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The synthesis and the structural characterization of the title compound H_2Na_3[W_3O(CCH_3)-(O_2CCH_3)_6(H_2O)_3][H_2W_(12)O_(40)]·13.5 H_2O are described.It is known that the mixed oxo-ethylidyne-capped tritungsten cluster can be obtained by Zn dust reduction of Na_2WO_4·2H_2O in acetic anhydride.The title compound has been characterized by X-ray diffraction,UV/VIS and ~1H NMR spectra.The tungsten atoms in the cluster cation and anion are in the oxidation states of W(IV)and W(VI)respectively.The crystal is rhombohedral with the space group R32,a=17.058(3),c=49.665(9),γ=120°,V=12516(9)~3,Z=6,final R=0.037 for 2071 reflections with I≥3σ(I).Boththe cluster cation and anion have a C_3 symmetry.The important interatomic distances in angstroms forthe cluster cation are:W—W,2.730(2);W—μ_3-O,2.00;W—O(carboxyl),2.12;W—O_t,2.18(2).
The synthesis and the structural characterization of the title compound H_2Na_3 [W_3O (CCH_3) - (O_2CCH_3) _6 (H_2O) _3] [H_2W_ (12) O_ (40)] · 13.5 H_2O are described. It is known that the mixed oxo- ethylidyne-capped tritium cluster can be obtained by Zn dust reduction of Na_2WO_4 · 2H_2O in acetic anhydride. The title compound has been characterized by X-ray diffraction, UV / VIS and ~ 1H NMR spectra.The tungsten atoms in the cluster cation and anion are in the oxidation states of W (IV) and W (VI). The crystal is rhombohedral with the space group R32, a = 17.058 (3), c = 49.665 (9), γ = 120 °, V = 12516 9) ~ 3, Z = 6, final R = 0.037 for 2071 reflections with I≥3σ (I) .Boththe cluster cation and anion have a C_3 symmetry.The important interatomic distances in angstroms forthe cluster cation are: W-W, 2.730 (2); W-μ_3-O, 2.00; W-O (carboxyl), 2.12; W-O_t, 2.18 (2).