高等学校化学学报

高等学校化学学报 ›› 2000, Vol. 21 ›› Issue (10): 1455.

• 论文 • 上一篇    下一篇

两个异亚硝基乙酰丙酮-N-芳基亚胺Pd(Ⅱ)配合物的合成、谱学性质和PdCl(C6H5—IAI)(C6H5NH2)的晶体结构

冯云龙, 刘世雄   

  1. 福州大学中心实验室, 福州 350002
  • 收稿日期:1999-10-22 出版日期:2000-10-24 发布日期:2000-10-24
  • 通讯作者: 刘世雄(1943年出生),男,教授,博士生导师,从事结构化学和固体化学研究.
  • 基金资助:

    福建省自然科学基金(批准号:B97006)资助

Syntheses and Spectral Properties of Two Complexes of Isonitrosoacetylacetone- N -arylimine and Crystal Structure of PdCl(C6H5-IAI)(C6H5NH2)

FENG Yun-Long, LIU Shi-Xiong   

  1. Central Laboratory, Fuzhou University, Fuzhou 350002, China
  • Received:1999-10-22 Online:2000-10-24 Published:2000-10-24

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摘要： 合成了两个异亚硝基乙酰丙酮-N-芳基亚胺的Pd(Ⅱ)配合物,PdCl(C6H5—IAI)(C6H5NH2)(1)和PdCl(p-CH3C6H4—IAI)(pCH3C6H4NH2)(2),并测定了配合物1的晶体结构.配合物1晶体属正交晶系,空间群为Pca21,晶胞参数a=1.8587(4)nm,b=0.9380(2)nm,c=2.1237(4)nm,Z=8,F(000)=1760,μ=1.160mm-1,R1=0.0271.二齿Schiff碱配体的异亚硝基(肟基)的N原子和亚胺的N原子,苯胺基N原子和Cl-离子与Pd(Ⅱ)配位,形成PdN3Cl平面正方形配位构型.红外和喇曼光谱表明,形成配合物后νC=O和νC=N移向低频,而νN—O则移向高频.电子光谱说明存在π-π*和d-π*跃迁.

关键词: 钯配合物, 异亚硝基乙酰丙酮亚胺, Schiff碱, 晶体结构

Abstract: Two complexes of isonitrosoacetylacetone-N-arylimine, PdCl(C6H5—IAI)(C6H5NH2)(1) and PdCl( p-CH3C6H4—IAI)( p-CH3C6H4NH2)(2), were synthesized and characterized by IRand Raman spectroscopy. Complex 1 crystallizes in orthorhombic system, space group Pca 21, with parameters a =1.8587(4) nm, b =0.9380(2) nm, c =2.1237(4) nm, V =3.702(1) nm3, Dc=1.572 g/cm3, Z =8, F (000)=1760 , μ =1.160 mm-1 . The final R1 value is 0.0271 for 3592 observed reflections with I≥2σ(I) . The Pd(Ⅱ) ion has a distorted square-planar PdN3Cl coordination composed of imino-nitrogen and oximo-nitrogen from the Schiff base ligand, amino-nitrogen from aniline and chlorine anion. The oxime group of the Schiff base ligand is coordinated to the Pd(Ⅱ) through its oximo-nitrogen atom, but not its oximo-oxygen-atom. The νC=O and νC=N bands display a shift to lower frequencies and νN-O bands to higher frequencies in IRand Raman spectra. There are π-π* transition and d-π* charge transfer transition in electronic spectra.

Key words: Pd complexes, Isonitrosoacetylacetoneimine, Schiff base, Crystal structure

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