Preparation of tetrabutylammonium salt of a mono-Ru(III)-substituted α-Keggin-type silicotungstate with a 4,4'-bipyridine ligand and its electrochemical behaviour in organic solvents.
Ogo, Shuhei; Moroi, Sachie; Ueda, Tadaharu; Komaguchi, Kenji; Hayakawa, Shinjiro; Ide, Yusuke; Sano, Tsuneji; Sadakane, Masahiro; Dalton transactions (Cambridge, England : 2003) 42 (2013) 7190–7195; doi:10.1039/c3dt50300c

data_7022927
_publ_section_title
;
 Preparation of tetrabutylammonium salt of a mono-Ru(III)-substituted
 \a-Keggin-type silicotungstate with a 4,4'-bipyridine ligand and its
 electrochemical behaviour in organic solvents.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7190
_journal_page_last               7195
_journal_paper_doi               10.1039/c3dt50300c
_journal_volume                  42
_journal_year                    2013
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C194 H16 N21 O78 Ru2 Si2 W22'
_chemical_formula_sum            'C194 H16 N21 O78 Ru2 Si2 W22'
_chemical_formula_weight         8191.37
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                89.680(6)
_cell_angle_beta                 70.539(5)
_cell_angle_gamma                70.719(5)
_cell_formula_units_Z            2
_cell_length_a                   20.3725(4)
_cell_length_b                   27.4946(5)
_cell_length_c                   28.3758(6)
_cell_measurement_reflns_used    154140
_cell_measurement_temperature    93
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      3.00
_cell_volume                     14047.9(9)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID II'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            64221
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.155
_exptl_absorpt_correction_T_max  0.633
_exptl_absorpt_correction_T_min  0.243
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.936
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             7390.00
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.050
_refine_diff_density_max         9.430
_refine_diff_density_min         -3.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     2768
_refine_ls_number_reflns         64221
_refine_ls_number_restraints     3812
_refine_ls_R_factor_gt           0.0820
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1231P)^2^+408.5678P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2500
_reflns_number_gt                47924
_reflns_number_total             64221
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c3dt50300c.txt
_cod_data_source_block           SC1011
_cod_database_code               7022927