HIGH-YIELD SYNTHESIS OF MIXED-METAL KEGGIN POLYOXOANIONS IN NONAQUEOUS SOLVENTS - PREPARATION OF (N-BU(4)N)(4)[PMW(11)O(40)] (M=V, NB, TA)

被引：72
作者：
RADKOV, E [1 ]
BEER, RH [1 ]
机构：
[1] COLUMBIA UNIV,DEPT CHEM,NEW YORK,NY 10027
来源：
POLYHEDRON | 1995年 / 14卷 / 15-16期
关键词：
D O I：
10.1016/0277-5387(95)00026-O
中图分类号：
O61 [无机化学];
学科分类号：
070301 ; 081704 ;
摘要：
The synthesis of (n-Bu(4)N)(4)[PMW(11)O(40)] (M = V, Nb, Ta) in non-aqueous solvents is described using the lacunary compound (n-Bu(4)N)(4)H-3[PW11O39] and commercially available VOCl3, NbCl5 and TaCl5. The yield and purity of the product vary depending on the solvent and the presence of base. W-183 NMR Spectroscopy of the title compounds reveal six resonances in the ratio 2:2:2:1:2:2 (M = Nb, Ta) consistent with their formulation as monosubstituted tungstophosphates with the Keggin structure. Their FAB mass spectra display protonated molecular ions in the positive ion mode and monoanionic fragments MO(x) and MW(n)O(x)(n greater than or equal to 1, x greater than or equal to n) (M = Nb, Ta) in the negative ion mode.
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页码：2139 / 2143
页数：5
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