首页> 外文期刊>Inorganica Chimica Acta >Crystal strucrures and coordiantion-site exchange reactions of palladium(II) and platinum(II) complexes containing tris[2-(tert-butylthio)ethyl]amine
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Crystal strucrures and coordiantion-site exchange reactions of palladium(II) and platinum(II) complexes containing tris[2-(tert-butylthio)ethyl]amine

机译:含三[2-(叔丁硫基)乙基]胺的钯(II)和铂(II)配合物的晶体结构和配位交换反应

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Palladium(I1) and platinum(I1) complexes, [PdX(NS3’Bu)JBPh4 iX = CI. Br. 1; NS.2Bu = tris[2-(rert -butylthio)ethyl]amine) and [PtCl(NS~’Bu)]BPh4, were prepared, and their structures were determined by X-ray analyses. The geometry around the palladium and platinum atoms is square planar. The NS~Bu ligand functions as a tridentate ligand and one sulfur atom is not coordinated to the metal. The 1H NMR spectrum of [PdCI(NS~1Bu)]BPh4 in acetone-d6 exhibited a dynamic behavior. At 200C the spectrum showed a singlet signal at 1.60 ppm that can be assigned to tert-butyl protons. whereas at — 700C three singlet signals were observed at 1.36. 1.61, and 1.70 ppm with an intensity ratio of 1: 0.25: 2. The signals at 1.36 and 1.70ppm are assigned to the tert-butyl protons in the square-planar structure, and these signals are consistent with the X-ray structure. The signal at 1.61 ppm can be assigned to the tert-butyl protons in a trigonal-bipyramid~l structure where the three tert-butyl groups are magnetically equivalent. Thus. we concluded that the coordination-site exchange occurred via a trigonal-bipyramidal intermediate~ The square-planar and trigonal-bipyramidal species of [PdC1(NS~Bu)]BPh4 are in equilibrium in acetone-d~ The equilibrium was shifted toward the square-planar species on decreasing the temperature. The H NMR spectra for [PdX(NS3’ Bu)]BPh4 (X = Cl, Br, and I) were similar to one another at the same temperature, suggesting that the site-exchange process is insensitive to the kind of coexisting halogen ligand. The site exchange reaction of [PtCl(NS~’ Bu)IBPh4 seems to occur more slowly than that of the palladium(II) analogue.
机译:钯(I1)和铂(I1)络合物[PdX(NS3’Bu)JBPh4 iX = CI。 Br。 1;制备了NS.2Bu =三[2-(叔丁硫基)乙基]胺和[PtCl(NS_’Bu)] BPh4,并通过X射线分析确定了它们的结构。钯和铂原子周围的几何形状为正方形平面。 NS-Bu配体起三齿配体的作用,并且一个硫原子不与金属配位。丙酮-d6中[PdCI(NS〜1Bu)] BPh4的1H NMR光谱显示出动态行为。在200℃下,光谱显示出在1.60ppm处的单重态信号,其可以归属于叔丁基质子。而在– 700C时,在1.36处观察到三个单峰信号。强度比为1:0.25:1.61和1.70ppm。1.36和1.70ppm处的信号分配给方形结构中的叔丁基质子,这些信号与X射线结构一致。可以将在1.61 ppm处的信号分配给一个三角双锥体结构的叔丁基质子,其中三个叔丁基是磁性等效的。从而。我们得出结论,配位位置交换是通过三角-双锥体中间体发生的。[PdC1(NS〜Bu)] BPh4的方形-平面和三角形-双锥体的物种在丙酮-d中处于平衡状态。 -平面种类降低温度。 [PdX(NS3'Bu)] BPh4(X = Cl,Br和I)的1 H NMR谱在相同温度下彼此相似,表明位点交换过程对共存卤素配体的种类不敏感。 [PtCl(NS〜’Bu)IBPh4的位点交换反应似乎比钯(II)类似物的反应更慢。

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