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

doi:10.1016/S0020-1693(99)00419-3

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

Chemistry and Biochemistry

Research output: Contribution to journal › Article › peer-review

12 Scopus citations

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 language	English (US)
Pages (from-to)	23-31
Number of pages	9
Journal	Inorganica Chimica Acta
Volume	300-302
DOIs	https://doi.org/10.1016/S0020-1693(99)00419-3
State	Published - Apr 30 2000

Keywords

Alkoxide complexes
Crystal structures
Oxorhenium complexes
Photoelectron spectroscopy
Rhenium polyhydrides

ASJC Scopus subject areas

Physical and Theoretical Chemistry
Inorganic Chemistry
Materials Chemistry

Access to Document

10.1016/S0020-1693(99)00419-3

Cite this

Smith, K. J., Ondracek, A. L., Gruhn, N. E., Lichtenberger, D. L., Fanwick, P. E., & Walton, R. A. (2000). 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. Inorganica Chimica Acta, 300-302, 23-31. https://doi.org/10.1016/S0020-1693(99)00419-3

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

Research output: Contribution to journal › Article › peer-review

Smith, KJ, Ondracek, AL, Gruhn, NE, Lichtenberger, DL, Fanwick, PE & Walton, RA 2000, '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', Inorganica Chimica Acta, vol. 300-302, pp. 23-31. https://doi.org/10.1016/S0020-1693(99)00419-3

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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.",

keywords = "Alkoxide complexes, Crystal structures, Oxorhenium complexes, Photoelectron spectroscopy, Rhenium polyhydrides",

author = "Smith, {Kimberly J.} and Ondracek, {Andrea L.} and Gruhn, {Nadine E.} and Lichtenberger, {Dennis L.} and Fanwick, {Phillip E.} and Walton, {Richard 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.

PY - 2000/4/30

Y1 - 2000/4/30

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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