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

Research output: Contribution to journalArticle

1 Citation (Scopus)

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 languageEnglish (US)
Pages (from-to)109-123
Number of pages15
JournalJournal of Cluster Science
Volume11
Issue number1
DOIs
StatePublished - Jan 1 2000

Fingerprint

Methane
phosphine
methane
Nuclear magnetic resonance
X-Rays
X rays
nuclear magnetic resonance
Rhenium
x rays
X ray crystallography
X Ray Crystallography
Chlorine
rhenium
Chelation
Ultraviolet spectroscopy
Acetonitrile
phosphines
Heating
spectroscopy
Nuclear magnetic resonance spectroscopy

Keywords

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

ASJC Scopus subject areas

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

Cite this

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.; Hicks, Rickey P.; Staples, Richard J.; Valente, Edward J.; Zubkowski, Jeffrey D.

In: Journal of Cluster Science, Vol. 11, No. 1, 01.01.2000, p. 109-123.

Research output: Contribution to journalArticle

Concolino, Thomas E. ; Eglin, Judith L. ; Hadden, Chad E. ; Hicks, Rickey P. ; Staples, Richard J. ; Valente, Edward J. ; Zubkowski, Jeffrey D. / 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. In: Journal of Cluster Science. 2000 ; Vol. 11, No. 1. pp. 109-123.
@article{01b0cc6180794c4f9988bbe7f8c43f48,
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.}",
year = "2000",
month = "1",
day = "1",
doi = "10.1023/A:1009012731250",
language = "English (US)",
volume = "11",
pages = "109--123",
journal = "Journal of Cluster Science",
issn = "1040-7278",
publisher = "Springer New York",
number = "1",

}

TY - JOUR

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.

PY - 2000/1/1

Y1 - 2000/1/1

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

UR - http://www.scopus.com/inward/record.url?scp=0034381074&partnerID=8YFLogxK

UR - http://www.scopus.com/inward/citedby.url?scp=0034381074&partnerID=8YFLogxK

U2 - 10.1023/A:1009012731250

DO - 10.1023/A:1009012731250

M3 - Article

AN - SCOPUS:0034381074

VL - 11

SP - 109

EP - 123

JO - Journal of Cluster Science

JF - Journal of Cluster Science

SN - 1040-7278

IS - 1

ER -