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金属离子导向的 Ni(II)、Cu(II) 和 Zn(II) 的 N2O2 型螯合配合物的合成:光谱、热和单晶研究。

Metal-ion directed synthesis of N2O2 type chelate complexes of Ni(II), Cu(II) and Zn(II): spectral, thermal and single crystal studies.

机构信息

Department of Chemistry, Aligarh Muslim University, Aligarh 202 002, India.

出版信息

Spectrochim Acta A Mol Biomol Spectrosc. 2012 Dec;98:240-6. doi: 10.1016/j.saa.2012.08.004. Epub 2012 Aug 16.

Abstract

A set of Ni(II), Cu(II) and Zn(II) complexes of Schiff base have been synthesized by one pot condensation reaction of 2-hydroxy-4-methoxybenzophenone with 1,3-diaminopropane in 1:2:1 molar ratio. They have been characterized by elemental analysis, conductance measurement, thermal analysis (TGA/DTA), FT-IR, (1)H-NMR, EPR spectra, ESI-MS and electronic spectral studies. In order to establish the geometry, a single crystal X-ray structure for [Ni(L)] complex was determined. It crystallizes in monoclinic system having unit cell parameters a=14.015(5)Å, b=13.391(5)Å, c=14.931(5)Å and α=90.000(5)(o), β=112.237(5)(o), γ=90.000(5)(o) with P 2(1)/c space group. No π-π stacking interaction was obtained in molecular packing diagram. A square-planar geometry has been confirmed for Ni(II) complex. Furthermore, on the basis of elemental analysis, IR, UV-visible and EPR data a square-planar geometry for Cu(II) and a distorted octahedral geometry for the Zn(II) complex has been established. In case of Zn(II) complex NO(3)(-) group was found to be coordinated in monodentate fashion. The low molar conductivity values of the complexes measured in chloroform and DMSO suggest their non-ionic nature.

摘要

由 2-羟基-4-甲氧基二苯甲酮与 1,3-二氨基丙烷以 1:2:1 的摩尔比在一锅反应中合成了一组 Ni(II)、Cu(II)和 Zn(II)的席夫碱配合物。它们通过元素分析、电导率测量、热分析(TGA/DTA)、FT-IR、(1)H-NMR、EPR 光谱、ESI-MS 和电子光谱研究进行了表征。为了确定几何形状,确定了[Ni(L)]配合物的单晶 X 射线结构。它结晶为单斜晶系,具有单元晶胞参数 a=14.015(5)Å、b=13.391(5)Å、c=14.931(5)Å 和 α=90.000(5)(o)、β=112.237(5)(o)、γ=90.000(5)(o),具有 P 2(1)/c 空间群。在分子堆积图中没有获得 π-π 堆积相互作用。证实了 Ni(II)配合物具有正方形平面几何形状。此外,根据元素分析、IR、UV-可见和 EPR 数据,Cu(II)配合物具有正方形平面几何形状,Zn(II)配合物具有扭曲的八面体几何形状。在 Zn(II)配合物中,发现 NO(3)(-) 基团以单齿配位方式配位。在氯仿和 DMSO 中测量的配合物的低摩尔电导率值表明它们具有非离子性质。

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