Crystal structure and spectral characterization of hexanuclear oxo titanium(IV) clusters: [Ti6O6(OSi(CH3)3)6(OOCR)6] (R = But, CH2But, C(CH3)2Et)

Hexanuclear oxo titanium(IV) siloxo carboxylate complexes with the general formula [Ti6O6(OSi(CH3)3)6(OOCR)6] (R = But (1), CH2But (2), C(CH3)2Et (3)) were synthesized in quantitative yield, by the reaction of Ti(OSiMe3)4 with the appropriate organic acid. Crystal structure determination revealed that molecules of 1–3 are composed of [Ti6-(μ3-O)6] cores stabilized by six syn–syn carboxylato bridges and six terminal siloxide ligands. Each metal atom is surrounded by six oxo atoms, capping the triangular faces of the distorted octahedron. Spectral characterization (IR, NMR) of 1–3 revealed a significant non-equivalence of the carboxylate group interactions, resulting from the asymmetry of the Ti-μ-OOC bonds of the syn–syn bridges. The thermal stability of the studied compounds was determined from TGA/DTA analysis.

Graphical abstractHexanuclear oxo titanium(IV) siloxo carboxylate complexes with the general formula [Ti6O6(OSi(CH3)3)6(OOCR)6] (R = But (1), CH2But (2), C(CH3)2Et (3)) were synthesized in quantitative yield, by the reaction of Ti(OSiMe3)4 with the appropriate organic acid. Crystal structure determination revealed that molecules of 1–3 are composed of [Ti6-(μ3-O)6] cores stabilized by six syn–syn carboxylato bridges and six terminal siloxide ligands. Each metal atom is surrounded by six oxo atoms, capping the triangular faces of the distorted octahedron. Spectral characterization (IR, NMR) of 1–3 revealed a significant non-equivalence of the carboxylate group interactions, resulting from the asymmetry of the Ti-μ-OOC bonds of the syn–syn bridges. The thermal stability of the studied compounds was determined from TGA/DTA analysis.Figure optionsDownload full-size imageDownload as PowerPoint slide