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_4112898
_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            'C60 H65 B F24 Ni P2'
_chemical_formula_weight         1373.58
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 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            4
_cell_length_a                   35.135(3)
_cell_length_b                   12.7230(11)
_cell_length_c                   13.4387(12)
_cell_measurement_temperature    373(2)
_cell_volume                     6007.4(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.970
_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  0.0508
_diffrn_reflns_av_sigmaI/netI    0.0614
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            35954
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    0.490
_exptl_absorpt_correction_T_max  0.9854
_exptl_absorpt_correction_T_min  0.9257
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   empirical
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_description       prizm
_exptl_crystal_F_000             2816
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.367
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.035(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     803
_refine_ls_number_reflns         13953
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.0579
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0681P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1283
_refine_ls_wR_factor_ref         0.1317
_reflns_number_gt                12570
_reflns_number_total             13953
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja047052zsi20040719_032951.cif
_cod_data_source_block           kristinm
_cod_database_code               4112898