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_4106596
_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            'C74 H77 B F24 N Ni P2'
_chemical_formula_weight         1567.83
_chemical_name_systematic
;

 

 ?

 

;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 90.907(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.2589(12)
_cell_length_b                   13.0889(11)
_cell_length_c                   39.706(3)
_cell_measurement_reflns_used    102
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.12
_cell_measurement_theta_min      2.55
_cell_volume                     7409.5(10)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.896
_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  0.0774
_diffrn_reflns_av_sigmaI/netI    0.1224
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            41170
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.03
_exptl_absorpt_coefficient_mu    0.408
_exptl_absorpt_correction_T_max  0.977
_exptl_absorpt_correction_T_min  0.960
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'Norton et al'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_description       block
_exptl_crystal_F_000             3228
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.775
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     945
_refine_ls_number_reflns         16471
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.1241
_refine_ls_R_factor_gt           0.0714
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0438P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1251
_refine_ls_wR_factor_ref         0.1433
_reflns_number_gt                10016
_reflns_number_total             16471
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2024993_si_002_2.cif
_cod_data_source_block           vlad817m
_cod_original_cell_volume        7409.5(11)
_cod_database_code               4106596