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Formation of isopolyoxometallate(VI) anions in the reaction between M(CO)6 (M = W, Mo) and acetic acid: X-ray crystal structure of [W3(μ3-O)2(μ2η2-O2CCH3)6(H2O)3]2[W10O32·solvent

Madden, A., McCann, M., Ryan, H., Cardin, C. and Convery, M. (1993) Formation of isopolyoxometallate(VI) anions in the reaction between M(CO)6 (M = W, Mo) and acetic acid: X-ray crystal structure of [W3(μ3-O)2(μ2η2-O2CCH3)6(H2O)3]2[W10O32·solvent. Polyhedron, 12 (5). pp. 473-477. ISSN 0277-5387

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To link to this item DOI: 10.1016/S0277-5387(00)83396-3

Abstract/Summary

W(CO)6 reacts with a mixture of acetic acid/acetic anhydride to give [W3 (μ3-O)2(μ2η2-O2CCH3)6(H2O)3](CH3CO2)2 (1), which was converted by HClO4 to [W3 (μ3-O)2(μ2η2-O2CCH3)6(H2O)3](ClO4)2 (2). Addition of CH3CO2Na to the above reaction mixture, and prolonged exposure of the solution to air, results in the formation of the WIV/WVI complex salt [W3(μ3-O)2(μ2η2-O2CCH3)6(H2O)3]2[W10O32]·solvent (3). Complex 3 was also prepared by reacting 1 with Na2WO4·2H2O in acetic acid, and it has been characterized by X-ray crystallography. Addition of [CH3(CH2)3]4N(ClO4) to the reaction filtrate remaining after the preparation of [Mo2(μ-O2CCH3)4][from Mo(CO)6, CH3CO2H and (CH3CO)2O], followed by exposure to air, gives ([CH3(CH2)3]4N)2[Mo6O19] (4).

Item Type:Article
Refereed:Yes
Divisions:Faculty of Science
ID Code:23803
Publisher:Elsevier

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