Abstract
Two novel examples of “sandwich” type heteropolyanions were synthesized and characterized by X-ray crystal structure and elemental analysis as well as infrared spectroscopy. Na13[H3Cu4(H2O)2(CuW9O34)2]⋅39H2O (1) and Na9K[Fe4(H2O)2(FeW9O34)2]⋅32H2O (2) were prepared in aqueous solution by reaction of sodium tungstate with FeIII and CuII cations, respectively. 1 crystallizes in the monoclinic space group P21/n (a=13.054(3) A, b=17.729(4) A, c=20.998(4) A, β=93.50(3)°), while 2 is triclinic, space group P¯1 (a=12.316(2) A, b=13.716(3) A, c=14.925(3) A, α=99.36(3)°, β=104.21(3)°, γ=101.55(3)°). Each anion consists of two [XW9O34] n− moieties (X=FeIII, n=11 (1) and CuII, n=12 (2)) which can be described as α-B-isomers of the defect Keggin anion. These units are linked via a belt of four FeIIIO6 or CuIIO6 groups. Two transition metal atoms fill their octahedral coordination sphere with one additional water ligand.
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