Issue 6, 2000
From the journal:

Journal of the Chemical Society, Dalton Transactions

Palladium(II) chloride complexes with 1,2,4-triazolo[1,5-a]pyrimidines: X-ray, 15N–1H NMR and 15N CP MAS studies

Edward Szłyk,*a   Antoni Grodzicki,a   Leszek Pazderski,a   Andrzej Wojtczak,a   Janusz Chatłas,a   Grzegorz Wrzeszcz,a   Jerzy Sitkowskib  and  Bohdan Kamieńskic  

* Corresponding authors

a Faculty of Chemistry, Nicholas Copernicus University, Gagarina 7, Toruń, Poland

b Drug Institute, Chełmska 30/34, Warsaw, Poland

c Institute of Organic Chemistry, Kasprzaka 44/52, Warsaw, Poland

Abstract

Palladium(II) complexes of formula [Pd(tp)2Cl2] 1, [Pd(dmtp)2Cl2]·H2O 2, [Pd(dptp)2Cl2]·H2O 3, [Pd(dbtp)2Cl2] 4a, 4b, where tp = 1,2,4-triazolo[1,5-a]pyrimidine, dmtp = 5,7-dimethyl-1,2,4-triazolo[1,5-a]pyrimidine, dptp = 5,7-diphenyl-1,2,4-triazolo[1,5-a]pyrimidine, dbtp = 5,7-di-tert-butyl-1,2,4-triazolo[1,5-a]pyrimidine, were prepared. The crystal structure of [Pd(dbtp)2Cl2]·0.5 C2H5OH 4c was resolved by X-ray diffraction analysis, exhibiting monomeric, nearly square-planar cis geometry and N(3) co-ordination. A small tetrahedral distortion from the co-ordination plane was observed. The Pd–Cl distances are 2.276(1) and 2.283(1) Å, and Pd–N 2.042(3) and 2.040(3) Å. Spectroscopic measurements (UV-VIS, IR, NMR) suggested analogous structures for 1, 2 and 3. Compounds 4a and 4b are most likely rotational isomers in solution and distortional isomers in the solid state. 15N–1H heteronuclear correlation NMR was measured for 2, 4a and 4b whereas 1 and 3 were characterized with 13C and 15N CP MAS. Significant shielding of the co-ordinated N(3) and adjacent C(2) or C(3a) nuclei was observed.

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Article information

DOI
https://doi.org/10.1039/A908469J
Article type
Paper
Submitted
25 Oct 1999
Accepted
24 Jan 2000
First published
01 Mar 2000

J. Chem. Soc., Dalton Trans., 2000, 867-872

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Palladium(II) chloride complexes with 1,2,4-triazolo[1,5-a]pyrimidines: X-ray, 15N–1H NMR and 15N CP MAS studies

E. Szłyk, A. Grodzicki, L. Pazderski, A. Wojtczak, J. Chatłas, G. Wrzeszcz, J. Sitkowski and B. Kamieński, J. Chem. Soc., Dalton Trans., 2000, 867 DOI: 10.1039/A908469J

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