First isolation of fully delocalized mixed-valent imido-bridged [Ti2]7+ complexes by one-electron reduction of [(C5R5)TiCl]2(m-NAr)2
Hayato Tsurugi; Haruki Nagae; Kazushi Mashima; Chem.Commun. 47 (2011) 5620–; doi:10.1039/c1cc10757g

data_7106368
_publ_section_title
;
 First isolation of fully delocalized mixed-valent imido-bridged [Ti2]7+
 complexes by one-electron reduction of [(C5R5)TiCl]2(m-NAr)2
;
_journal_name_full               Chem.Commun.
_journal_page_first              5620
_journal_paper_doi               10.1039/c1cc10757g
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety
'C26 H16 Cl2 F12 N2 Ti2, C10 H10 Co, 2(C1 H2 Cl2)'
_chemical_formula_sum            'C38 H30 Cl6 Co F12 N2 Ti2'
_chemical_formula_weight         1110.07
_chemical_name_common            5a
_chemical_name_systematic
;
?
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.064(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.139(12)
_cell_length_b                   11.696(7)
_cell_length_c                   21.035(14)
_cell_measurement_reflns_used    7677
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.04
_cell_volume                     4456(5)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    ORTEP-III
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'Il Milione (Burla, et al., 2007)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0867
_diffrn_reflns_av_sigmaI/netI    0.0754
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            41425
_diffrn_reflns_theta_full        27.43
_diffrn_reflns_theta_max         27.43
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    1.159
_exptl_absorpt_correction_T_max  0.7604
_exptl_absorpt_correction_T_min  0.5480
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.655
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2212
_exptl_crystal_size_max          0.59
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.593
_refine_diff_density_min         -0.785
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         10099
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.1462
_refine_ls_R_factor_gt           0.0964
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1489P)^2^+9.0337P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2514
_refine_ls_wR_factor_ref         0.2932
_reflns_number_gt                6253
_reflns_number_total             10099
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc10757g.txt
_cod_data_source_block           shelxl
_cod_database_code               7106368