A Five-Coordinate Nickel(II) Fluoroalkyl Complex as a Precursor to a Spectroscopically Detectable Ni(III) Species
Cheng-Pan Zhang; Huan Wang; Axel Klein; Christian Biewer; Kathrin Stirnat; Yoshitaka Yamaguchi; Long Xu; Valente Gomez-Benitez; David A. Vicic; Journal of the American Chemical Society 135 (2013) 8141–8144; doi:10.1021/ja4030462

data_4119844
_publ_section_title
;
 A Five-Coordinate Nickel(II) Fluoroalkyl Complex as a Precursor to a
 Spectroscopically Detectable Ni(III) Species
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8141
_journal_page_last               8144
_journal_paper_doi               10.1021/ja4030462
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C18 H15 F6 N2 Ni'
_chemical_formula_sum            'C18 H15 F6 N2 Ni'
_chemical_formula_weight         432.02
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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
_cell_angle_alpha                90.0000
_cell_angle_beta                 99.448(15)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   8.015(8)
_cell_length_b                   13.092(13)
_cell_length_c                   19.236(19)
_cell_measurement_reflns_used    2331
_cell_measurement_temperature    273
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      1.89
_cell_volume                     1991(3)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r7'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r7'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      273
_diffrn_detector_area_resol_mean 13.653
_diffrn_measured_fraction_theta_full 0.868
_diffrn_measured_fraction_theta_max 0.868
_diffrn_measurement_device_type  'Rigaku Mercury275R CCD (SCX mini)'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1195
_diffrn_reflns_limit_h_max       2
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            6959
_diffrn_reflns_theta_full        27.44
_diffrn_reflns_theta_max         27.44
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.032
_exptl_absorpt_correction_T_max  0.814
_exptl_absorpt_correction_T_min  0.522
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_description       prism
_exptl_crystal_F_000             876.00
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.100
_refine_diff_density_min         -0.530
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     238
_refine_ls_number_reflns         3980
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.1175
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.3979
_reflns_number_gt                1664
_reflns_number_total             4122
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja4030462_si_002_2.cif
_cod_data_source_block           '_Compound6'
_cod_database_code               4119844