refine_ls_number_reflns         9623
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0289
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0325P)^2^+0.1660P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0663
_refine_ls_wR_factor_ref         0.0697
_reflns_number_gt                8452
_reflns_number_total             9623
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja107927b_si_002_3.cif
_cod_data_source_block           5
_cod_database_code               4103527