Synthesis, structure and spectral characteristics of Ni(II), Pd(II) and Zn(II) complexes with N-(2-pyridinyl)morpholine-4-carbothioamide

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• 作者：S.I. Orysyk^a ; ^{orysyk@ionc.kiev.ua} ; V.V. Bon^a ; V.I. Pekhnyo^a ; Yu.L. Zborovskii^b ; V.V. Orysyk^b ; M.V. Vovk^b
• 关键词：Carbothioamide ; Carboimidothiol ; Zn(II) ; Ni(II) ; Pd(II) complexes ; NMR spectroscopy ; X-ray diffraction study
• 刊名：Polyhedron
• 出版年：2012
• 期刊代码：87_02775387
• 类别：ch
• 出版时间：11 May, 2012
• 卷：38
• 期：1
• 页码：15-25
• 文件大小：1531 K

摘要

A series of novel zinc(II), nickel(II) and palladium(II) complexes with a thiourea derivative (N-(2-pyridinyl)morpholine-4-carbothioamide) (HL) and its oxidation product (N-(2-pyridinyl)morpholine-4-carboxamide) (HL鈥? have been synthesized and characterized by single crystal X-ray diffraction study, IR, UV-Vis, ¹H and ¹³C NMR spectroscopy. It has been shown that under synthesis conditions, HL coordinates in a thiol tautomeric form leading to formation of mononuclear complexes cis-[ML₂], where two ligand molecules are coordinated to metal ions via pyridinyl nitrogen and imidothiolic sulfur in a bidentate manner with the formation of six-membered chelate metallocycles. It has been found that utilizing different conditions nickel complexes are able to crystallize in two polymorphic modifications, which differ solely in the mode of intermolecular interactions. It has been shown that a mixed-ligand complex Ni(C₁₀H₁₃N₃O₂)₂(C₂H₅SO₄)₂ can be obtained by reaction of Ni(NO₃)₂ with reaction by-products (pyridine-containing carboxamide and monoethyl sulfate) formed in selected synthesis conditions.