Synthesis, characterisation and thermal decomposition of tin(IV) dithiocarbamate derivatives – single source precursors for tin sulfide powders

• Published in: Polyhedron Vol. 23; no. 12; pp. 2103 - 2109
• Main Authors: Menezes, D.C., de Lima, G.M., Porto, A.O., Donnici, C.L., Ardisson, J.D., Doriguetto, A.C., Ellena, J.
• Format: Journal Article
• Language: English
• Published: OXFORD Elsevier Ltd 29.07.2004; Elsevier
• Subjects: Chemistry; Chemistry, Inorganic & Nuclear; Crystallography; Organotin derivatives; Physical Sciences; Pyrolysis; Science & Technology; Tin sulfide; Pyrolysis; Tin sulfide; Organotin derivatives; organotin derivatives; pyrolysis; C-13; tin sulfide; SN-119 NMR-SPECTRA
• ISSN: 0277-5387; 1873-3719
• DOI: 10.1016/j.poly.2004.06.007

The reaction of ammonium pyrrolidinedithiocarbamate with SnPh 2Cl 2 and SnPh 3Cl produced in good yield the compounds [Sn{S 2CN(CH 2) 4} 2{C 6H 5} 2] · toluene ( 1) and Sn{S 2CN(CH 2) 4}{C 6H 5} 3 ( 2). They were fully characterised by multinuclear NMR [ 1H, 13C{ 1H} and 119Sn{ 1H}] and 119Sn Mössbauer spectroscopies. The reaction of ammonium pyrrolidinedithiocarbamate with SnPh 2Cl 2 and SnPh 3Cl produced in good yield the compounds [Sn{S 2CN(CH 2) 4} 2{C 6H 5} 2] · toluene ( 1) and Sn{S 2CN(CH 2) 4}{C 6H 5} 3 ( 2). They were fully characterised by multinuclear NMR [ 1H, 13C{ 1H} and 119Sn{ 1H}] and 119Sn Mössbauer spectroscopies. In addition the structure of 1 was determined, and 2 was revised by X-ray crystallographic studies. Finally, thermal decomposition experiments were carried out for both compounds in nitrogen and the residues were characterised by X-ray powder diffraction (XRD), X-ray electron probe microanalysis (EPMA), scanning electron microscopy (SEM) and 119Sn Mössbauer spectroscopy. The results clearly indicate the formation of a mixture of γ-Sn 2S 3 and SnS, both orthorhombic phases.