A One-Pot Self-Assembly Reaction To Prepare a Supramolecular Palladium(II) Cyclometalated Complex: An Undergraduate Organometallic Laboratory Experiment

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• 作者：Alberto Fern谩ndez ; Margarita L贸pez-Torres ; Jes煤s J. Fern谩ndez ; Digna V谩zquez-Garc铆a ; Jos茅 M. Vila
• 刊名：Journal of Chemical Education
• 出版年：2012
• 出版时间：January 1, 2012
• 年：2012
• 卷：89
• 期：1
• 页码：156-158
• 全文大小：695K
• 年卷期：v.89,no.1(January 1, 2012)
• ISSN：1938-1328

文摘

A laboratory experiment for students in advanced inorganic chemistry is described. Students prepare palladium(II) cyclometalated complexes. A terdentate [C,N,O] Schiff base ligand is doubly deprotonated upon reaction with palladium(II) acetate in a self-assembly process to give a palladacycle with a characteristic tetranuclear structure. This complex reacts with triphenylphosphine in a ligand-substitution process, cleaving of the tetranuclear structure. Students assign the resonances in the ¹H, ¹³C-{¹H}, and ³¹P-{¹H} NMR spectra of the prepared compounds, whose 3D structure is given to understand the relative spatial disposition of the cyclometalated fragments. Mass spectra are interpreted taking into account the characteristic isotopic pattern originated by the tetranuclear [Pd₄L₄]⁺ molecular ion.

Keywords:

Upper-Division Undergraduate; Inorganic Chemistry; Laboratory Instruction; Hands-On Learning/Manipulatives; Coordination Compounds; Mass Spectrometry; NMR Spectroscopy; Organometallics; Synthesis