Tantalum(v) oxoalkoxides. Synthesis and structure |
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Authors: | A. I. Yanovsky N. Ya. Turova A. V. Korolev D. E. Chebukov A. P. Pisarevsky Yu. T. Struchkova |
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Affiliation: | (1) A. N. Nesmeyanov Institute of Otganoelement Compounds, Russian Academy of Sciences, 28 ul. Vavilova, 117813 Moscow, Russian Federation;(2) Department of Chemistry, M. V. Lomonosov Moscow State University, Vorob'evy Gory, 119899 Moscow, Russian Federation |
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Abstract: | Anodic oxidation of tantalum in isopropyl alcohol or prolonged reflux of an alcohol solution of Ta(OPri)5 afford crystalline oxoisopropoxide Ta2O(OPri)8 · PriOH (1). In its molecule, two octahedra about Ta atoms are linkedvia the shared edge [(OPri)O]. Compound1 is the first example of oxoalkoxide containing such a small number of metal atoms. Unlike the known polynuclear molecules MnOm(OR)p, oxoalkoxide1 is stable in solutions; on transition to the gas phase, this compound is desolvated to form a very stable molecule Ta2O(OPri)8 (apparently, consisting of two octahedra with a shared edge). According to the data of mass spectrometry, analogous molecules exist in the gas phase over Ta(OAlk)5 (Alk = Me, Et, Pri, or Bu11). When compound1 is heated invacuo (10–2–10–3 Torr), Ta(OPri)5 is sublimated. Crystals of Ta7O9(OPri)17 (2) were formed upon prolonged storage of solutions of1 in PriOH. Heptanuclear molecule2 consists of two [Ta4] tetrahedra with a shared vertex. These tetrahedra are additionally linked togethervia one 3-oxo and two 2-OPri groups. Complex2 is a representative of heptameric oxoalkoxides of a new structural type.Deceased in I995.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 1, pp. 125–131, January, 1996. |
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Keywords: | tantalum oxoalkoxides, electrochemical synthesis, X-ray structural analysis mass spectrometry |
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