Electrochemical, spectroscopic, magnetic and structural studies of complexes bearing ferrocenyl ligands of N-(3-hydroxypicolinoyl)picolinamide

The synthesis and in-depth characterisation including X-ray crystallography of a new hydroxy derivative of bis(2-pyridylcarbonyl)amine Hbpca, namely N-(3-hydroxypicolinoyl)picolinamide (Hbpca-OH), as well as two ferrocenyl derivatives of Hbpca-OH, namely 2-(picolinoylcarbamoyl)pyridin-3-yl ferroceno...

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Published inNew journal of chemistry Vol. 36; no. 9; pp. 1819 - 1827
Main Authors Gasser, Gilles, Mari, Cristina, Burkart, Michelle, Green, Stephen J., Ribas, Joan, Stoeckli-Evans, Helen, Tucker, James H. R.
Format Journal Article
LanguageEnglish
Published CAMBRIDGE Royal Soc Chemistry 01.01.2012
Subjects
Chemistry
Chemistry, Multidisciplinary
Physical Sciences
Science & Technology
BRIDGING LIGAND
CRYSTAL-STRUCTURE
MOLECULAR RECOGNITION
ORGANIC-COMPOUNDS
X-RAY
TRINUCLEAR COMPLEXES
REDOX PROPERTIES
RECEPTOR MOLECULES
DERIVATIVES
M(BPCA) M
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Summary:The synthesis and in-depth characterisation including X-ray crystallography of a new hydroxy derivative of bis(2-pyridylcarbonyl)amine Hbpca, namely N-(3-hydroxypicolinoyl)picolinamide (Hbpca-OH), as well as two ferrocenyl derivatives of Hbpca-OH, namely 2-(picolinoylcarbamoyl)pyridin-3-yl ferrocenoate (HL1) and bis(2-(picolinoylcarbamoyl)pyridin-3-yl) 1,1'-ferrocenoate (H2L2), is reported. HL1 and H2L2 were complexed with five different transition metal cations, namely Fe2+, Zn2+, Ni2+, Cu2+ and Cu+, to give ten complexes with varying stoichiometries, which were characterised by different analytical methods including H-1 NMR, ESI-MS, IR spectroscopy and microanalysis. The metal complexation was also confirmed by electrochemical measurements for all complexes except Zn(L-1)(2) and FeL2, for which the changes in formal redox potentials of ferrocene Delta E degrees' observed were not significant enough. Furthermore, two X-ray structures of Cu-II complexes, namely [Cu2I2L21] and [Cu2I2L2](n), were determined. Both structures contain an extremely rare Cu-II-I-2-Cu-II bridge. Finally, a small antiferromagnetic coupling in [Cu2I2L2](n) was observed.
ISSN:1144-0546
1369-9261
DOI:10.1039/c2nj40177k