Evidence for a NiI Active Species in the Catalytic Cross-Coupling of Alkyl Electrophiles
Thomas J. Anderson; Gavin D. Jones; David A. Vicic; Journal of the American Chemical Society 126 (2004) 8100–8101; doi:10.1021/ja0483903

data_4112726
_publ_section_title
;
 Evidence for a NiI Active Species in the Catalytic Cross-Coupling of
 Alkyl Electrophiles
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8100
_journal_page_last               8101
_journal_paper_doi               10.1021/ja0483903
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C16 H14 N3 Ni'
_chemical_formula_weight         307.01
_chemical_name_systematic
; 
 ? 
;
_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                73.6(3)
_cell_angle_beta                 68.1(3)
_cell_angle_gamma                68.0(2)
_cell_formula_units_Z            12
_cell_length_a                   13.80(5)
_cell_length_b                   18.43(6)
_cell_length_c                   18.41(7)
_cell_measurement_reflns_used    54
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.0212
_cell_measurement_theta_min      2.3355
_cell_volume                     3972(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.915
_diffrn_measured_fraction_theta_max 0.915
_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  0.1536
_diffrn_reflns_av_sigmaI/netI    0.3955
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            22117
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.34
_exptl_absorpt_coefficient_mu    2.184
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5709
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            violet/black
_exptl_crystal_density_diffrn    2.309
_exptl_crystal_description       plate
_exptl_crystal_F_000             2862
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.562
_refine_diff_density_min         -0.660
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1088
_refine_ls_number_reflns         14277
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.173
_refine_ls_R_factor_all          0.3490
_refine_ls_R_factor_gt           0.1867
_refine_ls_shift/su_max          2.466
_refine_ls_shift/su_mean         0.017
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+43.3621P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2776
_refine_ls_wR_factor_ref         0.3508
_reflns_number_gt                5327
_reflns_number_total             14277
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0483903si20040321_073905_1.cif
_cod_data_source_block           tpyNiMe
_cod_original_cell_volume        3974(24)
_cod_database_code               4112726