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_4126181
_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         'C42 H72 Cl4 N3 Nb'
_chemical_formula_sum            'C42 H72 Cl4 N3 Nb'
_chemical_formula_weight         853.77
_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                 104.615(4)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   15.1156(12)
_cell_length_b                   13.1540(8)
_cell_length_c                   24.238(3)
_cell_measurement_reflns_used    11187
_cell_measurement_temperature    113
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      3.03
_cell_volume                     4663.3(7)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      113
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            44154
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.46
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.517
_exptl_absorpt_correction_T_max  0.784
_exptl_absorpt_correction_T_min  0.727
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1816.00
_exptl_crystal_size_max          0.660
_exptl_crystal_size_mid          0.520
_exptl_crystal_size_min          0.470
_refine_diff_density_max         1.650
_refine_diff_density_min         -0.820
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     431
_refine_ls_number_reflns         10604
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0608
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0736P)^2^+8.5983P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1613
_reflns_number_gt                9460
_reflns_number_total             10604
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja7b02710_si_002.cif
_cod_data_source_block           5b
_cod_database_code               4126181