Molecular and Electronic Structures of Mononuclear and Dinuclear Titanium Complexes Containing π-Radical Anions of 2,2'-Bipyridine and 1,10-Phenanthroline: An Experimental and DFT Computational Study.
Wolff, Carina; Gottschlich, Andreas; England, Jason; Wieghardt, Karl; Saak, Wolfgang; Haase, Detlev; Beckhaus, Rüdiger; Inorganic chemistry 54 (2015) 4811–4820; doi:10.1021/acs.inorgchem.5b00285

data_4342976
_publ_section_title
;
 Molecular and Electronic Structures of Mononuclear and Dinuclear Titanium
 Complexes Containing \p-Radical Anions of 2,2'-Bipyridine and
 1,10-Phenanthroline: An Experimental and DFT Computational Study.
;
_journal_issue                   10
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4811
_journal_page_last               4820
_journal_paper_doi               10.1021/acs.inorgchem.5b00285
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'C46 H60 Cl2 N4 Ti2'
_chemical_formula_weight         835.68
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   31.7878(13)
_cell_length_b                   44.898(3)
_cell_length_c                   12.0946(6)
_cell_measurement_temperature    153(2)
_cell_volume                     17261.5(16)
_computing_cell_refinement       'IPDS (Stoe, 1999)'
_computing_data_collection       'IPDS (Stoe, 1999)'
_computing_data_reduction        'XRED (S toe, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELX-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0541
_diffrn_reflns_av_sigmaI/netI    0.0609
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       55
_diffrn_reflns_limit_k_min       -55
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            41174
_diffrn_reflns_theta_full        26.13
_diffrn_reflns_theta_max         26.13
_diffrn_reflns_theta_min         2.60
_exptl_absorpt_coefficient_mu    0.530
_exptl_absorpt_correction_T_max  0.7811
_exptl_absorpt_correction_T_min  0.7415
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             7072
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.49
_refine_diff_density_max         0.484
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.193(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.873
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         8445
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      0.872
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0295
_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^)+(0.0326P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0615
_refine_ls_wR_factor_ref         0.0631
_reflns_number_gt                6747
_reflns_number_total             8445
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b00285_si_002.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 4342975--4342977.cif.'
_cod_original_cell_volume        17261.4(15)
_cod_original_sg_symbol_H-M      Fdd2
_cod_database_code               4342976