Electron spin resonance and electrospray ionization mass spectroscopic studies of the interaction of alkali and alkaline earth cations with manganese bis(μ-oxo) dimers

Colin P. Horwitz; Joseph T. Warden; Susan T. Weintraub

doi:10.1016/0020-1693(96)05078-5

Electron spin resonance and electrospray ionization mass spectroscopic studies of the interaction of alkali and alkaline earth cations with manganese bis(μ-oxo) dimers

Colin P. Horwitz, Joseph T. Warden, Susan T. Weintraub

Department of Biochemistry & Structural Biology

Research output: Contribution to journal › Article › peer-review

16 Scopus citations

Abstract

The dimer [(3,3′-17-crown-6-SALPN)Mn^IV(μ-O)]₂ (2) was prepared by the reaction of (3,3′-17-crown-6-SALPN)Mn(II) with O₂ in CH₃CN. Dimer 2 when reacted with two molar equivalents of NaPF₆, KPF₆, CaTf₂ or BaTf₂ (Tf^- is SO₃CF₃^-) formed the complexes 2·2NaPF₆, 2·2KPF₆, 2·2CaTf₂ or 2·2BaTf₂, respectively. The dimers were reduced to the mixed-valent Mn^III,Mn^IV state either chemically with Cp₂Co or electrochemically and their ESR spectra recorded. The ESR spectrum of each mixed-valent dimer showed a 16-line pattern characteristic of a valence trapped antiferromagnetically coupled species. The cation containing Mn^IV,Mn^IV bis(μ-oxo) dimers were also analyzed by electrospray ionization mass spectrometry using CH₂Cl₂ and CH₃CN as solvents. Singly charged cations corresponding to the loss of one anion from the parent complex were observed for all four compounds. In addition, ions were detected in which cation exchange had occurred.

Original language	English (US)
Pages (from-to)	311-320
Number of pages	10
Journal	Inorganica Chimica Acta
Volume	246
Issue number	1-2 SPEC. ISSUE
DOIs	https://doi.org/10.1016/0020-1693(96)05078-5
State	Published - May 1996

Keywords

Dinuclear complexes
Electron spin resonance
Electrospray mass spectrometry
Manganese complexes
Oxo complexes

ASJC Scopus subject areas

Physical and Theoretical Chemistry
Inorganic Chemistry
Materials Chemistry

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10.1016/0020-1693(96)05078-5

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Electron spin resonance and electrospray ionization mass spectroscopic studies of the interaction of alkali and alkaline earth cations with manganese bis(μ-oxo) dimers. / Horwitz, Colin P.; Warden, Joseph T.; Weintraub, Susan T.

In: Inorganica Chimica Acta, Vol. 246, No. 1-2 SPEC. ISSUE, 05.1996, p. 311-320.

Research output: Contribution to journal › Article › peer-review

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title = "Electron spin resonance and electrospray ionization mass spectroscopic studies of the interaction of alkali and alkaline earth cations with manganese bis(μ-oxo) dimers",

abstract = "The dimer [(3,3′-17-crown-6-SALPN)MnIV(μ-O)]2 (2) was prepared by the reaction of (3,3′-17-crown-6-SALPN)Mn(II) with O2 in CH3CN. Dimer 2 when reacted with two molar equivalents of NaPF6, KPF6, CaTf2 or BaTf2 (Tf- is SO3CF3-) formed the complexes 2·2NaPF6, 2·2KPF6, 2·2CaTf2 or 2·2BaTf2, respectively. The dimers were reduced to the mixed-valent MnIII,MnIV state either chemically with Cp2Co or electrochemically and their ESR spectra recorded. The ESR spectrum of each mixed-valent dimer showed a 16-line pattern characteristic of a valence trapped antiferromagnetically coupled species. The cation containing MnIV,MnIV bis(μ-oxo) dimers were also analyzed by electrospray ionization mass spectrometry using CH2Cl2 and CH3CN as solvents. Singly charged cations corresponding to the loss of one anion from the parent complex were observed for all four compounds. In addition, ions were detected in which cation exchange had occurred.",

keywords = "Dinuclear complexes, Electron spin resonance, Electrospray mass spectrometry, Manganese complexes, Oxo complexes",

author = "Horwitz, {Colin P.} and Warden, {Joseph T.} and Weintraub, {Susan T.}",

note = "Funding Information: CPH wishes to thank the NSF (Grant CHE 9496236) for financial support. JTW acknowledges support in part by a Grant from the National Institutes of Health (GM26133) and a Biomedical Research Support Grant.",

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T1 - Electron spin resonance and electrospray ionization mass spectroscopic studies of the interaction of alkali and alkaline earth cations with manganese bis(μ-oxo) dimers

AU - Horwitz, Colin P.

AU - Warden, Joseph T.

AU - Weintraub, Susan T.

N1 - Funding Information: CPH wishes to thank the NSF (Grant CHE 9496236) for financial support. JTW acknowledges support in part by a Grant from the National Institutes of Health (GM26133) and a Biomedical Research Support Grant.

PY - 1996/5

Y1 - 1996/5

N2 - The dimer [(3,3′-17-crown-6-SALPN)MnIV(μ-O)]2 (2) was prepared by the reaction of (3,3′-17-crown-6-SALPN)Mn(II) with O2 in CH3CN. Dimer 2 when reacted with two molar equivalents of NaPF6, KPF6, CaTf2 or BaTf2 (Tf- is SO3CF3-) formed the complexes 2·2NaPF6, 2·2KPF6, 2·2CaTf2 or 2·2BaTf2, respectively. The dimers were reduced to the mixed-valent MnIII,MnIV state either chemically with Cp2Co or electrochemically and their ESR spectra recorded. The ESR spectrum of each mixed-valent dimer showed a 16-line pattern characteristic of a valence trapped antiferromagnetically coupled species. The cation containing MnIV,MnIV bis(μ-oxo) dimers were also analyzed by electrospray ionization mass spectrometry using CH2Cl2 and CH3CN as solvents. Singly charged cations corresponding to the loss of one anion from the parent complex were observed for all four compounds. In addition, ions were detected in which cation exchange had occurred.

AB - The dimer [(3,3′-17-crown-6-SALPN)MnIV(μ-O)]2 (2) was prepared by the reaction of (3,3′-17-crown-6-SALPN)Mn(II) with O2 in CH3CN. Dimer 2 when reacted with two molar equivalents of NaPF6, KPF6, CaTf2 or BaTf2 (Tf- is SO3CF3-) formed the complexes 2·2NaPF6, 2·2KPF6, 2·2CaTf2 or 2·2BaTf2, respectively. The dimers were reduced to the mixed-valent MnIII,MnIV state either chemically with Cp2Co or electrochemically and their ESR spectra recorded. The ESR spectrum of each mixed-valent dimer showed a 16-line pattern characteristic of a valence trapped antiferromagnetically coupled species. The cation containing MnIV,MnIV bis(μ-oxo) dimers were also analyzed by electrospray ionization mass spectrometry using CH2Cl2 and CH3CN as solvents. Singly charged cations corresponding to the loss of one anion from the parent complex were observed for all four compounds. In addition, ions were detected in which cation exchange had occurred.

KW - Dinuclear complexes

KW - Electron spin resonance

KW - Electrospray mass spectrometry

KW - Manganese complexes

KW - Oxo complexes

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Electron spin resonance and electrospray ionization mass spectroscopic studies of the interaction of alkali and alkaline earth cations with manganese bis(μ-oxo) dimers

Abstract

Keywords

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