Synthesis and characterization of the trihalophosphine compounds of ruthenium [RuX2(η6-cymene)(PY3)] (X = Cl, Br, Y = F, Cl, Br) and the related PF2(NMe2) and P(NMe2)3 compounds; multinuclear NMR spectroscopy and the X-ray single crystal structures of [RuBr2(η6-cymene) (PF3)]...

Ahmed M.A. Boshaala; Stephen J. Simpson; Jochen Autschbach; Shaohui Zheng

doi:10.1021/ic800611h

Synthesis and characterization of the trihalophosphine compounds of ruthenium [RuX₂(η⁶-cymene)(PY₃)] (X = Cl, Br, Y = F, Cl, Br) and the related PF₂(NMe₂) and P(NMe₂)₃ compounds; multinuclear NMR spectroscopy and the X-ray single crystal structures of [RuBr₂(η⁶-cymene) (PF₃)]...

Ahmed M.A. Boshaala
, Stephen J. Simpson
, Jochen Autschbach
, Shaohui Zheng

Chemistry

University of Salford
University of Exeter
SUNY Buffalo

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

16 Scopus citations

Abstract

Full title: Synthesis and characterization of the trihalophosphine compounds of ruthenium [RuX₂(η⁶-cymene)(PY₃)] (X = Cl, Br, Y = F, Cl, Br) and the related PF₂(NMe₂) and P(NMe₂)₃ compounds; multinuclear NMR spectroscopy and the X-ray single crystal structures of [RuBr₂(η⁶-cymene) (PF₃)], [RuBr₂(η⁶-cymene)(PF ₂{NMe₂})]. Treatment of the dimers [RuX₂(η⁶-cymene)] ₂ with PF₃ in hot heptane produces the compounds [RuX ₂(η⁶-cymene)(PF₃)] (X = Cl, Br, I) in good yield. Difluoro(dimethylamino)phosphine and tris(dimethylamino)phosphine react similarly to produce the compounds [RuX₂(η⁶-cymene) (PF₂{NMe₂})] and [RuX₂(η⁶- cymene)(P{NMe₂}₃)]. Reaction of the dimers [RuX ₂(η⁶-cymene)]₂ with PCl₃ and PBr₃ proceeded with the production of mononuclear products which had undergone halogen exchange at ruthenium in some cases. ¹H, ¹³C, ³¹P, and ¹⁹F NMR spectra have been obtained where appropriate together with (¹H-¹H) correlation spectroscopy (COSY) and (¹³C-¹H)-HETCORR spectra of selected compounds. The variation of ¹J( ³¹P-¹⁹F) with the nature of the auxiliary ligand (X) in the PF₃ and PF₂(NMe₂) complexes has been examined both experimentally and computationally using a natural localized molecular orbital-natural bond order approach. The single crystal X-ray structure of [RuBr₂(η⁶-cymene)(PF₃)] has been determined at 223 K and those of [RuBr₂(η⁶- cymene)(PF₂{NMe₂})] and [RuI₂(η ⁶-cymene)(P{NMe₂}₃)] at 294 K.

Original language	English
Pages (from-to)	9279-9292
Number of pages	14
Journal	Inorganic Chemistry
Volume	47
Issue number	20
DOIs	https://doi.org/10.1021/ic800611h
State	Published - Oct 20 2008

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Boshaala, A. M. A., Simpson, S. J., Autschbach, J., & Zheng, S. (2008). Synthesis and characterization of the trihalophosphine compounds of ruthenium [RuX₂(η⁶-cymene)(PY₃)] (X = Cl, Br, Y = F, Cl, Br) and the related PF₂(NMe₂) and P(NMe₂)₃ compounds; multinuclear NMR spectroscopy and the X-ray single crystal structures of [RuBr₂(η⁶-cymene) (PF₃)]... Inorganic Chemistry, 47(20), 9279-9292. https://doi.org/10.1021/ic800611h

Boshaala, Ahmed M.A. ; Simpson, Stephen J. ; Autschbach, Jochen et al. / Synthesis and characterization of the trihalophosphine compounds of ruthenium [RuX₂(η⁶-cymene)(PY₃)] (X = Cl, Br, Y = F, Cl, Br) and the related PF₂(NMe₂) and P(NMe₂)₃ compounds; multinuclear NMR spectroscopy and the X-ray single crystal structures of [RuBr₂(η⁶-cymene) (PF₃)]... In: Inorganic Chemistry. 2008 ; Vol. 47, No. 20. pp. 9279-9292.

@article{2c2bcaaa72c649f4a170cff2af1e45ed,

title = "Synthesis and characterization of the trihalophosphine compounds of ruthenium [RuX2(η6-cymene)(PY3)] (X = Cl, Br, Y = F, Cl, Br) and the related PF2(NMe2) and P(NMe2)3 compounds; multinuclear NMR spectroscopy and the X-ray single crystal structures of [RuBr2(η6-cymene) (PF3)]...",

abstract = "Full title: Synthesis and characterization of the trihalophosphine compounds of ruthenium [RuX2(η6-cymene)(PY3)] (X = Cl, Br, Y = F, Cl, Br) and the related PF2(NMe2) and P(NMe2)3 compounds; multinuclear NMR spectroscopy and the X-ray single crystal structures of [RuBr2(η6-cymene) (PF3)], [RuBr2(η6-cymene)(PF 2\{NMe2\})]. Treatment of the dimers [RuX2(η6-cymene)] 2 with PF3 in hot heptane produces the compounds [RuX 2(η6-cymene)(PF3)] (X = Cl, Br, I) in good yield. Difluoro(dimethylamino)phosphine and tris(dimethylamino)phosphine react similarly to produce the compounds [RuX2(η6-cymene) (PF2\{NMe2\})] and [RuX2(η6- cymene)(P\{NMe2\}3)]. Reaction of the dimers [RuX 2(η6-cymene)]2 with PCl3 and PBr3 proceeded with the production of mononuclear products which had undergone halogen exchange at ruthenium in some cases. 1H, 13C, 31P, and 19F NMR spectra have been obtained where appropriate together with (1H-1H) correlation spectroscopy (COSY) and (13C-1H)-HETCORR spectra of selected compounds. The variation of 1J( 31P-19F) with the nature of the auxiliary ligand (X) in the PF3 and PF2(NMe2) complexes has been examined both experimentally and computationally using a natural localized molecular orbital-natural bond order approach. The single crystal X-ray structure of [RuBr2(η6-cymene)(PF3)] has been determined at 223 K and those of [RuBr2(η6- cymene)(PF2\{NMe2\})] and [RuI2(η 6-cymene)(P\{NMe2\}3)] at 294 K.",

author = "Boshaala, \{Ahmed M.A.\} and Simpson, \{Stephen J.\} and Jochen Autschbach and Shaohui Zheng",

year = "2008",

month = oct,

day = "20",

doi = "10.1021/ic800611h",

language = "English",

volume = "47",

pages = "9279--9292",

journal = "Inorganic Chemistry",

issn = "0020-1669",

publisher = "American Chemical Society",

number = "20",

}

Boshaala, AMA, Simpson, SJ, Autschbach, J & Zheng, S 2008, 'Synthesis and characterization of the trihalophosphine compounds of ruthenium [RuX₂(η⁶-cymene)(PY₃)] (X = Cl, Br, Y = F, Cl, Br) and the related PF₂(NMe₂) and P(NMe₂)₃ compounds; multinuclear NMR spectroscopy and the X-ray single crystal structures of [RuBr₂(η⁶-cymene) (PF₃)]...', Inorganic Chemistry, vol. 47, no. 20, pp. 9279-9292. https://doi.org/10.1021/ic800611h

Synthesis and characterization of the trihalophosphine compounds of ruthenium [RuX₂(η⁶-cymene)(PY₃)] (X = Cl, Br, Y = F, Cl, Br) and the related PF₂(NMe₂) and P(NMe₂)₃ compounds; multinuclear NMR spectroscopy and the X-ray single crystal structures of [RuBr₂(η⁶-cymene) (PF₃)]... / Boshaala, Ahmed M.A.; Simpson, Stephen J.; Autschbach, Jochen et al.
In: Inorganic Chemistry, Vol. 47, No. 20, 20.10.2008, p. 9279-9292.

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

TY - JOUR

T1 - Synthesis and characterization of the trihalophosphine compounds of ruthenium [RuX2(η6-cymene)(PY3)] (X = Cl, Br, Y = F, Cl, Br) and the related PF2(NMe2) and P(NMe2)3 compounds; multinuclear NMR spectroscopy and the X-ray single crystal structures of [RuBr2(η6-cymene) (PF3)]...

AU - Boshaala, Ahmed M.A.

AU - Simpson, Stephen J.

AU - Autschbach, Jochen

AU - Zheng, Shaohui

PY - 2008/10/20

Y1 - 2008/10/20

N2 - Full title: Synthesis and characterization of the trihalophosphine compounds of ruthenium [RuX2(η6-cymene)(PY3)] (X = Cl, Br, Y = F, Cl, Br) and the related PF2(NMe2) and P(NMe2)3 compounds; multinuclear NMR spectroscopy and the X-ray single crystal structures of [RuBr2(η6-cymene) (PF3)], [RuBr2(η6-cymene)(PF 2{NMe2})]. Treatment of the dimers [RuX2(η6-cymene)] 2 with PF3 in hot heptane produces the compounds [RuX 2(η6-cymene)(PF3)] (X = Cl, Br, I) in good yield. Difluoro(dimethylamino)phosphine and tris(dimethylamino)phosphine react similarly to produce the compounds [RuX2(η6-cymene) (PF2{NMe2})] and [RuX2(η6- cymene)(P{NMe2}3)]. Reaction of the dimers [RuX 2(η6-cymene)]2 with PCl3 and PBr3 proceeded with the production of mononuclear products which had undergone halogen exchange at ruthenium in some cases. 1H, 13C, 31P, and 19F NMR spectra have been obtained where appropriate together with (1H-1H) correlation spectroscopy (COSY) and (13C-1H)-HETCORR spectra of selected compounds. The variation of 1J( 31P-19F) with the nature of the auxiliary ligand (X) in the PF3 and PF2(NMe2) complexes has been examined both experimentally and computationally using a natural localized molecular orbital-natural bond order approach. The single crystal X-ray structure of [RuBr2(η6-cymene)(PF3)] has been determined at 223 K and those of [RuBr2(η6- cymene)(PF2{NMe2})] and [RuI2(η 6-cymene)(P{NMe2}3)] at 294 K.

AB - Full title: Synthesis and characterization of the trihalophosphine compounds of ruthenium [RuX2(η6-cymene)(PY3)] (X = Cl, Br, Y = F, Cl, Br) and the related PF2(NMe2) and P(NMe2)3 compounds; multinuclear NMR spectroscopy and the X-ray single crystal structures of [RuBr2(η6-cymene) (PF3)], [RuBr2(η6-cymene)(PF 2{NMe2})]. Treatment of the dimers [RuX2(η6-cymene)] 2 with PF3 in hot heptane produces the compounds [RuX 2(η6-cymene)(PF3)] (X = Cl, Br, I) in good yield. Difluoro(dimethylamino)phosphine and tris(dimethylamino)phosphine react similarly to produce the compounds [RuX2(η6-cymene) (PF2{NMe2})] and [RuX2(η6- cymene)(P{NMe2}3)]. Reaction of the dimers [RuX 2(η6-cymene)]2 with PCl3 and PBr3 proceeded with the production of mononuclear products which had undergone halogen exchange at ruthenium in some cases. 1H, 13C, 31P, and 19F NMR spectra have been obtained where appropriate together with (1H-1H) correlation spectroscopy (COSY) and (13C-1H)-HETCORR spectra of selected compounds. The variation of 1J( 31P-19F) with the nature of the auxiliary ligand (X) in the PF3 and PF2(NMe2) complexes has been examined both experimentally and computationally using a natural localized molecular orbital-natural bond order approach. The single crystal X-ray structure of [RuBr2(η6-cymene)(PF3)] has been determined at 223 K and those of [RuBr2(η6- cymene)(PF2{NMe2})] and [RuI2(η 6-cymene)(P{NMe2}3)] at 294 K.

UR - https://www.scopus.com/pages/publications/55449096310

U2 - 10.1021/ic800611h

DO - 10.1021/ic800611h

M3 - Article

C2 - 18808107

AN - SCOPUS:55449096310

SN - 0020-1669

VL - 47

SP - 9279

EP - 9292

JO - Inorganic Chemistry

JF - Inorganic Chemistry

IS - 20

ER -

Boshaala AMA, Simpson SJ, Autschbach J, Zheng S. Synthesis and characterization of the trihalophosphine compounds of ruthenium [RuX₂(η⁶-cymene)(PY₃)] (X = Cl, Br, Y = F, Cl, Br) and the related PF₂(NMe₂) and P(NMe₂)₃ compounds; multinuclear NMR spectroscopy and the X-ray single crystal structures of [RuBr₂(η⁶-cymene) (PF₃)]... Inorganic Chemistry. 2008 Oct 20;47(20):9279-9292. doi: 10.1021/ic800611h

Synthesis and characterization of the trihalophosphine compounds of ruthenium [RuX2(η6-cymene)(PY3)] (X = Cl, Br, Y = F, Cl, Br) and the related PF2(NMe2) and P(NMe2)3 compounds; multinuclear NMR spectroscopy and the X-ray single crystal structures of [RuBr2(η6-cymene) (PF3)]...

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