Synthetic studies and structural aspects of novel metallacyclic compounds of titanium (IV) incorporating nitrogen, oxygen and sulphur: 1. Reactions of cis-dialkoxy-bis(acetylacetonato)titanium(IV) with alkoxyalkanols and the crystal structure of a ne

摘要

Reactions of cis-dialkoxy-bis(acetylacetonato)titanium(IV), [(acac)_2Ti(OR)_2] (R = Et, Pr~i) with alkoxyalkanols (R'OCH_2CH_2OH) (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)(OCH_2CH_2OR')_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 ~(13)C) spectral studies, a cis-octahedralenvironment around Ti~(IV) is proposed. On keeping the distilled dark brown-red viscous liquid [(acac)_2Ti(OEt)(OCH_2CH_2OBu)] 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.