Characterization of iron-sulfur cubane clusters by fast atom bombardment mass spectrometry: The Formation of ionic [FemSn] clusters through gas-phase unimolecular reduction their solution parallels

Wen Lian Lee, A. Gage, Zhi Heng Huang, Chi K. Chang, Mercouri G Kanatzidis, John Allison

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Abstract

Fast atom bombardment mass spectrometry (FAB-MS) has been used to analyze a series of iron-sulfur clusters (A)2Fe4S4X4, where A = R4N or Ph4P and X = Cl, Br, SEt, SPh. A cluster with mixed Cl, SPh ligands was also studied. The usefulness of the FAB technique in characterizing these and related biologically-relevant complexes is evaluated. The best FAB-MS results for these clusters were obtained with 3-nitrobenzyl alcohol (NBA) 2-nitrophenyl octyl ether (NPOE) as matrices. The most unique feature of the negative ion FAB mass spectra is the identification of the intact ionic core [Fe4S4X4]-, preformed anions [(A)Fe4S4X4]-, a series of cluster fragment ions. A mechanism is proposed to explain the formation of small [FemSn] clusters through unimolecular reduction processes that involve only +2 and +3 oxidation states for the Fe atoms. This work demonstrates that FAB-MS can be employed as a valid method for rapid molecular weight determination as well as structural elucidation of [Fe4S4] cluster-containing complexes.

Original languageEnglish
Pages (from-to)7132-7141
Number of pages10
JournalJournal of the American Chemical Society
Volume114
Issue number18
Publication statusPublished - 1992

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Fast Atom Bombardment Mass Spectrometry
Sulfur
Mass spectrometry
Iron
Gases
Atoms
Ions
Negative ions
Anions
Molecular Weight
Ligands
Ethers
Alcohols
Molecular weight
Oxidation

ASJC Scopus subject areas

  • Chemistry(all)

Cite this

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title = "Characterization of iron-sulfur cubane clusters by fast atom bombardment mass spectrometry: The Formation of ionic [FemSn] clusters through gas-phase unimolecular reduction their solution parallels",
abstract = "Fast atom bombardment mass spectrometry (FAB-MS) has been used to analyze a series of iron-sulfur clusters (A)2Fe4S4X4, where A = R4N or Ph4P and X = Cl, Br, SEt, SPh. A cluster with mixed Cl, SPh ligands was also studied. The usefulness of the FAB technique in characterizing these and related biologically-relevant complexes is evaluated. The best FAB-MS results for these clusters were obtained with 3-nitrobenzyl alcohol (NBA) 2-nitrophenyl octyl ether (NPOE) as matrices. The most unique feature of the negative ion FAB mass spectra is the identification of the intact ionic core [Fe4S4X4]-, preformed anions [(A)Fe4S4X4]-, a series of cluster fragment ions. A mechanism is proposed to explain the formation of small [FemSn] clusters through unimolecular reduction processes that involve only +2 and +3 oxidation states for the Fe atoms. This work demonstrates that FAB-MS can be employed as a valid method for rapid molecular weight determination as well as structural elucidation of [Fe4S4] cluster-containing complexes.",
author = "Lee, {Wen Lian} and A. Gage and Huang, {Zhi Heng} and Chang, {Chi K.} and Kanatzidis, {Mercouri G} and John Allison",
year = "1992",
language = "English",
volume = "114",
pages = "7132--7141",
journal = "Journal of the American Chemical Society",
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TY - JOUR

T1 - Characterization of iron-sulfur cubane clusters by fast atom bombardment mass spectrometry

T2 - The Formation of ionic [FemSn] clusters through gas-phase unimolecular reduction their solution parallels

AU - Lee, Wen Lian

AU - Gage, A.

AU - Huang, Zhi Heng

AU - Chang, Chi K.

AU - Kanatzidis, Mercouri G

AU - Allison, John

PY - 1992

Y1 - 1992

N2 - Fast atom bombardment mass spectrometry (FAB-MS) has been used to analyze a series of iron-sulfur clusters (A)2Fe4S4X4, where A = R4N or Ph4P and X = Cl, Br, SEt, SPh. A cluster with mixed Cl, SPh ligands was also studied. The usefulness of the FAB technique in characterizing these and related biologically-relevant complexes is evaluated. The best FAB-MS results for these clusters were obtained with 3-nitrobenzyl alcohol (NBA) 2-nitrophenyl octyl ether (NPOE) as matrices. The most unique feature of the negative ion FAB mass spectra is the identification of the intact ionic core [Fe4S4X4]-, preformed anions [(A)Fe4S4X4]-, a series of cluster fragment ions. A mechanism is proposed to explain the formation of small [FemSn] clusters through unimolecular reduction processes that involve only +2 and +3 oxidation states for the Fe atoms. This work demonstrates that FAB-MS can be employed as a valid method for rapid molecular weight determination as well as structural elucidation of [Fe4S4] cluster-containing complexes.

AB - Fast atom bombardment mass spectrometry (FAB-MS) has been used to analyze a series of iron-sulfur clusters (A)2Fe4S4X4, where A = R4N or Ph4P and X = Cl, Br, SEt, SPh. A cluster with mixed Cl, SPh ligands was also studied. The usefulness of the FAB technique in characterizing these and related biologically-relevant complexes is evaluated. The best FAB-MS results for these clusters were obtained with 3-nitrobenzyl alcohol (NBA) 2-nitrophenyl octyl ether (NPOE) as matrices. The most unique feature of the negative ion FAB mass spectra is the identification of the intact ionic core [Fe4S4X4]-, preformed anions [(A)Fe4S4X4]-, a series of cluster fragment ions. A mechanism is proposed to explain the formation of small [FemSn] clusters through unimolecular reduction processes that involve only +2 and +3 oxidation states for the Fe atoms. This work demonstrates that FAB-MS can be employed as a valid method for rapid molecular weight determination as well as structural elucidation of [Fe4S4] cluster-containing complexes.

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