A comparative study of the isomers of ReOCl3(PMe3)2 and ReOCl3(PEt3)2. The isolation and characterization of ReH7(PR3)2 and ReO(OEt)Cl2(PR3)2 (R = Me or Et) and the photoelectron spectrum of ReH7(PMe3)2

Kimberly J. Smith, Andrea L. Ondracek, Nadine E. Gruhn, Dennis L Lichtenberger, Phillip E. Fanwick, Richard A. Walton

Research output: Contribution to journalArticle

13 Citations (Scopus)

Abstract

The reactions of mer-trans-ReOCl3(PPh3)2 with PMe3 and PEt3 provide a route to the isomers fac-cis-ReOCl3(PR3)2 and mer-trans-ReOCl3(PR3)2 (R = Me or Et) which can be converted to ReH7(PR3)2 (R = Me or Et) in ca. 60% yield by reaction with LiAlH4 in THF and subsequent hydrolysis of the reaction mixtures. The properties of these heptahydrides have been examined, including studies of the remarkable stability of aqueous solutions of ReH7(PMe3)2 and the measurement of the gas-phase He(I) photoelectron spectrum of this complex. While the fac-cis and mer-trans isomers of ReOCl3(PR3)2 (R = Me or Et) do not convert to ReO(OEt)Cl2(PR3)2 upon reaction with ethanol, these ethoxides can be prepared by the reaction of mer-trans-ReO(OEt)Cl2(PPh3)2 with PMe3 and PEt3. The reactions of the isomers of ReOCl3(PMe3)2 with ethylamine, followed by the treatment of the reaction products with acetone, afford the salt [Me3PCMe2CH2C(O)CH3]ReO4. The compounds fac-cis-ReOCl3(PEt3)2, trans-ReO(OEt)Cl2(PMe3)2 and [Me3PCMe2CH2C(O)CH3]ReO4 have been structurally characterized by X-ray crystallography. (C) 2000 Elsevier Science S.A.

Original languageEnglish (US)
Pages (from-to)23-31
Number of pages9
JournalInorganica Chimica Acta
Volume300-302
DOIs
StatePublished - Apr 30 2000

Fingerprint

X Ray Crystallography
Photoelectrons
Acetone
Isomers
isolation
photoelectrons
Hydrolysis
Ethanol
isomers
Salts
Gases
X ray crystallography
Reaction products
reaction products
acetone
crystallography
hydrolysis
lithium aluminum hydride
ethylamine
ethyl alcohol

Keywords

  • Alkoxide complexes
  • Crystal structures
  • Oxorhenium complexes
  • Photoelectron spectroscopy
  • Rhenium polyhydrides

ASJC Scopus subject areas

  • Biochemistry
  • Inorganic Chemistry
  • Physical and Theoretical Chemistry
  • Materials Chemistry

Cite this

A comparative study of the isomers of ReOCl3(PMe3)2 and ReOCl3(PEt3)2. The isolation and characterization of ReH7(PR3)2 and ReO(OEt)Cl2(PR3)2 (R = Me or Et) and the photoelectron spectrum of ReH7(PMe3)2. / Smith, Kimberly J.; Ondracek, Andrea L.; Gruhn, Nadine E.; Lichtenberger, Dennis L; Fanwick, Phillip E.; Walton, Richard A.

In: Inorganica Chimica Acta, Vol. 300-302, 30.04.2000, p. 23-31.

Research output: Contribution to journalArticle

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title = "A comparative study of the isomers of ReOCl3(PMe3)2 and ReOCl3(PEt3)2. The isolation and characterization of ReH7(PR3)2 and ReO(OEt)Cl2(PR3)2 (R = Me or Et) and the photoelectron spectrum of ReH7(PMe3)2",
abstract = "The reactions of mer-trans-ReOCl3(PPh3)2 with PMe3 and PEt3 provide a route to the isomers fac-cis-ReOCl3(PR3)2 and mer-trans-ReOCl3(PR3)2 (R = Me or Et) which can be converted to ReH7(PR3)2 (R = Me or Et) in ca. 60{\%} yield by reaction with LiAlH4 in THF and subsequent hydrolysis of the reaction mixtures. The properties of these heptahydrides have been examined, including studies of the remarkable stability of aqueous solutions of ReH7(PMe3)2 and the measurement of the gas-phase He(I) photoelectron spectrum of this complex. While the fac-cis and mer-trans isomers of ReOCl3(PR3)2 (R = Me or Et) do not convert to ReO(OEt)Cl2(PR3)2 upon reaction with ethanol, these ethoxides can be prepared by the reaction of mer-trans-ReO(OEt)Cl2(PPh3)2 with PMe3 and PEt3. The reactions of the isomers of ReOCl3(PMe3)2 with ethylamine, followed by the treatment of the reaction products with acetone, afford the salt [Me3PCMe2CH2C(O)CH3]ReO4. The compounds fac-cis-ReOCl3(PEt3)2, trans-ReO(OEt)Cl2(PMe3)2 and [Me3PCMe2CH2C(O)CH3]ReO4 have been structurally characterized by X-ray crystallography. (C) 2000 Elsevier Science S.A.",
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T1 - A comparative study of the isomers of ReOCl3(PMe3)2 and ReOCl3(PEt3)2. The isolation and characterization of ReH7(PR3)2 and ReO(OEt)Cl2(PR3)2 (R = Me or Et) and the photoelectron spectrum of ReH7(PMe3)2

AU - Smith, Kimberly J.

AU - Ondracek, Andrea L.

AU - Gruhn, Nadine E.

AU - Lichtenberger, Dennis L

AU - Fanwick, Phillip E.

AU - Walton, Richard A.

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N2 - The reactions of mer-trans-ReOCl3(PPh3)2 with PMe3 and PEt3 provide a route to the isomers fac-cis-ReOCl3(PR3)2 and mer-trans-ReOCl3(PR3)2 (R = Me or Et) which can be converted to ReH7(PR3)2 (R = Me or Et) in ca. 60% yield by reaction with LiAlH4 in THF and subsequent hydrolysis of the reaction mixtures. The properties of these heptahydrides have been examined, including studies of the remarkable stability of aqueous solutions of ReH7(PMe3)2 and the measurement of the gas-phase He(I) photoelectron spectrum of this complex. While the fac-cis and mer-trans isomers of ReOCl3(PR3)2 (R = Me or Et) do not convert to ReO(OEt)Cl2(PR3)2 upon reaction with ethanol, these ethoxides can be prepared by the reaction of mer-trans-ReO(OEt)Cl2(PPh3)2 with PMe3 and PEt3. The reactions of the isomers of ReOCl3(PMe3)2 with ethylamine, followed by the treatment of the reaction products with acetone, afford the salt [Me3PCMe2CH2C(O)CH3]ReO4. The compounds fac-cis-ReOCl3(PEt3)2, trans-ReO(OEt)Cl2(PMe3)2 and [Me3PCMe2CH2C(O)CH3]ReO4 have been structurally characterized by X-ray crystallography. (C) 2000 Elsevier Science S.A.

AB - The reactions of mer-trans-ReOCl3(PPh3)2 with PMe3 and PEt3 provide a route to the isomers fac-cis-ReOCl3(PR3)2 and mer-trans-ReOCl3(PR3)2 (R = Me or Et) which can be converted to ReH7(PR3)2 (R = Me or Et) in ca. 60% yield by reaction with LiAlH4 in THF and subsequent hydrolysis of the reaction mixtures. The properties of these heptahydrides have been examined, including studies of the remarkable stability of aqueous solutions of ReH7(PMe3)2 and the measurement of the gas-phase He(I) photoelectron spectrum of this complex. While the fac-cis and mer-trans isomers of ReOCl3(PR3)2 (R = Me or Et) do not convert to ReO(OEt)Cl2(PR3)2 upon reaction with ethanol, these ethoxides can be prepared by the reaction of mer-trans-ReO(OEt)Cl2(PPh3)2 with PMe3 and PEt3. The reactions of the isomers of ReOCl3(PMe3)2 with ethylamine, followed by the treatment of the reaction products with acetone, afford the salt [Me3PCMe2CH2C(O)CH3]ReO4. The compounds fac-cis-ReOCl3(PEt3)2, trans-ReO(OEt)Cl2(PMe3)2 and [Me3PCMe2CH2C(O)CH3]ReO4 have been structurally characterized by X-ray crystallography. (C) 2000 Elsevier Science S.A.

KW - Alkoxide complexes

KW - Crystal structures

KW - Oxorhenium complexes

KW - Photoelectron spectroscopy

KW - Rhenium polyhydrides

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