Synthesis and reactions of phenylimidotrimethyl-bis(trimethylphosphine)-rhenium(V). Synthesis and X-ray crystal structure of bis(trimethylsilylmethyl)oxo-rhenium(V)-μ-oxo-tetrakis(trimethylphosphine)rhenium (I)-(trimethylsilylmethyl)dioxorhenium(V), (Re–Re)

Kwok W. Chiu; Wai Kwok Wong; Geoffrey Wilkinson; Anita M.R. Galas; Michael B. Hursthouse

doi:10.1016/S0277-5387(00)81064-5

Synthesis and reactions of phenylimidotrimethyl-bis(trimethylphosphine)-rhenium(V). Synthesis and X-ray crystal structure of bis(trimethylsilylmethyl)oxo-rhenium(V)-μ-oxo-tetrakis(trimethylphosphine)rhenium (I)-(trimethylsilylmethyl)dioxorhenium(V), (Re–Re)

Kwok W. Chiu
, Wai Kwok Wong
, Geoffrey Wilkinson^*
, Anita M.R. Galas
, Michael B. Hursthouse

^*Corresponding author for this work

Department of Chemistry

Research output: Contribution to journal › Journal article › peer-review

22 Citations (Scopus)

Abstract

The interaction of phenylimidotrichloro bis(trimethylphosphine) with dimethylmagnesium gives the trimethyl compound, Re(NPh)Me₃(PMe₃)₂. Exchange reactions between the trichloro and trimethyl compounds are studied by ¹H nuclear magnetic resonance and the intermediates Re(NPh)Me₂Cl(PMe₃)₂ and Re(NPh)MeCl₂(PMe₃)₂ isolated.

The trimethyl reacts with fluoroboric acid to give a phenylamido complex [Re(NHPh)Me₂F(PMe₃)₂]BF₄, with acetic acid to give Re(NPh)Me(CO₂Me₃)₂, and with trityltetrafluoroborate to give [Re(NPh)Me₂(PMe₃)₂]BF₄.

The interaction of Re(NPh)Cl₃(PMe₃)₂ with excess of bis(trimethylsilylmethyl)magnesium and of trimethyl-phosphine in tetrahydrofuran gives an unusual tri-rhenium compound, (Me₃SiCH₂)₃(O)Re-μ-O-Re(PMe₃)₄Re(O)₂(CH₂SiMe₃) whose structure as a thf solvate, has been determined by X-ray crystallography. Crystals of the latter are monoclinic, space group P2₁/n with a = 15.512(3), b = 15.392(2), c = 21.506(4) Å, β = 100.19(2)°, Z = 4. The structure has been refined to an R of 0.07 for 5028 observed diffractometer data. The molecule is tri-nuclear with the central rhenium carrying four PMe₃ groups being bound to the second rhenium by a short Re–Re bond and to the third by an asymmetric oxygen bridge. The end rhenium bound to the bridge oxygen carries two CH₂SiMe₃ groups and an oxygen atom, while the other has one CH₂SiMe₃ group and two oxygen atoms.

Original language	English
Pages (from-to)	31-36
Number of pages	6
Journal	Polyhedron
Volume	1
Issue number	1
DOIs	https://doi.org/10.1016/S0277-5387(00)81064-5
Publication status	Published - Jan 1982

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Chiu, K. W., Wong, W. K., Wilkinson, G., Galas, A. M. R., & Hursthouse, M. B. (1982). Synthesis and reactions of phenylimidotrimethyl-bis(trimethylphosphine)-rhenium(V). Synthesis and X-ray crystal structure of bis(trimethylsilylmethyl)oxo-rhenium(V)-μ-oxo-tetrakis(trimethylphosphine)rhenium (I)-(trimethylsilylmethyl)dioxorhenium(V), (Re–Re). Polyhedron, 1(1), 31-36. https://doi.org/10.1016/S0277-5387(00)81064-5

Chiu, Kwok W. ; Wong, Wai Kwok ; Wilkinson, Geoffrey et al. / Synthesis and reactions of phenylimidotrimethyl-bis(trimethylphosphine)-rhenium(V). Synthesis and X-ray crystal structure of bis(trimethylsilylmethyl)oxo-rhenium(V)-μ-oxo-tetrakis(trimethylphosphine)rhenium (I)-(trimethylsilylmethyl)dioxorhenium(V), (Re–Re). In: Polyhedron. 1982 ; Vol. 1, No. 1. pp. 31-36.

@article{ef5e1dbe28ad41069a9bacc749f0679a,

title = "Synthesis and reactions of phenylimidotrimethyl-bis(trimethylphosphine)-rhenium(V). Synthesis and X-ray crystal structure of bis(trimethylsilylmethyl)oxo-rhenium(V)-μ-oxo-tetrakis(trimethylphosphine)rhenium (I)-(trimethylsilylmethyl)dioxorhenium(V), (Re–Re)",

abstract = "The interaction of phenylimidotrichloro bis(trimethylphosphine) with dimethylmagnesium gives the trimethyl compound, Re(NPh)Me3(PMe3)2. Exchange reactions between the trichloro and trimethyl compounds are studied by 1H nuclear magnetic resonance and the intermediates Re(NPh)Me2Cl(PMe3)2 and Re(NPh)MeCl2(PMe3)2 isolated.The trimethyl reacts with fluoroboric acid to give a phenylamido complex [Re(NHPh)Me2F(PMe3)2]BF4, with acetic acid to give Re(NPh)Me(CO2Me3)2, and with trityltetrafluoroborate to give [Re(NPh)Me2(PMe3)2]BF4.The interaction of Re(NPh)Cl3(PMe3)2 with excess of bis(trimethylsilylmethyl)magnesium and of trimethyl-phosphine in tetrahydrofuran gives an unusual tri-rhenium compound, (Me3SiCH2)3(O)Re-μ-O-Re(PMe3)4Re(O)2(CH2SiMe3) whose structure as a thf solvate, has been determined by X-ray crystallography. Crystals of the latter are monoclinic, space group P21/n with a = 15.512(3), b = 15.392(2), c = 21.506(4) {\AA}, β = 100.19(2)°, Z = 4. The structure has been refined to an R of 0.07 for 5028 observed diffractometer data. The molecule is tri-nuclear with the central rhenium carrying four PMe3 groups being bound to the second rhenium by a short Re–Re bond and to the third by an asymmetric oxygen bridge. The end rhenium bound to the bridge oxygen carries two CH2SiMe3 groups and an oxygen atom, while the other has one CH2SiMe3 group and two oxygen atoms.",

author = "Chiu, \{Kwok W.\} and Wong, \{Wai Kwok\} and Geoffrey Wilkinson and Galas, \{Anita M.R.\} and Hursthouse, \{Michael B.\}",

note = "Publisher copyright: {\textcopyright} 1982 Published by Elsevier Ltd.",

year = "1982",

month = jan,

doi = "10.1016/S0277-5387(00)81064-5",

language = "English",

volume = "1",

pages = "31--36",

journal = "Polyhedron",

issn = "0277-5387",

publisher = "Elsevier Ltd.",

number = "1",

}

Chiu, KW, Wong, WK, Wilkinson, G, Galas, AMR & Hursthouse, MB 1982, 'Synthesis and reactions of phenylimidotrimethyl-bis(trimethylphosphine)-rhenium(V). Synthesis and X-ray crystal structure of bis(trimethylsilylmethyl)oxo-rhenium(V)-μ-oxo-tetrakis(trimethylphosphine)rhenium (I)-(trimethylsilylmethyl)dioxorhenium(V), (Re–Re)', Polyhedron, vol. 1, no. 1, pp. 31-36. https://doi.org/10.1016/S0277-5387(00)81064-5

Synthesis and reactions of phenylimidotrimethyl-bis(trimethylphosphine)-rhenium(V). Synthesis and X-ray crystal structure of bis(trimethylsilylmethyl)oxo-rhenium(V)-μ-oxo-tetrakis(trimethylphosphine)rhenium (I)-(trimethylsilylmethyl)dioxorhenium(V), (Re–Re). / Chiu, Kwok W.; Wong, Wai Kwok; Wilkinson, Geoffrey et al.
In: Polyhedron, Vol. 1, No. 1, 01.1982, p. 31-36.

Research output: Contribution to journal › Journal article › peer-review

TY - JOUR

T1 - Synthesis and reactions of phenylimidotrimethyl-bis(trimethylphosphine)-rhenium(V). Synthesis and X-ray crystal structure of bis(trimethylsilylmethyl)oxo-rhenium(V)-μ-oxo-tetrakis(trimethylphosphine)rhenium (I)-(trimethylsilylmethyl)dioxorhenium(V), (Re–Re)

AU - Chiu, Kwok W.

AU - Wong, Wai Kwok

AU - Wilkinson, Geoffrey

AU - Galas, Anita M.R.

AU - Hursthouse, Michael B.

PY - 1982/1

Y1 - 1982/1

N2 - The interaction of phenylimidotrichloro bis(trimethylphosphine) with dimethylmagnesium gives the trimethyl compound, Re(NPh)Me3(PMe3)2. Exchange reactions between the trichloro and trimethyl compounds are studied by 1H nuclear magnetic resonance and the intermediates Re(NPh)Me2Cl(PMe3)2 and Re(NPh)MeCl2(PMe3)2 isolated.The trimethyl reacts with fluoroboric acid to give a phenylamido complex [Re(NHPh)Me2F(PMe3)2]BF4, with acetic acid to give Re(NPh)Me(CO2Me3)2, and with trityltetrafluoroborate to give [Re(NPh)Me2(PMe3)2]BF4.The interaction of Re(NPh)Cl3(PMe3)2 with excess of bis(trimethylsilylmethyl)magnesium and of trimethyl-phosphine in tetrahydrofuran gives an unusual tri-rhenium compound, (Me3SiCH2)3(O)Re-μ-O-Re(PMe3)4Re(O)2(CH2SiMe3) whose structure as a thf solvate, has been determined by X-ray crystallography. Crystals of the latter are monoclinic, space group P21/n with a = 15.512(3), b = 15.392(2), c = 21.506(4) Å, β = 100.19(2)°, Z = 4. The structure has been refined to an R of 0.07 for 5028 observed diffractometer data. The molecule is tri-nuclear with the central rhenium carrying four PMe3 groups being bound to the second rhenium by a short Re–Re bond and to the third by an asymmetric oxygen bridge. The end rhenium bound to the bridge oxygen carries two CH2SiMe3 groups and an oxygen atom, while the other has one CH2SiMe3 group and two oxygen atoms.

AB - The interaction of phenylimidotrichloro bis(trimethylphosphine) with dimethylmagnesium gives the trimethyl compound, Re(NPh)Me3(PMe3)2. Exchange reactions between the trichloro and trimethyl compounds are studied by 1H nuclear magnetic resonance and the intermediates Re(NPh)Me2Cl(PMe3)2 and Re(NPh)MeCl2(PMe3)2 isolated.The trimethyl reacts with fluoroboric acid to give a phenylamido complex [Re(NHPh)Me2F(PMe3)2]BF4, with acetic acid to give Re(NPh)Me(CO2Me3)2, and with trityltetrafluoroborate to give [Re(NPh)Me2(PMe3)2]BF4.The interaction of Re(NPh)Cl3(PMe3)2 with excess of bis(trimethylsilylmethyl)magnesium and of trimethyl-phosphine in tetrahydrofuran gives an unusual tri-rhenium compound, (Me3SiCH2)3(O)Re-μ-O-Re(PMe3)4Re(O)2(CH2SiMe3) whose structure as a thf solvate, has been determined by X-ray crystallography. Crystals of the latter are monoclinic, space group P21/n with a = 15.512(3), b = 15.392(2), c = 21.506(4) Å, β = 100.19(2)°, Z = 4. The structure has been refined to an R of 0.07 for 5028 observed diffractometer data. The molecule is tri-nuclear with the central rhenium carrying four PMe3 groups being bound to the second rhenium by a short Re–Re bond and to the third by an asymmetric oxygen bridge. The end rhenium bound to the bridge oxygen carries two CH2SiMe3 groups and an oxygen atom, while the other has one CH2SiMe3 group and two oxygen atoms.

UR - https://www.scopus.com/pages/publications/0346337214

U2 - 10.1016/S0277-5387(00)81064-5

DO - 10.1016/S0277-5387(00)81064-5

M3 - Journal article

AN - SCOPUS:0346337214

SN - 0277-5387

VL - 1

SP - 31

EP - 36

JO - Polyhedron

JF - Polyhedron

IS - 1

ER -

Chiu KW, Wong WK, Wilkinson G, Galas AMR, Hursthouse MB. Synthesis and reactions of phenylimidotrimethyl-bis(trimethylphosphine)-rhenium(V). Synthesis and X-ray crystal structure of bis(trimethylsilylmethyl)oxo-rhenium(V)-μ-oxo-tetrakis(trimethylphosphine)rhenium (I)-(trimethylsilylmethyl)dioxorhenium(V), (Re–Re). Polyhedron. 1982 Jan;1(1):31-36. doi: 10.1016/S0277-5387(00)81064-5

Synthesis and reactions of phenylimidotrimethyl-bis(trimethylphosphine)-rhenium(V). Synthesis and X-ray crystal structure of bis(trimethylsilylmethyl)oxo-rhenium(V)-μ-oxo-tetrakis(trimethylphosphine)rhenium (I)-(trimethylsilylmethyl)dioxorhenium(V), (Re–Re)

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