Synthesis and Characterization of Three-Coordinate Ni(III)-Imide Complexes
Vlad M. Iluc; Alexander J. M. Miller; John S. Anderson; Marisa J. Monreal; Mark P. Mehn; Gregory L. Hillhouse; Journal of the American Chemical Society 133 (2011) 13055–13063; doi:10.1021/ja2024993

data_4106595
_publ_section_title
;
 Synthesis and Characterization of Three-Coordinate Ni(III)-Imide
 Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13055
_journal_page_last               13063
_journal_paper_doi               10.1021/ja2024993
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C60 H67 B F24 N Ni P2'
_chemical_formula_weight         1389.61
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_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                 112.082(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.736(5)
_cell_length_b                   16.476(4)
_cell_length_c                   23.481(6)
_cell_measurement_reflns_used    11176
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.55
_cell_volume                     6358(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0381
_diffrn_reflns_av_sigmaI/netI    0.0458
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            32564
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.55
_exptl_absorpt_coefficient_mu    0.465
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_F_000             2852
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.685
_refine_diff_density_min         -0.351
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.236
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     868
_refine_ls_number_reflns         11176
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.236
_refine_ls_R_factor_all          0.0837
_refine_ls_R_factor_gt           0.0717
_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^)+(0.0487P)^2^+0.0146P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1453
_refine_ls_wR_factor_ref         0.1500
_reflns_number_gt                9654
_reflns_number_total             11176
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2024993_si_002_1.cif
_cod_data_source_block           vlad111s
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4106595