Carbon Radical Generation by d0 Tantalum Complexes with α-Diimine Ligands through Ligand-Centered Redox Processes
Hayato Tsurugi; Teruhiko Saito; Hiromasa Tanahashi; John Arnold; Kazushi Mashima; Journal of the American Chemical Society 133 (2011) 18673–18683; doi:10.1021/ja204665s

data_4107131
_publ_section_title
;
 Carbon Radical Generation by d0 Tantalum Complexes with \a-Diimine
 Ligands through Ligand-Centered Redox Processes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              18673
_journal_page_last               18683
_journal_paper_doi               10.1021/ja204665s
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C72 H80 Cl5 N4 Ta2, Cl6 Ta, 2(C H2 Cl2)'
_chemical_formula_sum            'C74 H84 Cl15 N4 Ta3'
_chemical_formula_weight         2104.05
_chemical_name_common            3c
_chemical_name_systematic
; 
 ? 
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                111.449(2)
_cell_angle_beta                 102.867(2)
_cell_angle_gamma                101.062(2)
_cell_formula_units_Z            2
_cell_length_a                   15.355(4)
_cell_length_b                   16.774(5)
_cell_length_c                   18.605(5)
_cell_measurement_reflns_used    10990
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      3.04
_cell_volume                     4146(2)
_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    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_sigmaI/netI    0.0504
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            36809
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    4.474
_exptl_absorpt_correction_T_max  0.4681
_exptl_absorpt_correction_T_min  0.4681
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.685
_exptl_crystal_description       block
_exptl_crystal_F_000             2060
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.20
_refine_diff_density_max         12.589
_refine_diff_density_min         -2.555
_refine_diff_density_rms         0.253
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     865
_refine_ls_number_reflns         16624
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0556
_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^)+(0.0865P)^2^+55.6196P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1565
_refine_ls_wR_factor_ref         0.1601
_reflns_number_gt                15281
_reflns_number_total             16624
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja204665s_si_002_2.cif
_cod_data_source_block           3c
_cod_original_cell_volume        4146.1(19)
_cod_database_code               4107131