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_4119846
_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            'C68 H87 F14 N9 Ni3 O'
_chemical_formula_weight         1488.60
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
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_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                 98.476(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.819(3)
_cell_length_b                   11.1285(12)
_cell_length_c                   25.279(3)
_cell_measurement_temperature    100(2)
_cell_volume                     7184.0(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.680
_diffrn_measured_fraction_theta_max 0.680
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            20790
_diffrn_reflns_theta_full        29.24
_diffrn_reflns_theta_max         29.24
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    0.862
_exptl_absorpt_correction_T_max  0.8962
_exptl_absorpt_correction_T_min  0.7136
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_F_000             3104
_exptl_crystal_size_max          0.42
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_refine_diff_density_max         1.187
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_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
_refine_ls_number_parameters     877
_refine_ls_number_reflns         13285
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.1635
_refine_ls_R_factor_gt           0.0767
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1042P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1765
_refine_ls_wR_factor_ref         0.2135
_reflns_number_gt                6809
_reflns_number_total             13285
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4030462_si_002_4.cif
_cod_data_source_block           Compound10
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' tag value 'monoclinin' was replaced with
'monoclinic' value as specified in the replacement file
'/home/robertas/cod-tools/perl-scripts/inputs/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        7184.1(14)
_cod_database_code               4119846