Alkyl and hydrido derivatives of tetrakis(trimethylphosphine)osmium(II). X-Ray crystal structure of the metallacycle Os[(CH2)2SiMe2](PMe3)4

Torsten Behling; Gregory S Girolami; Geoffrey Wilkinson; Richard G. Somerville; Michael B. Hursthouse

doi:10.1039/DT9840000877

Alkyl and hydrido derivatives of tetrakis(trimethylphosphine)osmium(II). X-Ray crystal structure of the metallacycle Os[(CH₂)₂SiMe₂](PMe₃)₄

Torsten Behling, Gregory S Girolami, Geoffrey Wilkinson, Richard G. Somerville, Michael B. Hursthouse

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

Abstract

The interaction of the osmium acetato-complexes trans-Os^II(O₂CMe)₂(PMe₃)₄ and Os^III₂Cl₂(μ-O₂CMe)₄ with alkylating agents in the presence of trimethylphosphine has led to the isolation of cis-OsMe₂(PMe₃)₄, Os[(CH₂)₂SiMe₂](PMe₃)₄, OsCl(CH₂PMe₂)(PMe₃)₃, and Os(CH₂C₆H₄)(PMe₃)₄. The hydride cis-OsH₂(PMe₃)₄ has been obtained from K₂[OsO₂(OMe)₄] by interaction with PMe₃ and methanol. The ¹H, ¹³C-{¹H}, and ³¹P-{¹H} n.m.r. spectra of the compounds are discussed. The X-ray crystal structure of the metallacycle Os[(CH₂)₂SiMe₂](PMe₃)₄ has been determined, and the [graphic omitted] ring found to be flat. The Os-C distances are 2.24(1) Å, while the Os-P distances of 2.32 (trans to C) and 2.35 Å (trans to P) indicate the trans influence of the metallacyclobutane is low compared to that of the σ alkyl groups.

Original language	English (US)
Pages (from-to)	877-881
Number of pages	5
Journal	Journal of the Chemical Society, Dalton Transactions
Issue number	5
DOIs	https://doi.org/10.1039/DT9840000877
State	Published - 1984
Externally published	Yes

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Chemistry(all)

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@article{b925623e9f24400b9c03aa2581fe7f62,

title = "Alkyl and hydrido derivatives of tetrakis(trimethylphosphine)osmium(II). X-Ray crystal structure of the metallacycle Os[(CH2)2SiMe2](PMe3)4",

abstract = "The interaction of the osmium acetato-complexes trans-OsII(O2CMe)2(PMe3)4 and OsIII2Cl2(μ-O2CMe)4 with alkylating agents in the presence of trimethylphosphine has led to the isolation of cis-OsMe2(PMe3)4, Os[(CH2)2SiMe2](PMe3)4, OsCl(CH2PMe2)(PMe3)3, and Os(CH2C6H4)(PMe3)4. The hydride cis-OsH2(PMe3)4 has been obtained from K2[OsO2(OMe)4] by interaction with PMe3 and methanol. The 1H, 13C-{1H}, and 31P-{1H} n.m.r. spectra of the compounds are discussed. The X-ray crystal structure of the metallacycle Os[(CH2)2SiMe2](PMe3)4 has been determined, and the [graphic omitted] ring found to be flat. The Os-C distances are 2.24(1) {\AA}, while the Os-P distances of 2.32 (trans to C) and 2.35 {\AA} (trans to P) indicate the trans influence of the metallacyclobutane is low compared to that of the σ alkyl groups.",

author = "Torsten Behling and Girolami, {Gregory S} and Geoffrey Wilkinson and Somerville, {Richard G.} and Hursthouse, {Michael B.}",

year = "1984",

doi = "10.1039/DT9840000877",

language = "English (US)",

pages = "877--881",

journal = "Dalton Transactions",

issn = "1470-479X",

publisher = "Royal Society of Chemistry",

number = "5",

}

TY - JOUR

T1 - Alkyl and hydrido derivatives of tetrakis(trimethylphosphine)osmium(II). X-Ray crystal structure of the metallacycle Os[(CH2)2SiMe2](PMe3)4

AU - Behling, Torsten

AU - Girolami, Gregory S

AU - Wilkinson, Geoffrey

AU - Somerville, Richard G.

AU - Hursthouse, Michael B.

PY - 1984

Y1 - 1984

N2 - The interaction of the osmium acetato-complexes trans-OsII(O2CMe)2(PMe3)4 and OsIII2Cl2(μ-O2CMe)4 with alkylating agents in the presence of trimethylphosphine has led to the isolation of cis-OsMe2(PMe3)4, Os[(CH2)2SiMe2](PMe3)4, OsCl(CH2PMe2)(PMe3)3, and Os(CH2C6H4)(PMe3)4. The hydride cis-OsH2(PMe3)4 has been obtained from K2[OsO2(OMe)4] by interaction with PMe3 and methanol. The 1H, 13C-{1H}, and 31P-{1H} n.m.r. spectra of the compounds are discussed. The X-ray crystal structure of the metallacycle Os[(CH2)2SiMe2](PMe3)4 has been determined, and the [graphic omitted] ring found to be flat. The Os-C distances are 2.24(1) Å, while the Os-P distances of 2.32 (trans to C) and 2.35 Å (trans to P) indicate the trans influence of the metallacyclobutane is low compared to that of the σ alkyl groups.

AB - The interaction of the osmium acetato-complexes trans-OsII(O2CMe)2(PMe3)4 and OsIII2Cl2(μ-O2CMe)4 with alkylating agents in the presence of trimethylphosphine has led to the isolation of cis-OsMe2(PMe3)4, Os[(CH2)2SiMe2](PMe3)4, OsCl(CH2PMe2)(PMe3)3, and Os(CH2C6H4)(PMe3)4. The hydride cis-OsH2(PMe3)4 has been obtained from K2[OsO2(OMe)4] by interaction with PMe3 and methanol. The 1H, 13C-{1H}, and 31P-{1H} n.m.r. spectra of the compounds are discussed. The X-ray crystal structure of the metallacycle Os[(CH2)2SiMe2](PMe3)4 has been determined, and the [graphic omitted] ring found to be flat. The Os-C distances are 2.24(1) Å, while the Os-P distances of 2.32 (trans to C) and 2.35 Å (trans to P) indicate the trans influence of the metallacyclobutane is low compared to that of the σ alkyl groups.

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