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Homometallic glycolates containing hydroxyl functionality for anchoring another metal: synthesis and characterization of heterometallic alkoxideglycolates of Ti and Zr incorporating Al and Nb

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Reaction of Ti(OPr i )4 with 2-methyl-2,4-pentanediol [HOGOH, where G = CMe2CH2CH(Me)] in 1 : 3 M ratio under reflux afforded the monomeric [Ti(OGO)(OGOH)2] (1), which on further reactions with [Al(OPr i )3] or [Nb(OPr i )5] in 1 : 1 and 1 : 2 M ratios afforded heterometallic derivatives, [Ti(OGO)3{M(OPr i )n−2}] and [Ti(OGO)3{M(OPr i )n−1}2] [where M = Al (n = 3), Nb (n = 5)], respectively. Similar reactions of Zr(OPr i )4Pr i OH with a number of glycols [HOGOH, where G = CH(Me)CH(Me), CMe2CMe2, CMe2CH2CH(Me)] yielded dimeric [Zr2(OGO)2(OGOH)4]. [Zr2(OGO)6{M(OPr i )n−2}2] and [Zr2(OGO)4(OGOH)2M(OPr i )n−2] [M = Al (n = 3), Ti (n = 4), Nb (n = 5)] were prepared by 1 : 2 and 1 : 1 reactions, respectively, of [Zr2(OGO)2(OGOH)4] with Al(OPr i )3, Ti(OPr i )4, or Nb(OPr i )5. Surprisingly, a 1 : 2 reaction of [VO(OPr i )3] with 2,2-diethyl-1,3-propanediol in benzene followed a different reaction and produced a neutral tetranuclear derivative [V4(O)4(μ-OCH2CEt2CH2O)2(OCH2CEt2CH2O)4] (18). All of these derivatives were characterized by elemental analysis, molecular weight measurements, FT-IR, and 1H NMR (and wherever possible, by 27Al or 51V NMR) spectroscopic studies. The derivatives [Zr2(OCMe2CH2CH(Me)O)2(OCMe2CH2CH(Me)OH)4] (9 and 18) were additionally characterized by single-crystal X-ray structure analysis.
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Keywords: Metal glycolates; X-ray structure; alkoxides; heterometallics; precursors

Document Type: Research Article

Affiliations: 1: Department of Chemistry, University of Rajasthan, Jaipur, India 2: Centre de Diffractométrie Henri Longchambon, University of Lyon 1, Villeurbanne, France 3: IRCELYON, University of Lyon 1, Villeurbanne, France

Publication date: January 2, 2016

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