Volume 25, Issue 32
Preparative Inorganic Chemistry
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ChemInform Abstract: Hydrothermal Synthesis of a New Molybdate with a Layered Structure, ( NMe4)Mo4-δO12.

J. GUO

J. GUO

Dep. Chem., State Univ. N. Y., Binghamton, NY 13902-6000, USA

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P. ZAVALIJ

P. ZAVALIJ

Dep. Chem., State Univ. N. Y., Binghamton, NY 13902-6000, USA

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M. S. WHITTINGHAM

M. S. WHITTINGHAM

Dep. Chem., State Univ. N. Y., Binghamton, NY 13902-6000, USA

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First published: August 9, 1994

Abstract

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ChemInform Abstract

Dark brown microcrystallites of the title compound of bright metallic luster are prepared in 60% yield based on Mo by acidifying a mixture of H2MoO4 and 25% Me4NOH (TMA) (1:2 molar Mo:TMA ratio) with 3 M HCl to pH 3-4 and reacting the resultant gel hydrothermally in an autoclave at 200 °C and autogenous pressure. As shown by powder XRD and supported by SEM images, the crystallites have a layered structure of a new MoO6 octahedra arrangement. Layers of Mo4O16 units sharing corners and edges are stacked along the 001 direction and are separated by NMe+ 4 cations. The pattern is indexed with monoclinic symmetry. Systematic extinction suggest a space group C2/m.

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