Tin( ii ) ketoacidoximates: synthesis, X-ray structures and processing to tin( ii ) oxide
KAUST DepartmentPhysical Sciences and Engineering (PSE) Division
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AbstractTin(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.
CitationKhanderi J, Davaasuren B, Alshankiti BA, Rothenberger A (2015) Tin( ii ) ketoacidoximates: synthesis, X-ray structures and processing to tin( ii ) oxide . Dalton Trans 44: 19820–19828. Available: http://dx.doi.org/10.1039/c5dt03103f.
SponsorsThis 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.
PublisherRoyal Society of Chemistry (RSC)
Is Supplemented ByKhanderi, J., Davaasuren, B., Alshankiti, B. A., & Rothenberger, A. (2015). CCDC 1048728: Experimental Crystal Structure Determination [Data set]. Cambridge Crystallographic Data Centre. https://doi.org/10.5517/cc1468yk
Khanderi, J., Davaasuren, B., Alshankiti, B. A., & Rothenberger, A. (2015). CCDC 1048729: Experimental Crystal Structure Determination [Data set]. Cambridge Crystallographic Data Centre. https://doi.org/10.5517/cc1468zl
Khanderi, J., Davaasuren, B., Alshankiti, B. A., & Rothenberger, A. (2015). CCDC 1048727: Experimental Crystal Structure Determination [Data set]. Cambridge Crystallographic Data Centre. https://doi.org/10.5517/cc1468xj
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