Selective oxidation and reduction of trinuclear titanium(II) hexaazatrinaphthylene complexes-synthesis, structure, and electrochemical investigations.
Piglosiewicz, Ingmar M.; Beckhaus, Rüdiger; Wittstock, Gunther; Saak, Wolfgang; Haase, Detlef; Inorganic chemistry 46 (2007) 7610–7620; doi:10.1021/ic701009u

data_4338902
_publ_section_title
;
 Selective oxidation and reduction of trinuclear titanium(II)
 hexaazatrinaphthylene complexes-synthesis, structure, and electrochemical
 investigations.
;
_journal_issue                   18
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7610
_journal_page_last               7620
_journal_paper_doi               10.1021/ic701009u
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C69 H72 B4 F16 N6 O3 Ti3'
_chemical_formula_weight         1524.27
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 92.708(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.8067(6)
_cell_length_b                   29.0762(11)
_cell_length_c                   19.5370(16)
_cell_measurement_temperature    153(2)
_cell_volume                     7266.9(7)
_computing_cell_refinement       'IPDS (Stoe, 1999)'
_computing_data_collection       'IPDS (Stoe, 1999)'
_computing_data_reduction        'XRED (Stoe, 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 0.943
_diffrn_measured_fraction_theta_max 0.943
_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  0.2438
_diffrn_reflns_av_sigmaI/netI    0.2886
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            60017
_diffrn_reflns_theta_full        26.20
_diffrn_reflns_theta_max         26.20
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    0.412
_exptl_absorpt_correction_T_max  0.9678
_exptl_absorpt_correction_T_min  0.9004
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'XRED (Stoe, 1997)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             3128
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.413
_refine_diff_density_min         -0.955
_refine_diff_density_rms         0.244
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.602
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         13759
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.603
_refine_ls_R_factor_all          0.3414
_refine_ls_R_factor_gt           0.2130
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4325
_refine_ls_wR_factor_ref         0.4656
_reflns_number_gt                4572
_reflns_number_total             13759
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701009u-file005.cif
_cod_data_source_block           IP380C
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4338902