Synthesis of new palladium(II) complexes containing tetradentate-nitrogen donor ligands: Combined structural studies by NMR spectroscopy and X-ray crystallography

详细信息	查看全文 | 推荐本文 |

• 作者：Mò ; nica Espinal ; Josefina Pons ; Jordi Garc&#xed ; a-Antó ; n ; Xavier Solans ; Mercè ; Font-Bardia ; Josep Ros
• 关键词：Palladium(II) ; Tetradentate-nitrogen ligands ; Pyrazole complexes ; Crystal structure
• 刊名：Inorganica Chimica Acta
• 出版年：2008
• 期刊代码：40_00201693
• 类别：ch
• 出版时间：27 June 2008
• 卷：361
• 期：9-10
• 页码：2648-2658
• 文件大小：324 K

摘要

Treatment of the tetradentate (NN′N′N) N-alkylaminopyrazole ligands 3,6-dimethyl-1,8-(3,5-dimethyl-1-pyrazolyl)-3,6-diazaoctane (ddad) and 1,4-bis[2-(3,5-dimethyl-1-pyrazolyl)ethyl]piperazine (bedp) with [PdCl₂(CH₃CN)₂] in a 1:1 M/L ratio in acetonitrile produces [Pd₂Cl₄(L)] and [PdCl₂(L)] (L = ddad and bedp). Treatment of the corresponding complex [PdCl₂(L)] (L = ddad, bedp) in the presence of AgBF₄ in CH₂Cl₂/methanol (2:1) or NaBF₄ in acetonitrile gives [Pd(L)](BF₄)₂. The Pd(II) complexes have been characterised by elemental analyses, conductivity measurements, IR and ¹H and ¹³C{¹H} NMR spectroscopies when possible. The X-ray structure of the complex [Pd(ddad)]Cl₂ · 3H₂O has been determined. The Pd(II) is coordinated to the ddad ligand by two nitrogen atoms of pyrazolyl groups and two nitrogen atoms of the amine groups, in a slightly distorted square-planar geometry.