4.5 Article

Synthesis, characterisation and crystal structures of new water-soluble 1-alkanaminedicarbonyl(η5-cyclopentadienyl)ruthenium(II) tetrafluoroborate complex salts

Journal

INORGANICA CHIMICA ACTA
Volume 415, Issue -, Pages 44-51

Publisher

ELSEVIER SCIENCE SA
DOI: 10.1016/j.ica.2014.02.026

Keywords

Ruthenium alkanamine complexes; Crystal structure; Ruthenium carbonyl; Cyclopentadienyl ruthenium; Melting point trends

Funding

  1. NRF
  2. THRIP
  3. UKZN (URF)

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New water-soluble 1-alkanaminedicarbonyl(eta(5)-cyclopentadienyl) ruthenium(II) tetrafluoroborate complex salts, [CpRu(CO)(2)NH2R]+BF4 (Cp = eta(5)-C5H5) (R= CH3 1, C2H5 2, C3H7 3, C4H9 4, C5H11 5 and C6H13 6), were synthesised by the reaction of the organometallic Lewis acid, [CpRu(CO)(2)](+) BF4, with slight excesses of 1-alkanamines, RNH2, in dry methylene chloride at room temperature and pressure. These compounds are reported for the first time and have been fully characterised by IR, electrospray ionisation mass spectroscopy, H-1 and C-13 NMR spectroscopy, and elemental analysis. Spectral data show that the n-alkanamines are sigma-bonded to the metal centre via the nitrogen atom. Complexes 2-5 were characterised by single crystal X-ray diffraction and all four cationic species feature a pseudo-octahedral three-legged piano stool'' structure in which the ruthenium centre is coordinated through a sigma bond to the amine N atom and two carbonyl ligands at the base of the stool and the cyclopentadienyl ring in the apex of the stool. IR studies showed that peaks of the nu CO stretching vibrations shifted slightly to lower frequency as the carbon chain length increased. The melting point and percentage yields were observed to generally decrease with increase in n-value. (C) 2014 Elsevier B.V. All rights reserved.

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