Synthesis of new palladium(II) complexes containing tetradentate-nitrogen donor ligands: Combined structural studies by NMR spectroscopy and X-ray crystallography
摘要:
Treatment of the tetradentate (N N' 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 [PdCl(2)(CH(3)CN)(2)] in a 1:1 M/L ratio in acetonitrile produces [Pd(2)Cl(4)(L)] and [PdCl(2)(L)] (L = ddad and bedp). Treatment of the corresponding complex [PdCl(2)(L)] (L = ddad, bedp) in the presence of AgBF(4) in CH(2)Cl(2)/methanol (2:1) or NaBF(4) in acetonitrile gives [Pd(L)](BF(4))(2). The Pd(II) complexes have been characterised by elemental analyses, conductivity measurements, IR and (1)H and (13)C{(1)H} NMR spectroscopies when possible. The X-ray structure of the complex [Pd(ddad)]Cl(2) center dot 3H(2)O 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. (C) 2007 Elsevier B.V. All rights reserved.