Synthesis and characterization of μ3222- C60 trirhenium hydrido cluster complexes

Hyunjoon Song, Yumi Lee, Zel Ho Choi, Kwangyeol Lee, Joon T. Park, Juhyoun Kwak, Moon Gun Choi

Research output: Contribution to journalArticle

32 Citations (Scopus)

Abstract

The reaction of C60 with Re3(μ-H)3(CO)11(NCMe) in refluxing chlorobenzene produces Re3(μ-H)3(CO)93- η222-C60) (1) in 50% yield. Initial decarbonylation of 1 with Me3NO/MeCN followed by reaction with PPh3 in boiling chlorobenzene affords Re3(μ-H)3(CO)8(PPh3)- (μ3222- C60) (2) in a low yield (26%). Treatment of 1 with PhCH2N=PPh3 at room temperature gives a benzyl isocyanide substituted product Re3(μ-H)3(CO)8(CNCH2Ph) (μ3 η222-C60) (3) in 53% yield. Compounds 1, 2, and 3 have been isolated as crystalline solids and characterized by spectroscopic (infrared, mass, 1H, 31P, and 13C NMR) and analytical data. The structure of 3 has been determined by a single-crystal X-ray diffraction study. The C60 ligand is coordinated to the trirhenium triangle in a μ3222 bonding mode, and the benzyl isocyanide ligand occupies an axial position of a rhenium atom. Electrochemical properties of 1 and 2 have been studied by cyclic voltammetry (CV) in chlorobenzene (CB) solutions. The general features of CV curves have revealed four reversible redox couples for 1 and 2 in the CB potential window. The CV results suggest that a C60-mediated electron transfer to the trirhenium center takes place in 12- species for 1 and 23- for 2.

Original languageEnglish
Pages (from-to)3139-3144
Number of pages6
JournalOrganometallics
Volume20
Issue number14
DOIs
Publication statusPublished - 2001 Jul 9
Externally publishedYes

Fingerprint

chlorobenzenes
Carbon Monoxide
Cyclic voltammetry
Cyanides
synthesis
Rhenium
Ligands
ligands
rhenium
Electrochemical properties
triangles
boiling
Boiling liquids
electron transfer
Nuclear magnetic resonance
Single crystals
Crystalline materials
Infrared radiation
X ray diffraction
Atoms

ASJC Scopus subject areas

  • Inorganic Chemistry
  • Organic Chemistry

Cite this

Song, H., Lee, Y., Choi, Z. H., Lee, K., Park, J. T., Kwak, J., & Choi, M. G. (2001). Synthesis and characterization of μ3222- C60 trirhenium hydrido cluster complexes. Organometallics, 20(14), 3139-3144. https://doi.org/10.1021/om0101341

Synthesis and characterization of μ3222- C60 trirhenium hydrido cluster complexes. / Song, Hyunjoon; Lee, Yumi; Choi, Zel Ho; Lee, Kwangyeol; Park, Joon T.; Kwak, Juhyoun; Choi, Moon Gun.

In: Organometallics, Vol. 20, No. 14, 09.07.2001, p. 3139-3144.

Research output: Contribution to journalArticle

Song, H, Lee, Y, Choi, ZH, Lee, K, Park, JT, Kwak, J & Choi, MG 2001, 'Synthesis and characterization of μ3222- C60 trirhenium hydrido cluster complexes', Organometallics, vol. 20, no. 14, pp. 3139-3144. https://doi.org/10.1021/om0101341
Song, Hyunjoon ; Lee, Yumi ; Choi, Zel Ho ; Lee, Kwangyeol ; Park, Joon T. ; Kwak, Juhyoun ; Choi, Moon Gun. / Synthesis and characterization of μ3222- C60 trirhenium hydrido cluster complexes. In: Organometallics. 2001 ; Vol. 20, No. 14. pp. 3139-3144.
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title = "Synthesis and characterization of μ3-η2,η2,η2- C60 trirhenium hydrido cluster complexes",
abstract = "The reaction of C60 with Re3(μ-H)3(CO)11(NCMe) in refluxing chlorobenzene produces Re3(μ-H)3(CO)9(μ3- η2,η2,η2-C60) (1) in 50{\%} yield. Initial decarbonylation of 1 with Me3NO/MeCN followed by reaction with PPh3 in boiling chlorobenzene affords Re3(μ-H)3(CO)8(PPh3)- (μ3-η2,η2,η2- C60) (2) in a low yield (26{\%}). Treatment of 1 with PhCH2N=PPh3 at room temperature gives a benzyl isocyanide substituted product Re3(μ-H)3(CO)8(CNCH2Ph) (μ3 η2,η2,η2-C60) (3) in 53{\%} yield. Compounds 1, 2, and 3 have been isolated as crystalline solids and characterized by spectroscopic (infrared, mass, 1H, 31P, and 13C NMR) and analytical data. The structure of 3 has been determined by a single-crystal X-ray diffraction study. The C60 ligand is coordinated to the trirhenium triangle in a μ3-η2,η2,η2 bonding mode, and the benzyl isocyanide ligand occupies an axial position of a rhenium atom. Electrochemical properties of 1 and 2 have been studied by cyclic voltammetry (CV) in chlorobenzene (CB) solutions. The general features of CV curves have revealed four reversible redox couples for 1 and 2 in the CB potential window. The CV results suggest that a C60-mediated electron transfer to the trirhenium center takes place in 12- species for 1 and 23- for 2.",
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AU - Park, Joon T.

AU - Kwak, Juhyoun

AU - Choi, Moon Gun

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N2 - The reaction of C60 with Re3(μ-H)3(CO)11(NCMe) in refluxing chlorobenzene produces Re3(μ-H)3(CO)9(μ3- η2,η2,η2-C60) (1) in 50% yield. Initial decarbonylation of 1 with Me3NO/MeCN followed by reaction with PPh3 in boiling chlorobenzene affords Re3(μ-H)3(CO)8(PPh3)- (μ3-η2,η2,η2- C60) (2) in a low yield (26%). Treatment of 1 with PhCH2N=PPh3 at room temperature gives a benzyl isocyanide substituted product Re3(μ-H)3(CO)8(CNCH2Ph) (μ3 η2,η2,η2-C60) (3) in 53% yield. Compounds 1, 2, and 3 have been isolated as crystalline solids and characterized by spectroscopic (infrared, mass, 1H, 31P, and 13C NMR) and analytical data. The structure of 3 has been determined by a single-crystal X-ray diffraction study. The C60 ligand is coordinated to the trirhenium triangle in a μ3-η2,η2,η2 bonding mode, and the benzyl isocyanide ligand occupies an axial position of a rhenium atom. Electrochemical properties of 1 and 2 have been studied by cyclic voltammetry (CV) in chlorobenzene (CB) solutions. The general features of CV curves have revealed four reversible redox couples for 1 and 2 in the CB potential window. The CV results suggest that a C60-mediated electron transfer to the trirhenium center takes place in 12- species for 1 and 23- for 2.

AB - The reaction of C60 with Re3(μ-H)3(CO)11(NCMe) in refluxing chlorobenzene produces Re3(μ-H)3(CO)9(μ3- η2,η2,η2-C60) (1) in 50% yield. Initial decarbonylation of 1 with Me3NO/MeCN followed by reaction with PPh3 in boiling chlorobenzene affords Re3(μ-H)3(CO)8(PPh3)- (μ3-η2,η2,η2- C60) (2) in a low yield (26%). Treatment of 1 with PhCH2N=PPh3 at room temperature gives a benzyl isocyanide substituted product Re3(μ-H)3(CO)8(CNCH2Ph) (μ3 η2,η2,η2-C60) (3) in 53% yield. Compounds 1, 2, and 3 have been isolated as crystalline solids and characterized by spectroscopic (infrared, mass, 1H, 31P, and 13C NMR) and analytical data. The structure of 3 has been determined by a single-crystal X-ray diffraction study. The C60 ligand is coordinated to the trirhenium triangle in a μ3-η2,η2,η2 bonding mode, and the benzyl isocyanide ligand occupies an axial position of a rhenium atom. Electrochemical properties of 1 and 2 have been studied by cyclic voltammetry (CV) in chlorobenzene (CB) solutions. The general features of CV curves have revealed four reversible redox couples for 1 and 2 in the CB potential window. The CV results suggest that a C60-mediated electron transfer to the trirhenium center takes place in 12- species for 1 and 23- for 2.

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