Two-Coordinate d9 Complexes. Synthesis and Oxidation of NHC Nickel(I) Amides
Carl A. Laskowski; Gregory L. Hillhouse; Journal of the American Chemical Society 130 (2008) 13846–13847; doi:10.1021/ja805804s

data_4108519
_publ_section_title
;
 Two-Coordinate d9 Complexes. Synthesis and Oxidation of NHC Nickel(I)
 Amides
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13846
_journal_page_last               13847
_journal_paper_doi               10.1021/ja805804s
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C87 H74 B F24 N3 Ni O4'
_chemical_formula_weight         1751.01
_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                 96.741(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.789(2)
_cell_length_b                   32.507(5)
_cell_length_c                   20.860(3)
_cell_measurement_temperature    100(2)
_cell_volume                     8612(2)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.1337
_diffrn_reflns_av_sigmaI/netI    0.0861
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            27688
_diffrn_reflns_theta_full        20.00
_diffrn_reflns_theta_max         20.00
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    0.327
_exptl_absorpt_correction_T_max  0.3637
_exptl_absorpt_correction_T_min  0.1784
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_description       plate
_exptl_crystal_F_000             3592
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.144
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1097
_refine_ls_number_reflns         8036
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0992
_refine_ls_R_factor_gt           0.0830
_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^)+(0.1531P)^2^+15.0048P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2286
_refine_ls_wR_factor_ref         0.2431
_reflns_number_gt                6299
_reflns_number_total             8036
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja805804s_si_002_3.cif
_cod_data_source_block           carl60a
_cod_original_cell_volume        8613(2)
_cod_database_code               4108519