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_7106364
_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         'C16 H17 Cl2 F6 N Si Ti'
_chemical_formula_sum            'C16 H17 Cl2 F6 N Si Ti'
_chemical_formula_weight         484.20
_chemical_name_common            3a
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 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                 110.026(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.519(6)
_cell_length_b                   23.699(15)
_cell_length_c                   10.892(7)
_cell_measurement_reflns_used    4144
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     2066(2)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_molecular_graphics    ORTEP-III
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  SHELXL
_computing_structure_solution    SHELXS97
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Rigaku Mercury'
_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  0.0484
_diffrn_reflns_av_sigmaI/netI    0.0421
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19168
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         3.07
_exptl_absorpt_coefficient_mu    0.784
_exptl_absorpt_correction_T_max  0.8464
_exptl_absorpt_correction_T_min  0.7445
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.036
_refine_diff_density_min         -0.896
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         4645
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_gt           0.0608
_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^)+(0.1235P)^2^+0.8152P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1735
_refine_ls_wR_factor_ref         0.2014
_reflns_number_gt                3572
_reflns_number_total             4645
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc10757g.txt
_cod_data_source_block           shelxl
_cod_database_code               7106364