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_4119845
_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_sum            'C38 H35 F10 N3 Ni'
_chemical_formula_weight         782.40
_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                 101.288(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.6079(3)
_cell_length_b                   19.1642(5)
_cell_length_c                   18.4101(5)
_cell_measurement_temperature    100(2)
_cell_volume                     3670.23(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0587
_diffrn_reflns_av_sigmaI/netI    0.0452
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            34054
_diffrn_reflns_theta_full        25.44
_diffrn_reflns_theta_max         25.44
_diffrn_reflns_theta_min         2.96
_exptl_absorpt_coefficient_mu    0.611
_exptl_absorpt_correction_T_max  0.9415
_exptl_absorpt_correction_T_min  0.8673
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.521
_refine_diff_density_min         -0.611
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         6747
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0994
_refine_ls_R_factor_gt           0.0706
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0804P)^2^+12.7548P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1707
_refine_ls_wR_factor_ref         0.1907
_reflns_number_gt                4979
_reflns_number_total             6747
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4030462_si_002_3.cif
_cod_data_source_block           Compound9
_cod_database_code               4119845