Synthesis and characterization of (η3-CPh3)Re(CO)4, a thermal precursor for generation of the Re(CO)5 radical

Lisa S. Crocke, Bruce M. Mattson, D. Michael Heinekey, Gayle K. Schulte

Research output: Contribution to journalArticle

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Abstract

Reaction of NaRe(CO)5 with Ph3CPF6 affords Re(CO)43-CPh3) (1). Complex 1 reacts readily with CO at room temperature to give the Re(CO)5 radical, which forms Re2(CO)10 in the absence of trapping agents. The radical reacts with CCl4 to give Re(CO)5Cl and with Fe(CO)5 to give Re2Fe(CO)14 (2). Compounds 1 and 2 have been structurally characterized. Compound 1 crystallizes in the triclinic space group P1 with lattice parameters a = 11.062 (2) Å, b = 11.383 (1) Å, c = 17.961 (3) Å, α = 104.62 (1)°, γ = 94.77 (2)°, and γ = 98.52 (1)°. The final R value was 3.7%. The structure shows a Re(CO)4 moiety coordinated to the central carbon of the triphenylmethyl unit and two carbons of one phenyl ring. Complex 2 crystallizes in the monoclinic space group C2/m with lattice parameters a = 12.083 (3) Å, b = 14.705 (4) Å, c = 11.822 (3) Å, and β = 97.43 (2)°. The final R value was 3.4%. The structure shows a linear Re-Fe-Re array.

Original languageEnglish
Pages (from-to)3722-3725
Number of pages4
JournalInorganic Chemistry
Volume27
Issue number21
StatePublished - 1988
Externally publishedYes

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Carbon Monoxide
lattice parameters
carbon
synthesis
trapping
rings
room temperature
Lattice constants
Carbon
Hot Temperature

All Science Journal Classification (ASJC) codes

  • Inorganic Chemistry

Cite this

Synthesis and characterization of (η3-CPh3)Re(CO)4, a thermal precursor for generation of the Re(CO)5 radical. / Crocke, Lisa S.; Mattson, Bruce M.; Michael Heinekey, D.; Schulte, Gayle K.

In: Inorganic Chemistry, Vol. 27, No. 21, 1988, p. 3722-3725.

Research output: Contribution to journalArticle

Crocke, Lisa S. ; Mattson, Bruce M. ; Michael Heinekey, D. ; Schulte, Gayle K. / Synthesis and characterization of (η3-CPh3)Re(CO)4, a thermal precursor for generation of the Re(CO)5 radical. In: Inorganic Chemistry. 1988 ; Vol. 27, No. 21. pp. 3722-3725.
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title = "Synthesis and characterization of (η3-CPh3)Re(CO)4, a thermal precursor for generation of the Re(CO)5 radical",
abstract = "Reaction of NaRe(CO)5 with Ph3CPF6 affords Re(CO)4(η3-CPh3) (1). Complex 1 reacts readily with CO at room temperature to give the •Re(CO)5 radical, which forms Re2(CO)10 in the absence of trapping agents. The radical reacts with CCl4 to give Re(CO)5Cl and with Fe(CO)5 to give Re2Fe(CO)14 (2). Compounds 1 and 2 have been structurally characterized. Compound 1 crystallizes in the triclinic space group P1 with lattice parameters a = 11.062 (2) {\AA}, b = 11.383 (1) {\AA}, c = 17.961 (3) {\AA}, α = 104.62 (1)°, γ = 94.77 (2)°, and γ = 98.52 (1)°. The final R value was 3.7{\%}. The structure shows a Re(CO)4 moiety coordinated to the central carbon of the triphenylmethyl unit and two carbons of one phenyl ring. Complex 2 crystallizes in the monoclinic space group C2/m with lattice parameters a = 12.083 (3) {\AA}, b = 14.705 (4) {\AA}, c = 11.822 (3) {\AA}, and β = 97.43 (2)°. The final R value was 3.4{\%}. The structure shows a linear Re-Fe-Re array.",
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T1 - Synthesis and characterization of (η3-CPh3)Re(CO)4, a thermal precursor for generation of the Re(CO)5 radical

AU - Crocke, Lisa S.

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AU - Michael Heinekey, D.

AU - Schulte, Gayle K.

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N2 - Reaction of NaRe(CO)5 with Ph3CPF6 affords Re(CO)4(η3-CPh3) (1). Complex 1 reacts readily with CO at room temperature to give the •Re(CO)5 radical, which forms Re2(CO)10 in the absence of trapping agents. The radical reacts with CCl4 to give Re(CO)5Cl and with Fe(CO)5 to give Re2Fe(CO)14 (2). Compounds 1 and 2 have been structurally characterized. Compound 1 crystallizes in the triclinic space group P1 with lattice parameters a = 11.062 (2) Å, b = 11.383 (1) Å, c = 17.961 (3) Å, α = 104.62 (1)°, γ = 94.77 (2)°, and γ = 98.52 (1)°. The final R value was 3.7%. The structure shows a Re(CO)4 moiety coordinated to the central carbon of the triphenylmethyl unit and two carbons of one phenyl ring. Complex 2 crystallizes in the monoclinic space group C2/m with lattice parameters a = 12.083 (3) Å, b = 14.705 (4) Å, c = 11.822 (3) Å, and β = 97.43 (2)°. The final R value was 3.4%. The structure shows a linear Re-Fe-Re array.

AB - Reaction of NaRe(CO)5 with Ph3CPF6 affords Re(CO)4(η3-CPh3) (1). Complex 1 reacts readily with CO at room temperature to give the •Re(CO)5 radical, which forms Re2(CO)10 in the absence of trapping agents. The radical reacts with CCl4 to give Re(CO)5Cl and with Fe(CO)5 to give Re2Fe(CO)14 (2). Compounds 1 and 2 have been structurally characterized. Compound 1 crystallizes in the triclinic space group P1 with lattice parameters a = 11.062 (2) Å, b = 11.383 (1) Å, c = 17.961 (3) Å, α = 104.62 (1)°, γ = 94.77 (2)°, and γ = 98.52 (1)°. The final R value was 3.7%. The structure shows a Re(CO)4 moiety coordinated to the central carbon of the triphenylmethyl unit and two carbons of one phenyl ring. Complex 2 crystallizes in the monoclinic space group C2/m with lattice parameters a = 12.083 (3) Å, b = 14.705 (4) Å, c = 11.822 (3) Å, and β = 97.43 (2)°. The final R value was 3.4%. The structure shows a linear Re-Fe-Re array.

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