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一些 2,5-己二酮双(水杨酰腙)配合物的光谱和结构研究:其 Ni(II)和 Cu(II)配合物及 N-(2,5-二甲基-1H-吡咯-1-基)-2-羟基苯甲酰胺的晶体结构。

Spectroscopic and structural study of some 2,5-hexanedione bis(salicyloylhydrazone) complexes: crystal structures of its Ni(II) and Cu(II) complexes and N-(2,5-dimethyl-1H-pyrrol-1-yl)-2-hydroxy-benzamide.

机构信息

Chemistry Department, Faculty of Science, Kuwait University, P.O. Box 5969, Safat 13060, Kuwait.

Chemistry Department, Faculty of Science, Kuwait University, P.O. Box 5969, Safat 13060, Kuwait.

出版信息

Spectrochim Acta A Mol Biomol Spectrosc. 2014 Aug 14;129:307-13. doi: 10.1016/j.saa.2014.02.195. Epub 2014 Mar 13.

Abstract

The reaction between 2,5-hexanedione and salicylic acid hydrazide produced two compounds: 2,5-hexanedione bis(salicyloylhydrazone) [HDSH] (ethanol insoluble) and N-(2,5-dimethyl-1H-pyrrol-1-yl)-2-hydroxybenzamide [DPH] (ethanol soluble). HDSH formed complexes with Co(II), Ni(II), Cu(II), Zn(II), Cd(II), Hg(II) and Pd(II) which are characterized by elemental analyses, spectra (IR, (1)H NMR, ESR and MS), thermal and magnetic measurements. The crystals of [Ni(HDSH-2H)(EtOH)(H2O)] and [Cu(HDSH-2H)] were solved having octahedral and square-planar geometries, respectively. The other complexes have the formulae [Co(HDSH-2H)(H2O)2], [Cu(HDSH-H)2], [Zn(HDSH-2H)(H2O)2], [Cd2(HDSH-4H)(H2O)4], [Cd2(HDSH-2H)(H2O)4Cl2]; [Hg(HDSH-2H)] and [Pd2(HDSH-4H)(H2O)4]. The obtained complexes are stable in air and non-hygroscopic. The magnetic moments and electronic spectra of the complexes provide different geometries. The ESR spectra support the mononuclear geometry for [Cu(HDSH-2H)] and [Cu(HDSH-H)2]. The thermal decomposition of the complexes revealed the coordinated waters as well as the end product which is in most cases the metal oxide. The crystal structure of N-(2,5-dimethyl-1H-pyrrol-1-yl)-2-hydroxybenzamide is solved by X-ray technique.

摘要

2,5-己二酮与水杨酰肼反应生成两种化合物:2,5-己二酮双(水杨酰腙)[HDSH](不溶于乙醇)和 N-(2,5-二甲基-1H-吡咯-1-基)-2-羟基苯甲酰胺[DPH](溶于乙醇)。HDSH 与 Co(II)、Ni(II)、Cu(II)、Zn(II)、Cd(II)、Hg(II)和 Pd(II)形成配合物,这些配合物通过元素分析、光谱(IR、(1)H NMR、ESR 和 MS)、热和磁测量来表征。[Ni(HDSH-2H)(EtOH)(H2O)]和[Cu(HDSH-2H)]的晶体结构分别为八面体和平面正方形。其他配合物的化学式为[Co(HDSH-2H)(H2O)2]、[Cu(HDSH-H)2]、[Zn(HDSH-2H)(H2O)2]、[Cd2(HDSH-4H)(H2O)4]、[Cd2(HDSH-2H)(H2O)4Cl2]、[Hg(HDSH-2H)]和[Pd2(HDSH-4H)(H2O)4]。所得到的配合物在空气中稳定且不吸湿。配合物的磁矩和电子光谱提供了不同的几何形状。ESR 光谱支持[Cu(HDSH-2H)]和[Cu(HDSH-H)2]的单核几何形状。配合物的热分解揭示了配位水以及最终产物,大多数情况下是金属氧化物。N-(2,5-二甲基-1H-吡咯-1-基)-2-羟基苯甲酰胺的晶体结构通过 X 射线技术得到解决。

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