Tin( ii ) ketoacidoximates: synthesis, X-ray structures and processing to tin( ii ) oxide
KAUST DepartmentPhysical Sciences and Engineering (PSE) Division
KAUST Grant NumberBAS/1/1302-01-01
Permanent link to this recordhttp://hdl.handle.net/10754/622361
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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)
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