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_4119843
_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         'C6 H6 F6 N2 Ni'
_chemical_formula_sum            'C6 H6 F6 N2 Ni'
_chemical_formula_weight         278.82
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_symmetry_cell_setting           monoclinic
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_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            12
_cell_length_a                   8.200(16)
_cell_length_b                   17.10(3)
_cell_length_c                   21.72(4)
_cell_measurement_reflns_used    3170
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.20
_cell_measurement_theta_min      2.40
_cell_volume                     3046(10)
_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      173
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Rigaku Mercury70 CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1463
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_diffrn_reflns_limit_h_min       -10
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_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
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_diffrn_reflns_theta_full        27.21
_diffrn_reflns_theta_max         27.21
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.967
_exptl_absorpt_correction_T_max  0.854
_exptl_absorpt_correction_T_min  0.631
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.824
_exptl_crystal_description       prism
_exptl_crystal_F_000             1656.00
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.780
_refine_diff_density_min         -1.000
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_reflns         6675
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_refine_ls_shift/su_max          0.092
_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         0.4213
_reflns_number_gt                2458
_reflns_number_total             6892
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja4030462_si_002_1.cif
_cod_data_source_block           '__Compound1'
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