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Synthesis and Structural Characterization of ... - Jacobs University

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Chapter 5<br />

Published Results<br />

polymolybdates. Hence, 26 combines three important features previously unknown for<br />

tungstotellurate anions. First, the structure involves face-shared WO 6 octahedra; second, the<br />

{W 10 } unit coordinated to tellurium(IV) atoms is novel; <strong>and</strong> third, the tellurium atoms adopt a<br />

see-saw configuration.<br />

Another novel tungstotellurate(IV), [NaTeW 15 O 54 ] 13−<br />

(27), is present in a mixture <strong>of</strong><br />

products if the synthesis solution <strong>of</strong> 26 is heated. Single-crystal X-ray diffraction analysis<br />

revealed that [NaTeW 15 O 54 ]·26H 2 O (Na-27) crystallizes in the orthorhombic space group<br />

Pccn. Polyanion 27 is composed <strong>of</strong> a triangular assembly <strong>of</strong> 15 edge- <strong>and</strong> corner-shared WO 6<br />

octahedra, surrounding a trigonal-pyramidal tellurium(IV) center located in the central cavity<br />

<strong>and</strong> a capping sodium ion (Figure 5.5). The tellurium <strong>and</strong> the sodium atom, both closely<br />

associated with the polyanion, are disoredered showing 50 % occupancy for each. Polyanion<br />

27 is composed <strong>of</strong> three identical {W 5 } building-blocks which are made up <strong>of</strong> five WO 6<br />

octahedra.<br />

Figure 5.5. Ball-<strong>and</strong>-stick representations <strong>of</strong> [NaTeW 15 O 54 ] 13− (27). The color code is as the<br />

same as Figure 5.2.<br />

176

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