Synthesis and Characterisation of Modified Germanium (IV) Isopropoxide with Internally Functionalised oximes: Soft Transformation of Some of These to Pure Nano-Sized Germania

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Reactions of [Ge(OPr i ) 4 ] with internally functionalised oximes in 1:1 and 1:2 molar ratios in refluxing anhydrous benzene yielded complexes of the type [Ge(OPr i ) 4- n {ONC(CH 3 )C 4 H 3 O-2} n ] (1, 2); [Ge(OPr i ) 4- n {ONC(CH 3 )C 4 H 3 S-2} n ] (3, 4); [Ge(OPr i ) 4- n {ONC(CH 3 )C 5 H 4 N-2} n ] (5, 6); [Ge(OPr i ) 4- n {ONC(H)C 4 H 3 O-2} n ] (7, 8); [Ge(OPr i ) 4- n {ONC(H)C 4 H 3 S-2} n ] (9, 10); [Ge(OPr i ) 4- n {ONC(H)C 5 H 4 N-2} n ] (11, 12) (where n = 1 or 2), All the above monomeric complexes are soluble in organic solvents and have been characterised by elemental analyses and spectroscopy. Thermal and hydrolytic studies of complexes 2, 4 and 8 suggest them to be potential molecular precursors for the synthesis of pure GeO 2 at low temperatures by the sol-gel technique. Powder X-ray diffraction, IR spectral studies as well as SEM images of the GeO 2 indicate formation of pure nano-crystalline hexagonal (α-quartz) germania at 550°C.