A new organometallic palladium(II) compound derived of 2,6-diacetylpyridine mono(thiosemicarbazone): Synthesis, spectroscopic properties and crystal structure of two solvatomorphic forms

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• 作者：Ana I. Matesanz ; Carolina Hern谩ndez ; Pilar Souza
• 关键词：Cyclopalladated ; 2 ; 6-Diacetylpyridine ; Solvatomorph ; Thiosemicarbazone ; X-ray
• 刊名：Journal of Organometallic Chemistry
• 出版年：1 February, 2014
• 年：2014
• 卷：751
• 期：Complete
• 页码：374-378
• 全文大小：575 K

文摘

Preparation and characterization of a novel 2,6-diacetylpyridine mono(4-methoxyphenyl-thiosemicarbazone), H₂L, is described. Treatment of H₂L with PdCl₂(PPh₃)₂ gave the neutral mononuclear complex [PdL(PPh₃)]. Both compounds have been characterized by elemental analysis and FAB⁺ spectrometry and by IR and ¹H NMR spectroscopy. Recrystallization of [PdL(PPh₃)] in DMSO led to the isolation of two solvatomorphic forms of this compound which were studied by X-ray crystallography. In each solvatomorph, the thiosemicarbazone ligand acts as dianionic [CNS] tridentate donor coordinating to the palladium(II) ion in a square planar geometry through the iminic nitrogen atom, the sulfur atom and one ortho carbon atom of the pyridine ring and the fourth site is occupied by P atom from the PPh₃ coligand. The overall molecular conformation of the two solvatomorphs is very similar and the largest difference lies in the orientation of the methyl group of the 4-methoxyphenyl substituent with respect to the sulfur atom.