Electronic Structures of Homoleptic [Tris(2,2'-bipyridine)M]n Complexes of the Early Transition Metals (M = Sc, Y, Ti, Zr, Hf, V, Nb, Ta; n= 1+, 0, 1-, 2-, 3-): An Experimental and Density Functional Theoretical Study
Amanda C. Bowman; Jason England; Stephen Sproules; Thomas Weyhermüller; Karl Wieghardt; Inorganic Chemistry 52 (2013) 2242–2256; doi:10.1021/ic302799s

data_4333952
_publ_section_title
;
 Electronic Structures of Homoleptic [Tris(2,2'-bipyridine)M]n Complexes
 of the Early Transition Metals (M = Sc, Y, Ti, Zr, Hf, V, Nb, Ta; n= 1+,
 0, 1-, 2-, 3-): An Experimental and Density Functional Theoretical Study
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2242
_journal_page_last               2256
_journal_paper_doi               10.1021/ic302799s
_journal_volume                  52
_journal_year                    2013
_chemical_compound_source        tetrahydrofuran,diethylether
_chemical_formula_moiety         'C54 H72 N6 Ta, C20 H40 Na O5'
_chemical_formula_sum            'C74 H112 N6 Na O5 Ta'
_chemical_formula_weight         1369.64
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                101.796(10)
_cell_angle_beta                 98.280(12)
_cell_angle_gamma                115.563(10)
_cell_formula_units_Z            2
_cell_length_a                   13.7748(14)
_cell_length_b                   14.105(2)
_cell_length_c                   21.909(4)
_cell_measurement_reflns_used    64934
_cell_measurement_temperature    100
_cell_measurement_theta_max      33.0986
_cell_measurement_theta_min      2.6513
_cell_volume                     3626.7(10)
_computing_cell_refinement       'DENZO (Bruker AXS, 2006)'
_computing_data_collection       'DATCOL (Bruker AXS, 2006)'
_computing_data_reduction        'DENZO (Bruker AXS, 2006)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 18.02
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker AXS Enraf-Nonius KappaCCD'
_diffrn_measurement_method       'CCD \f- and \w-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         '0.2 x 2mm^2^ focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0853
_diffrn_reflns_av_sigmaI/netI    0.0899
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            57688
_diffrn_reflns_theta_full        32.50
_diffrn_reflns_theta_max         32.50
_diffrn_reflns_theta_min         2.66
_exptl_absorpt_coefficient_mu    1.573
_exptl_absorpt_correction_T_max  0.69878
_exptl_absorpt_correction_T_min  0.38039
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2008)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_description       prism
_exptl_crystal_F_000             1444
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.12
_refine_diff_density_max         5.031
_refine_diff_density_min         -6.384
_refine_diff_density_rms         0.196
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     834
_refine_ls_number_reflns         25624
_refine_ls_number_restraints     100
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0651
_refine_ls_shift/su_max          0.035
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0948P)^2^+8.1901P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1618
_refine_ls_wR_factor_ref         0.1757
_reflns_number_gt                21855
_reflns_number_total             25624
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302799s_si_002.cif
_cod_data_source_block           '[Na(thf)5]Ta(tbpy)3'
_cod_original_cell_volume        3626.7(9)
_cod_database_code               4333952