A. Singhal, D. Dutta, A. K. Tyagi
Nov 1, 2007
Citations
0
Influential Citations
27
Citations
Journal
Journal of Organometallic Chemistry
Abstract
In an effort to find simple and common single-source precursors for palladium sulfide nanostructures, palladium(II) complexes, [Pd(S 2 X) 2 ] (X = COMe ( 1 ), CO i Pr ( 2 )) and η 3 -allylpalladium complexes with xanthate ligands, [(η 3 -CH 2 C(CH 3 )CR 2 )Pd(S 2 X)] (R = H, X = COMe ( 3 ); R = H, X = COEt ( 4 ); R = H, X = CO i Pr ( 5 ); R = CH 3 , X = COMe ( 6 )), have been investigated. The crystal structures of [Pd(S 2 X) 2 ] (X = COMe ( 1 ), Co i Pr ( 2 )) and [(η 3 -CH 2 C(CH 3 )CH 2 )Pd(S 2 COMe)] ( 3 ) have been established by single crystal X-ray diffraction analysis. The complexes, 1 , 2 and 3 all contain a square planar palladium(II) centre. In the allyl complex 3 , this is defined by the two sulfurs of the xanthate and the outer carbons of the 2-methylallyl ligand, while in the complexes, 1 and 2 it is defined by the four sulfur atoms of the xanthate ligand. Thermogravimetric studies have been carried out to evaluate the thermal stability of η 3 -allylpalladium(II) analogues. The complexes are useful precursors for the growth of nanocrystals of PdS either by furnace decomposition or solvothermolysis in dioctyl ether. The solvothermal decomposition of complexes in dioctyl ether gives a new metastable phase of PdS which can be transformed to the more stable tetragonal phase at 320 °C. The nanocrystals obtained have been characterized by PXRD, SEM, TEM and EDX.