Issue 46, 2015

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

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

Article type
Paper
Submitted
11 Aug 2015
Accepted
21 Oct 2015
First published
21 Oct 2015

Dalton Trans., 2015,44, 19820-19828

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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