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PubMed1996

Synthesis, Structural Characterization, and Oxidation-Reduction Behavior of the gamma-Isomer of the Dodecatungstosilicate Anion.

The reaction of tungstate ions with the gamma-10-tungstosilicate in mixed water-ethanol (v/v) yields the corresponding isomer of the 12-tungstosilicate isolated as its tetrabutylammonium salt. It was characterized by means of (183)W NMR, infrared, Raman, and UV spectroscopies and was identified with the isomer resulting from the Keggin structure (alpha-isomer) by rotation of two tritungstic groups by pi/3. Cyclic voltammetry shows that the reducibility increases in the sequence alpha-beta-gamma as the number of rotated tritungstic groups. Whereas the gamma-12-tungstosilicate anion is unstable in pure aqueous solution whatever the pH value, it is stable in mixed aqueous-organic or pure organic solvents, even at boiling temperatures. In contrast, the two- and four-electron-reduced blue species are stable in aqueous media but not the one-electron-reduced blue. Study of the (183)W NMR spectrum of the two-electron-reduced species showed that the two spin-paired electrons are delocalized on all the W atoms on the NMR time scale but have a larger residency time on one group of four atoms.

Journal Article↗
PubMed2002

Hydrothermal oxidation-reduction methods for the preparation of pure and single crystalline alunites: synthesis and characterization of a new series of vanadium jarosites.

Three new redox-based, hydrothermal, synthetic methods have been developed for the preparation of a new series of jarosites, AV(3)(OH)(6)(SO(4))(2) (A = Na(+), K(+), Rb(+), Tl(+), and NH(4)(+)), in high purity and in single crystalline form. The V(3+) jarosites have been characterized by single-crystal X-ray and elemental analysis, and by infrared and electronic absorption spectroscopy. The synthetic methods employed here represent a new approach for the preparation of the jarosite class of compounds, which for the past several decades, have been notoriously difficult to prepare in pure form. To demonstrate the impact of our new synthetic techniques on the magnetic properties of jarosites, the V(3+) jarosites were also prepared according to the nonredox techniques used over the past 30 years. A comparative study of these samples and those prepared by our new synthetic methods reveals widely divergent magnetic properties, thus pointing to the importance of the new redox synthetic methods to future magnetism studies of jarosite compounds.

Journal Article↗