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

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

All Science Journal Classification (ASJC) codes

  • Physical and Theoretical Chemistry
  • Organic Chemistry
  • Inorganic 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
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.",
author = "Hyunjoon Song and Yumi Lee and Choi, {Zel Ho} and Kwangyeol Lee and Park, {Joon T.} and Juhyoun Kwak and Moon-Gun Choi",
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Song, H, Lee, Y, Choi, ZH, Lee, K, Park, JT, Kwak, J & Choi, M-G 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

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

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T1 - Synthesis and characterization of μ3-η2,η2,η2- C60 trirhenium hydrido cluster complexes

AU - Song, Hyunjoon

AU - Lee, Yumi

AU - Choi, Zel Ho

AU - Lee, Kwangyeol

AU - Park, Joon T.

AU - Kwak, Juhyoun

AU - Choi, Moon-Gun

PY - 2001/7/9

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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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