Structural and Electronic Noninnocence of α-Diimine Ligands on Niobium for Reductive C-Cl Bond Activation and Catalytic Radical Addition Reactions.
Nishiyama, Haruka; Ikeda, Hideaki; Saito, Teruhiko; Kriegel, Benjamin; Tsurugi, Hayato; Arnold, John; Mashima, Kazushi; Journal of the American Chemical Society 139 (2017) 6494–6505; doi:10.1021/jacs.7b02710

data_4126180
_publ_section_title
;
 Structural and Electronic Noninnocence of \a-Diimine Ligands on Niobium
 for Reductive C-Cl Bond Activation and Catalytic Radical Addition
 Reactions.
;
_journal_issue                   18
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6494
_journal_page_last               6505
_journal_paper_doi               10.1021/jacs.7b02710
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'C26 H36 Cl4 N2 Nb'
_chemical_formula_sum            'C26 H36 Cl4 N2 Nb'
_chemical_formula_weight         611.30
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_cell_angle_alpha                90.1387(18)
_cell_angle_beta                 90.051(3)
_cell_angle_gamma                90.043(3)
_cell_formula_units_Z            4
_cell_length_a                   10.4231(9)
_cell_length_b                   12.6112(9)
_cell_length_c                   21.4888(15)
_cell_measurement_reflns_used    28870
_cell_measurement_temperature    113
_cell_measurement_theta_max      27.66
_cell_measurement_theta_min      3.17
_cell_volume                     2824.6(4)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      113
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0612
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            56457
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.821
_exptl_absorpt_correction_T_max  0.775
_exptl_absorpt_correction_T_min  0.349
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1260.00
_exptl_crystal_size_max          0.510
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.310
_refine_diff_density_max         1.620
_refine_diff_density_min         -2.010
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     611
_refine_ls_number_reflns         12755
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0872
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0942P)^2^+20.2053P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2344
_reflns_number_gt                10167
_reflns_number_total             12755
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja7b02710_si_002.cif
_cod_data_source_block           6b
_cod_database_code               4126180