Tin( ii ) ketoacidoximates: synthesis, X-ray structures and processing to tin( ii ) oxide

Jayaprakash Khanderi, Bambar Davaasuren, Buthainah Alshankiti, Alexander Rothenberger

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Tin(ii) ketoacidoximates of the type [HONCRCOO]Sn (R = Me 1, CHPh 2) and (MeONCMeCOO)Sn] NH·2HO 3 were synthesized by reacting pyruvate- and hydroxyl- or methoxylamine RONH (R = H, Me) with tin(ii) chloride dihydrate SnCl·2HO. The single crystal X-ray structure reveals that the geometry at the Sn atom is trigonal bipyramidal in 1, 2 and trigonal pyramidal in 3. Inter- or intramolecular hydrogen bonding is observed in 1-3. Thermogravimetric (TG) analysis shows that the decomposition of 1-3 to SnO occurs at ca. 160 °C. The evolved gas analysis during TG indicates complete loss of the oximato ligand in one step for 1 whereas a small organic residue is additionally removed at temperatures >400 °C for 2. Above 140 °C, [HONC(Me)COO]Sn (1) decomposes in air to spherical SnO particles of size 10-500 nm. Spin coating of 1 on Si or a glass substrate followed by heating at 200 °C results in a uniform film of SnO. The band gap of the produced SnO film and nanomaterial was determined by diffuse reflectance spectroscopy to be in the range of 3.0-3.3 eV. X-ray photoelectron spectroscopy indicates surface oxidation of the SnO film to SnO in ambient atmosphere.
Original languageEnglish (US)
Pages (from-to)19820-19828
Number of pages9
JournalDalton Trans.
Issue number46
StatePublished - 2015

Bibliographical note

KAUST Repository Item: Exported on 2020-10-01
Acknowledged KAUST grant number(s): BAS/1/1302-01-01
Acknowledgements: This work was supported by the King Abdullah University of Science & Technology (KAUST) baseline (BAS/1/1302-01-01) and AEA funding. J. K. thanks Dr Rachid Sougrat and Ms Nini Wei for TEM imaging and Dr Mohamed Nejib Hedhili for XPS analysis.


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