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Issue 46, 2015

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

Author affiliations

Abstract

Tin(II) ketoacidoximates of the type [HON[double bond, length as m-dash]CRCOO]2Sn (R = Me 1, CH2Ph 2) and (MeON[double bond, length as m-dash]CMeCOO)3Sn] NH4+·2H2O 3 were synthesized by reacting pyruvate- and hydroxyl- or methoxylamine RONH2 (R = H, Me) with tin(II) chloride dihydrate SnCl2·2H2O. 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, [HON[double bond, length as m-dash]C(Me)COO]2Sn (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 SnO2 in ambient atmosphere.

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

Supplementary files

Article information


Submitted
11 Aug 2015
Accepted
21 Oct 2015
First published
21 Oct 2015

Dalton Trans., 2015,44, 19820-19828
Article type
Paper
Author version available

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

J. Khanderi, B. Davaasuren, B. A. Alshankiti and A. Rothenberger, Dalton Trans., 2015, 44, 19820 DOI: 10.1039/C5DT03103F

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