Preparation and Characterization of New Ruthenium and Osmium Containing Polyoxometalates, [M(DMSO)3Mo7O24]4- (M = Ru(II), Os(II)), and Their Use as Catalysts for the Aerobic Oxidation of Alcohols
Alexander M. Khenkin; Linda J. W. Shimon; Ronny Neumann; Inorganic Chemistry 42 (2003) 3331–3339; doi:10.1021/ic026003p

data_4313625
_publ_section_title
;
 Preparation and Characterization of New Ruthenium and Osmium Containing
 Polyoxometalates, [M(DMSO)3Mo7O24]4- (M = Ru(II), Os(II)), and Their Use
 as Catalysts for the Aerobic Oxidation of Alcohols
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3331
_journal_page_last               3339
_journal_paper_doi               10.1021/ic026003p
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C6 H18 Mo7 N4 O33.5 Ru S3'
_chemical_formula_weight         1551.07
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 124.23(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   36.310(7)
_cell_length_b                   12.239(2)
_cell_length_c                   22.379(5)
_cell_measurement_temperature    293(2)
_cell_volume                     8223(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0465
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            11426
_diffrn_reflns_theta_full        23.82
_diffrn_reflns_theta_max         23.82
_diffrn_reflns_theta_min         3.12
_exptl_absorpt_coefficient_mu    2.674
_exptl_crystal_density_diffrn    2.506
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5888
_refine_diff_density_max         4.806
_refine_diff_density_min         -1.445
_refine_diff_density_rms         0.262
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         6208
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0572
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0472P)^2^+597.3041P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1429
_refine_ls_wR_factor_ref         0.1461
_reflns_number_gt                5578
_reflns_number_total             6208
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic026003psi20021219_041731.cif
_cod_data_source_block           22
_cod_original_cell_volume        8223(3)
_cod_original_formula_sum        'C6 H18 Mo7 N4 O33.50 Ru S3'
_cod_database_code               4313625