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Synthetic studies and structural aspects of novel metallacyclic compoundsof titanium(IV) incorporating nitrogen, oxygen and sulphur: 1. Reactions of cis-dialkoxy-bis(acetylacetonato)titanium(IV) with alkoxyalkanols and the crystal structure of a new modification: di-μ-oxo-bis[diacetylacetonatotitanium(IV)]

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Abstract

Reactions of cis-dialkoxy-bis(acetylacetonato)titanium(IV), [(acac)2Ti(OR)2] (R = Et, Pri) with alkoxyalkanols (R′OCH2CH2OH) (R′ = Me, Et, n-Bu) in 1:1 and 1:2 molar ratios in refluxing benzene under anhydrous conditions yield [(acac)2Ti(OR)2−n (OCH2CH2OR′) n ] (n = 1 or 2) complexes, which were purified by distillation under reduced pressure. On the basis of i.r. and n.m.r. (1H- and 13C-) spectral studies, a cis-octahedral environment around TiIV is proposed. On keeping the distilled dark brown-red viscous liquid [(acac)2Ti(OEt)(OCH2CH2OBu)] for 2 weeks, orange yellow crystals of [(acac)2TiO]2 were obtained. A single crystal X-ray diffraction study suggests the product is a new modification of [(acac)2TiO]2.

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Pathak, M., Bohra, R., Mehrotra, R.C. et al. Synthetic studies and structural aspects of novel metallacyclic compoundsof titanium(IV) incorporating nitrogen, oxygen and sulphur: 1. Reactions of cis-dialkoxy-bis(acetylacetonato)titanium(IV) with alkoxyalkanols and the crystal structure of a new modification: di-μ-oxo-bis[diacetylacetonatotitanium(IV)]. Transition Metal Chemistry 28, 187–192 (2003). https://doi.org/10.1023/A:1022901918955

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