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_4108520
_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            'C146 H140 B2 Cl8 F48 N6 Ni2 O0'
_chemical_formula_weight         3313.28
_chemical_name_systematic
; 
 ? 
;
_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                102.917(4)
_cell_angle_beta                 101.969(4)
_cell_angle_gamma                114.548(4)
_cell_formula_units_Z            1
_cell_length_a                   16.127(3)
_cell_length_b                   16.608(4)
_cell_length_c                   16.626(3)
_cell_measurement_temperature    100(2)
_cell_volume                     3714.8(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0866
_diffrn_reflns_av_sigmaI/netI    0.1267
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15536
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.44
_exptl_absorpt_coefficient_mu    0.510
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_description       block
_exptl_crystal_F_000             1692
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.309
_refine_diff_density_min         -1.201
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     981
_refine_ls_number_reflns         9639
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1504
_refine_ls_R_factor_gt           0.1048
_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^)+(0.1938P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2813
_refine_ls_wR_factor_ref         0.3071
_reflns_number_gt                5851
_reflns_number_total             9639
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja805804s_si_002_4.cif
_cod_data_source_block           carl19a
_cod_original_cell_volume        3714.7(13)
_cod_database_code               4108520