摘 要: | The single crystal of two-electron heteropoly blue with Si as the heteroatom and α-Keggin structure K_2H_4SiMo(Ⅴ)_2Mo(Ⅵ)_(10)O_(40)·12H_2O was obtained by electrolytic reduction. It crystallizes in a triclinic system with space group P , Mr=2117.73, a= 13.702(4), b=14.107(3), c=14.184(2) ; α=119.27(1), β=93.14(2), ;γ=110. 3(2)°, V=2154.29~3, Z=2, F(000)=1999, μ=36.39cm~(-1), Dc=3.26 g/cm~3. Final R factor is 0.0515. Mo(Ⅴ) is situated in two different edge-shared Mo_3O_(13) groups. The heteropoly blue was characterized by IR, UV, polarography, X-ray photoelectron spectra and ESR. All the results show that the structure of the heteropoly anion with Keggin structure remains unchanged basically in the process of reduction.
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