Tuning of Redox Potentials by Introducing a Cyclometalated Bond to Bis-tridentate Ruthenium(II) Complexes Bearing Bis(N-methylbenzimidazolyl)benzene or -pyridine Ligands
Wen-Wen Yang; Yu-Wu Zhong; Shinpei Yoshikawa; Jiang-Yang Shao; Shigeyuki Masaoka; Ken Sakai; Jiannian Yao; Masa-aki Haga; Inorganic Chemistry 51 (2012) 890–899; doi:10.1021/ic2016885

data_4327974
_publ_contact_author_address
;
    Department of Applied Chemistry
    Faculty of Science and Engineering
    Chuo University
    1-13-27 Kasuga, Bunkyo-ku
    Tokyo 112-8551, Japan
;
_publ_contact_author_email       mhaga@chem.chuo-u.ac.jp
_publ_contact_author_fax         '81 3 3817 1908'
_publ_contact_author_name        'Prof. Masa-aki Haga'
_publ_contact_author_phone       '81 3 3817 1908'
_publ_section_title
;
 Tuning of Redox Potentials by Introducing a Cyclometalated Bond to
 Bis-tridentate Ruthenium(II) Complexes Bearing
 Bis(N-methylbenzimidazolyl)benzene or -pyridine Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              890
_journal_page_last               899
_journal_paper_doi               10.1021/ic2016885
_journal_volume                  51
_journal_year                    2012
_chemical_formula_iupac          'C65 H55 B N8 Ru'
_chemical_formula_moiety         'C39 H32 N7 Ru, C24 H20 B, C2 H3 N'
_chemical_formula_sum            'C65 H55 B N8 Ru'
_chemical_formula_weight         1060.05
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2010/03/02
_audit_creation_method
'from SHELXL97 and KenX, based on form.cif supplied from IUCr'
_audit_update_record
;
2010-05-12 Manually Edited
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.0541(19)
_cell_length_b                   14.2024(15)
_cell_length_c                   20.996(2)
_cell_measurement_reflns_used    6142
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.70
_cell_measurement_theta_min      2.39
_cell_volume                     5085.4(9)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'KENX (Sakai, 2002)'
_computing_publication_material
;
SHELXL97, TEXSAN (Molecular Structure Corporation, 2001), 
KENX, and ORTEP (Johnson, 1976)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device
'Bruker SMART APEX CCD-detector diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0499
_diffrn_reflns_av_sigmaI/netI    0.0733
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            26023
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    0.361
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_correction_T_min  0.837
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, G. M., 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_description       needle
_exptl_crystal_F_000             2200
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.579
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details 'Flack (1983), 2899 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.05(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     681
_refine_ls_number_reflns         9932
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0383
_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^)+(0.0298P)^2^+0.9259P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0690
_refine_ls_wR_factor_ref         0.0771
_reflns_number_gt                7677
_reflns_number_total             9932
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2016885_si_002.cif
_cod_data_source_block           tacn
_cod_original_cell_volume        5085.5(10)
_cod_original_sg_symbol_Hall     'P 2c -2ac '
_cod_database_code               4327974