DOI: 10.1002/cber.19971300912. Synthesis, Redox Chemistry, and Mixed‐Valence Phenomena of Cyanide‐Bridged Dinuclear Organometallic Complexes

Synthesis, Redox Chemistry, and Mixed‐Valence Phenomena of Cyanide‐Bridged Dinuclear Organometallic Complexes

10.1002/cber.19971300912

Crossref journal-article

Wiley

Chemische Berichte (311)

Abstract

Abstract21 new organometallic complexes of the type M–Cn–M′ containing the building blocks M, M′ = (CO)5Cr, (CO)5Mo, (CO)5W, Cp(CO)2Mn, Cp(CO)2Fe, Cp(CO)(CN)Fe, Cp(dppe)Fe, Cp(PPh3)2Ru, Cp(PPh3)Ni, and (PPh3)2Ag were obtained from the reagents M–Cn and M–X (X = leaving group). Among them are five pairs of linkage isomers M–CN–M′/M–NC‐M′. Structure determinations of (CO)5Cr–CN–M′ with M′ = Fe(dppe)Cp, Ni(PPh3)Cp, Ag(PPh3)2 and of (CO)5Cr–NC‐Fe(dppe)Cp have proved their identity and the linkage isomerism. Systematic variations of the v(CN) and v(CO) IR bands allow as assessment of the relative electron pair acceptor strengths of the building blocks M and M′ and a reliable identification of the individual linkage isomers. All dinuclear complexes are redox‐active, showing at lease one reversible oxidation. The redox potentials are characteristically dependent upon the nature of the building blocks M and M′ and upon the orientation of the cyanide link (CN vs. NC), 6 oxidized complexes of the type [M–Cn–Fe(dppe)Cp]+ were prepared chemically and isolated as PF6 or BF4salts. The molecular structure of [(CO)5Cr–CN–Fe(dppe)Cp]BF4 is not significantly different from those of the corresponding neutral Cr–CN–Fe or Cr–NC‐Fe complexes. Upon oxidation the v(CN) band of the complexes shifts to lower wavenumbers and becomes much more intense. The oxidized complexes show the paramagnetism due to one unpaired electron. They give rise to very intense metal‐to metal charge‐transfer bands in the near infrared region whose position was found to be characteristically dependent on solvent polarity of [(CO)5Cr–CN–Fe(dppe)Cp]BF4. A semiquantitative treatment of the optical and electrochemical measurements shows that the electron delocalization and metal–metal interaction in the oxidized dinuclear complexes is significant and that they belong to the class‐II mixed‐valence systems.

Bibliography

Zhu, N., & Vahrenkamp, H. (1997). Synthesis, Redox Chemistry, and MixedâValence Phenomena of CyanideâBridged Dinuclear Organometallic Complexes. Chemische Berichte, 130(9), 1241â1252. Portico.

Authors 2

Nianyoung Zhu (first)
Heinrich Vahrenkamp (additional)

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Crystallographic data (excluding structure factors) for the structures reported in this paper have been deposited with the Cambridge Crystallographic Data Centre as supplementary publication no. CCDC‐100389. Copies of the data can be obtained free of charge on appication to The Director CCDC 12 Union Road Cambridge CB2 1EZ UK [fax: int. code +44(1223)336–033 e‐mail: deposit@chemcrys.cam.ac. uk].
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Dates

Type	When
Created	18 years, 2 months ago (July 2, 2007, 8:56 p.m.)
Deposited	2 years ago (Sept. 2, 2023, 2:20 a.m.)
Indexed	1 year, 10 months ago (Oct. 16, 2023, 1:21 a.m.)
Issued	28 years ago (Sept. 1, 1997)
Published	28 years ago (Sept. 1, 1997)
Published Online	19 years, 7 months ago (Jan. 25, 2006)
Published Print	28 years ago (Sept. 1, 1997)

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BibTeX

@article{Zhu_1997, title={Synthesis, Redox Chemistry, and Mixed‐Valence Phenomena of Cyanide‐Bridged Dinuclear Organometallic Complexes}, volume={130}, ISSN={0009-2940}, url={http://dx.doi.org/10.1002/cber.19971300912}, DOI={10.1002/cber.19971300912}, number={9}, journal={Chemische Berichte}, publisher={Wiley}, author={Zhu, Nianyoung and Vahrenkamp, Heinrich}, year={1997}, month=sep, pages={1241–1252} }

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  "abstract": "<jats:title>Abstract</jats:title><jats:p>21 new organometallic complexes of the type M\u2013Cn\u2013M\u2032 containing the building blocks M, M\u2032 = (CO)<jats:sub>5</jats:sub>Cr, (CO)<jats:sub>5</jats:sub>Mo, (CO)<jats:sub>5</jats:sub>W, Cp(CO)<jats:sub>2</jats:sub>Mn, Cp(CO)<jats:sub>2</jats:sub>Fe, Cp(CO)(CN)Fe, Cp(dppe)Fe, Cp(PPh<jats:sub>3</jats:sub>)<jats:sub>2</jats:sub>Ru, Cp(PPh<jats:sub>3</jats:sub>)Ni, and (PPh<jats:sub>3</jats:sub>)<jats:sub>2</jats:sub>Ag were obtained from the reagents M\u2013Cn and M\u2013X (X = leaving group). Among them are five pairs of linkage isomers M\u2013CN\u2013M\u2032/M\u2013NC\u2010M\u2032. Structure determinations of (CO)<jats:sub>5</jats:sub>Cr\u2013CN\u2013M\u2032 with M\u2032 = Fe(dppe)Cp, Ni(PPh<jats:sub>3</jats:sub>)Cp, Ag(PPh<jats:sub>3</jats:sub>)<jats:sub>2</jats:sub> and of (CO)<jats:sub>5</jats:sub>Cr\u2013NC\u2010Fe(dppe)Cp have proved their identity and the linkage isomerism. Systematic variations of the <jats:italic>v</jats:italic>(CN) and <jats:italic>v</jats:italic>(CO) IR bands allow as assessment of the relative electron pair acceptor strengths of the building blocks M and M\u2032 and a reliable identification of the individual linkage isomers. All dinuclear complexes are redox\u2010active, showing at lease one reversible oxidation. The redox potentials are characteristically dependent upon the nature of the building blocks M and M\u2032 and upon the orientation of the cyanide link (CN vs. NC), 6 oxidized complexes of the type [M\u2013Cn\u2013Fe(dppe)Cp]<jats:sup>+</jats:sup> were prepared chemically and isolated as PF<jats:sub>6</jats:sub> or BF<jats:sub>4</jats:sub>salts. The molecular structure of [(CO)<jats:sub>5</jats:sub>Cr\u2013CN\u2013Fe(dppe)Cp]BF<jats:sub>4</jats:sub> is not significantly different from those of the corresponding neutral Cr\u2013CN\u2013Fe or Cr\u2013NC\u2010Fe complexes. Upon oxidation the <jats:italic>v</jats:italic>(CN) band of the complexes shifts to lower wavenumbers and becomes much more intense. The oxidized complexes show the paramagnetism due to one unpaired electron. They give rise to very intense metal\u2010to metal charge\u2010transfer bands in the near infrared region whose position was found to be characteristically dependent on solvent polarity of [(CO)<jats:sub>5</jats:sub>Cr\u2013CN\u2013Fe(dppe)Cp]BF<jats:sub>4</jats:sub>. A semiquantitative treatment of the optical and electrochemical measurements shows that the electron delocalization and metal\u2013metal interaction in the oxidized dinuclear complexes is significant and that they belong to the class\u2010II mixed\u2010valence systems.</jats:p>",
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