Studies on the reduction of [(C5Me5)2Mo2O5] in methanol/water/acetate solutions by on-line electrochemical flowcell and electrospray mass spectrometry

Jenny Gun*, Alexandre Modestov, Ovadia Lev, Dirk Saurenz, Mikhail A. Vorotyntsev, Rinaldo Poli

*Corresponding author for this work

Research output: Contribution to journalArticlepeer-review

31 Scopus citations

Abstract

The complex [Cp*2Mo2O5] (Cp* = η5-C5Me5) and its electrochemical reduction products in acetic acid/acetate-buffered (pH = 4.0) water/methanol solutions were investigated by combined electrochemical (EC) flowcell and on-line electrospray ionization mass spectrometry (ESI-MS). Mono-, di-, tri-, and tetranuclear organometallic molybdenum oxides were identified in the starting solution. The effect of the relevant ESI-MS parameters (ionic mode, heated capillary voltage, and heated capillary temperature) and of the concentration on the observed distribution of ions in the mass spectrometer was studied in order to minimize side reactions in the ESI chamber. It was verified that reduction in the ESI-MS is undetectable under open-circuit conditions. The on-line electrochemical study revealed the potential-dependent formation of previously unknown mono-, di-, tri-, and tetranuclear MoV, MoIV, and mixed-valence complexes. The compounds were identified by their characteristic isotope patterns and their ion trap MSn fragmentations. The observed formation potentials reflect the higher stability of the multinuclear species relative to the mononuclear ones with the same oxidation state. (

Original languageAmerican English
Pages (from-to)482-492
Number of pages11
JournalEuropean Journal of Inorganic Chemistry
Issue number3
DOIs
StatePublished - Feb 2003

Keywords

  • Cyclopentadienyl ligands
  • Electrochemistry
  • Mass spectrometry
  • Molybdenum
  • Oxo ligands

Fingerprint

Dive into the research topics of 'Studies on the reduction of [(C5Me5)2Mo2O5] in methanol/water/acetate solutions by on-line electrochemical flowcell and electrospray mass spectrometry'. Together they form a unique fingerprint.

Cite this