Characterization of [Re2Cl3(μ-dppm)2(NCCH3) 2][Cl] and [Re2Cl3(μ-dppm)2(NCC6H 5)2][Cl] · 2CH2Cl2 by X-ray Crystallographic and Two-Dimensional NMR Spectroscopic Techniques

Thomas E. Concolino; Judith L. Eglin; Chad E. Hadden; Rickey P. Hicks; Richard J. Staples; Edward J. Valente; Jeffrey D. Zubkowski

doi:10.1023/A:1009012731250

Characterization of [Re₂Cl₃(μ-dppm)₂(NCCH₃) ₂][Cl] and [Re₂Cl₃(μ-dppm)₂(NCC₆H ₅)₂][Cl] · 2CH₂Cl₂ by X-ray Crystallographic and Two-Dimensional NMR Spectroscopic Techniques

Thomas E. Concolino, Judith L. Eglin, Chad E. Hadden, Rickey P. Hicks, Richard J. Staples, Edward J. Valente, Jeffrey D. Zubkowski

Biochemistry and Molecular Biology

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

1 Scopus citations

Abstract

The complex Re₂Cl₆(P-n-Bu₃)₂ prepared in situ reacts with CH₃CN to form a blue-green solution. Addition of the chelating phosphine bis(diphenylphosphino)methane (dppm) results in the formation of the complex [Re₂Cl₃(μ-dppm)₂(NCCH₃) ₂][Cl] (1) upon heating. The two acetonitrile molecules adopt a trans geometry on the rhenium center with the axially coordinated chlorine. The analogous trans benzonitrile species [Re₂Cl₃(μ-dppm)₂(NCC₆H ₅)₂][Cl] · 2CH₂Cl₂ (2) is synthesized under the same reaction conditions. The coupling constants of the AA′BB′ ³¹P{¹H} NMR spectra of the compounds were elucidated from ³¹P-³¹P homonuclear J-resolved NMR experiments. Additional characterization methods include ³¹P{¹H} NMR spectroscopy, UV-vis spectroscopy, and X-ray crystallography.

Original language	English (US)
Pages (from-to)	109-123
Number of pages	15
Journal	Journal of Cluster Science
Volume	11
Issue number	1
DOIs	https://doi.org/10.1023/A:1009012731250
State	Published - 2000

Keywords

Metal-metal bonds
Two-dimensional homonuclear J-resolved NMR spectroscopy

ASJC Scopus subject areas

Biochemistry
Chemistry(all)
Materials Science(all)
Condensed Matter Physics

Access to Document

10.1023/A:1009012731250

Cite this

Concolino, T. E., Eglin, J. L., Hadden, C. E., Hicks, R. P., Staples, R. J., Valente, E. J., & Zubkowski, J. D. (2000). Characterization of [Re₂Cl₃(μ-dppm)₂(NCCH₃) ₂][Cl] and [Re₂Cl₃(μ-dppm)₂(NCC₆H ₅)₂][Cl] · 2CH₂Cl₂ by X-ray Crystallographic and Two-Dimensional NMR Spectroscopic Techniques. Journal of Cluster Science, 11(1), 109-123. https://doi.org/10.1023/A:1009012731250

Characterization of [Re₂Cl₃(μ-dppm)₂(NCCH₃) ₂][Cl] and [Re₂Cl₃(μ-dppm)₂(NCC₆H ₅)₂][Cl] · 2CH₂Cl₂ by X-ray Crystallographic and Two-Dimensional NMR Spectroscopic Techniques. / Concolino, Thomas E.; Eglin, Judith L.; Hadden, Chad E. et al.
In: Journal of Cluster Science, Vol. 11, No. 1, 2000, p. 109-123.

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

Concolino, TE, Eglin, JL, Hadden, CE, Hicks, RP, Staples, RJ, Valente, EJ & Zubkowski, JD 2000, 'Characterization of [Re₂Cl₃(μ-dppm)₂(NCCH₃) ₂][Cl] and [Re₂Cl₃(μ-dppm)₂(NCC₆H ₅)₂][Cl] · 2CH₂Cl₂ by X-ray Crystallographic and Two-Dimensional NMR Spectroscopic Techniques', Journal of Cluster Science, vol. 11, no. 1, pp. 109-123. https://doi.org/10.1023/A:1009012731250

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title = "Characterization of [Re2Cl3(μ-dppm)2(NCCH3) 2][Cl] and [Re2Cl3(μ-dppm)2(NCC6H 5)2][Cl] · 2CH2Cl2 by X-ray Crystallographic and Two-Dimensional NMR Spectroscopic Techniques",

abstract = "The complex Re2Cl6(P-n-Bu3)2 prepared in situ reacts with CH3CN to form a blue-green solution. Addition of the chelating phosphine bis(diphenylphosphino)methane (dppm) results in the formation of the complex [Re2Cl3(μ-dppm)2(NCCH3) 2][Cl] (1) upon heating. The two acetonitrile molecules adopt a trans geometry on the rhenium center with the axially coordinated chlorine. The analogous trans benzonitrile species [Re2Cl3(μ-dppm)2(NCC6H 5)2][Cl] · 2CH2Cl2 (2) is synthesized under the same reaction conditions. The coupling constants of the AA′BB′ 31P{1H} NMR spectra of the compounds were elucidated from 31P-31P homonuclear J-resolved NMR experiments. Additional characterization methods include 31P{1H} NMR spectroscopy, UV-vis spectroscopy, and X-ray crystallography.",

keywords = "Metal-metal bonds, Two-dimensional homonuclear J-resolved NMR spectroscopy",

author = "Concolino, {Thomas E.} and Eglin, {Judith L.} and Hadden, {Chad E.} and Hicks, {Rickey P.} and Staples, {Richard J.} and Valente, {Edward J.} and Zubkowski, {Jeffrey D.}",

note = "Funding Information: Authors T. Concolino and J. Eglin would like to acknowledge the Donors of The Petroleum Research Fund, administered by the American Chemical Society, for the partial support of this research and NSF Grant * CHE-9630192. NMR measurements were made at the Mississippi Magnetic Resonance Facility at Mississippi State University, supported by the National Science Foundation and Mississippi State University. Author R. Hicks would like to acknowledge Alan Deese for his technical assistance. Authors E. Valente and J. Zubkowski acknowledge the support of the Office of Naval Research.",

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doi = "10.1023/A:1009012731250",

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T1 - Characterization of [Re2Cl3(μ-dppm)2(NCCH3) 2][Cl] and [Re2Cl3(μ-dppm)2(NCC6H 5)2][Cl] · 2CH2Cl2 by X-ray Crystallographic and Two-Dimensional NMR Spectroscopic Techniques

AU - Concolino, Thomas E.

AU - Eglin, Judith L.

AU - Hadden, Chad E.

AU - Hicks, Rickey P.

AU - Staples, Richard J.

AU - Valente, Edward J.

AU - Zubkowski, Jeffrey D.

N1 - Funding Information: Authors T. Concolino and J. Eglin would like to acknowledge the Donors of The Petroleum Research Fund, administered by the American Chemical Society, for the partial support of this research and NSF Grant * CHE-9630192. NMR measurements were made at the Mississippi Magnetic Resonance Facility at Mississippi State University, supported by the National Science Foundation and Mississippi State University. Author R. Hicks would like to acknowledge Alan Deese for his technical assistance. Authors E. Valente and J. Zubkowski acknowledge the support of the Office of Naval Research.

PY - 2000

Y1 - 2000

N2 - The complex Re2Cl6(P-n-Bu3)2 prepared in situ reacts with CH3CN to form a blue-green solution. Addition of the chelating phosphine bis(diphenylphosphino)methane (dppm) results in the formation of the complex [Re2Cl3(μ-dppm)2(NCCH3) 2][Cl] (1) upon heating. The two acetonitrile molecules adopt a trans geometry on the rhenium center with the axially coordinated chlorine. The analogous trans benzonitrile species [Re2Cl3(μ-dppm)2(NCC6H 5)2][Cl] · 2CH2Cl2 (2) is synthesized under the same reaction conditions. The coupling constants of the AA′BB′ 31P{1H} NMR spectra of the compounds were elucidated from 31P-31P homonuclear J-resolved NMR experiments. Additional characterization methods include 31P{1H} NMR spectroscopy, UV-vis spectroscopy, and X-ray crystallography.

AB - The complex Re2Cl6(P-n-Bu3)2 prepared in situ reacts with CH3CN to form a blue-green solution. Addition of the chelating phosphine bis(diphenylphosphino)methane (dppm) results in the formation of the complex [Re2Cl3(μ-dppm)2(NCCH3) 2][Cl] (1) upon heating. The two acetonitrile molecules adopt a trans geometry on the rhenium center with the axially coordinated chlorine. The analogous trans benzonitrile species [Re2Cl3(μ-dppm)2(NCC6H 5)2][Cl] · 2CH2Cl2 (2) is synthesized under the same reaction conditions. The coupling constants of the AA′BB′ 31P{1H} NMR spectra of the compounds were elucidated from 31P-31P homonuclear J-resolved NMR experiments. Additional characterization methods include 31P{1H} NMR spectroscopy, UV-vis spectroscopy, and X-ray crystallography.

KW - Metal-metal bonds

KW - Two-dimensional homonuclear J-resolved NMR spectroscopy

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