Preparation of Stable Alkyl Complexes of Ni(I) and Their One-Electron Oxidation to Ni(II) Complex Cations
Kristina D. Kitiachvili; Daniel J. Mindiola; Gregory L. Hillhouse; Journal of the American Chemical Society 126 (2004) 10554–10555; doi:10.1021/ja047052z

data_4112896
_publ_section_title
;
 Preparation of Stable Alkyl Complexes of Ni(I) and Their One-Electron
 Oxidation to Ni(II) Complex Cations
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10554
_journal_page_last               10555
_journal_paper_doi               10.1021/ja047052z
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C22 H51 F6 Ni P3 Si'
_chemical_formula_weight         609.34
_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                 92.104(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.806(3)
_cell_length_b                   18.744(5)
_cell_length_c                   13.238(4)
_cell_measurement_temperature    373(2)
_cell_volume                     2927.5(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.939
_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  0.0591
_diffrn_reflns_av_sigmaI/netI    0.0729
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17701
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    0.916
_exptl_absorpt_correction_T_max  0.9303
_exptl_absorpt_correction_T_min  0.8980
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   empirical
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_description       plate
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.079
_refine_diff_density_min         -0.630
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         6874
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0902
_refine_ls_R_factor_gt           0.0711
_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^)+(0.0660P)^2^+2.1196P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1490
_refine_ls_wR_factor_ref         0.1571
_reflns_number_gt                5494
_reflns_number_total             6874
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja047052zsi20040719_032902.cif
_cod_data_source_block           danm17t
_cod_original_cell_volume        2927.4(14)
_cod_database_code               4112896