Synthesis and structural characterization of bis-chelate Pd(II) complexes derived from substituted di-(2-pyridyl)methane ligands

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• 作者：Uvaldo Herná ; ndez-Balderas^a ; Gabriela Rodr&iacute ; guez-Garc&iacute ; a^a ; Noem&iacute ; Andrade-Ló ; pez^a ; ^{nandrade@uaeh.edu.mx} ; José ; G. Alvarado-Rodr&iacute ; guez^a ; Rafael Moreno-Esparza^b ; Marcos Flores-Alamo^b
• 关键词：Palladium complexes ; X-ray diffraction ; Bis-chelate complexes ; NMR
• 刊名：Polyhedron
• 出版年：2012
• 期刊代码：87_02775387
• 类别：ch
• 出版时间：4 April, 2012
• 卷：36
• 期：1
• 页码：104-111
• 文件大小：927 K

摘要

Bis-chelate complexes of palladium(II) derived from dipyridyl ligands of general formula [Pd(L)₂](BF₄)₂ (L = (C₅H₄N)₂C(OH)₂, (C₅H₄N)₂CH(OH), (C₅H₄N)₂CH(Cl), (C₅H₄N)₂CH(S₂CNEt₂) and (C₅H₄N)₂CH(S-C₅H₄N)) have been synthesized and characterized by elemental analyses, X-ray diffraction, vibrational, and NMR spectroscopy. Crystal structures of the complexes [bis-{di-(2-pyridyl)dihydroxymethane}palladium(II)]tetrafluoroborate (1), [bis-{di-(2-pyridyl)hydroxymethane}palladium(II)]tetrafluoroborate (2), [bis-{di-(2-pyridyl)chloromethane}palladium(II)]tetrafluoroborate (3), [bis-{di-(2-pyridyl)-N,N鈥?diethyldithiocarbamatemethane}palladium(II)]tetrafluoroborate (4) and [bis-{di-(2-pyridyl)-2-pyridylsulfanylmethane}palladium(II)]tetrafuoroborate (5) displayed to the substituted di-2-pyridylmethane ligands in a bidentate coordination mode to the palladium atom with the formation of six-membered chelate rings. In these complexes, the palladium atom showed a distorted square planar local geometry. Crystal structures of the complexes 3-5 displayed the -Cl, -S₂C(NEt)₂ and -S-C₅H₄N groups on the bridge carbon atom in a flagpole position, which is stabilized by weak intramolecular interactions of type Pd鈰疌l (for 3) and Pd鈰疭 (for 4 and 5). However, in 2 the crystallographic data showed to the major conformer containing the -OH group in a bowsprit position, displaying an intramolecular Pd鈰疕 interaction.