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_4106597
_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 H68 B F24 N Ni P2'
_chemical_formula_weight         1390.61
_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                95.168(2)
_cell_angle_beta                 100.073(2)
_cell_angle_gamma                103.594(2)
_cell_formula_units_Z            4
_cell_length_a                   16.6160(19)
_cell_length_b                   19.441(2)
_cell_length_c                   20.680(2)
_cell_measurement_reflns_used    128
_cell_measurement_temperature    373(2)
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      0
_cell_volume                     6332.7(12)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      373(2)
_diffrn_measured_fraction_theta_full 0.902
_diffrn_measured_fraction_theta_max 0.902
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_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  0.0514
_diffrn_reflns_av_sigmaI/netI    0.1143
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            40000
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         1.09
_exptl_absorpt_coefficient_mu    0.466
_exptl_absorpt_correction_T_max  0.3737
_exptl_absorpt_correction_T_min  0.3152
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            green-blue
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_description       prism
_exptl_crystal_F_000             2856
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.850
_refine_diff_density_min         -1.057
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1611
_refine_ls_number_reflns         28323
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.1379
_refine_ls_R_factor_gt           0.0981
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0752P)^2^+12.8734P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2048
_refine_ls_wR_factor_ref         0.2238
_reflns_number_gt                19978
_reflns_number_total             28323
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2024993_si_002_3.cif
_cod_data_source_block           vlad115m
_cod_original_cell_volume        6332.8(12)
_cod_database_code               4106597