Synthesis and characterization of oxorhenium-'3 + 1' mixed-thiolate complexes. Crystal and molecular structures of [ReO{η3-(SCH2CH2)2S}(C 6H4X-4-CH2S)] (X = F, Cl, Br, OMe) and of the pendant thiolate compounds

Kevin P. Maresca; Grant H. Bonavia; John W. Babich; Jon Zubieta

doi:10.1016/s0020-1693(98)00296-5

Synthesis and characterization of oxorhenium-'3 + 1' mixed-thiolate complexes. Crystal and molecular structures of [ReO{η³-(SCH₂CH₂)₂S}(C ₆H₄X-4-CH₂S)] (X = F, Cl, Br, OMe) and of the pendant thiolate compounds

Kevin P. Maresca, Grant H. Bonavia, John W. Babich, Jon Zubieta

Department of Chemistry

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

38 Scopus citations

Abstract

The reaction of [(n-C₄H₉)₄N][ReOBr₄(OPPh ₃)] with bis(2-mercaptoethyl) sulfide produces [ReOBr{η³-(SCH₂CH₂)₂S}] (1), which can be reacted in turn to replace the labile bromine atom with various monodentate thiolate ligands. The reactions of [ReOBr{η³-(SCH₂CH₂)₂S}] (1) with (C₆H₄X-4-CH₂S) where X = Br, Cl, F and OMe in alcohol treated with triethylamine has led to the isolation of a series of rhenium complexes of the type [ReO{(SCH₂CH₂)₂S}(C₆H ₄X-4-CH₂S)]. The reaction of [ReOCl₃(DMS) (OPPh₃)] with 2-mercaptoethyl sulfide and base results in the isolation of [ReO{η³-(SCH₂CH₂)₂S}(η ¹-SCH₂CH₂SCH₂CH₂SH)] (6) while the reaction of 1 with dithioerythritol and triethylamine results in the formation of [ReO{η³-(SCH₂CH₂)₂S}{η ¹-SCH₂CH(OH)CH(OH)CH₂SH}] (7), unusual examples of '3 + 1' coordination chemistry with a pendant thiol arm. The X-ray structures of [ReO{η³-(SCH₂CH₂)₂S}(C ₆H₄X-4-CH₂S)] (X = Br (2), Cl (3), F (4), and OMe (5)), [ReO(η³-(SCH₂(CH₂)₂S}{η ¹-SCH₂CH₂SCH₂CH₂SH)] (6) and [ReO{η³-(SCH₂CH₂)₂S}{η ¹-SCH₂CH(OH)CH₂CH(OH)CH₂SH}] (7) have been determined.

Original language	English (US)
Pages (from-to)	252-257
Number of pages	6
Journal	Inorganica Chimica Acta
Volume	284
Issue number	2
DOIs	https://doi.org/10.1016/s0020-1693(98)00296-5
State	Published - Jan 30 1999

Keywords

Crystal structures
Oxo complexes
Rhenium complexes
Thiolate complexes

ASJC Scopus subject areas

Physical and Theoretical Chemistry
Inorganic Chemistry
Materials Chemistry

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10.1016/s0020-1693(98)00296-5

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Synthesis and characterization of oxorhenium-'3 + 1' mixed-thiolate complexes. Crystal and molecular structures of [ReO{η³-(SCH₂CH₂)₂S}(C ₆H₄X-4-CH₂S)] (X = F, Cl, Br, OMe) and of the pendant thiolate compounds. / Maresca, Kevin P.; Bonavia, Grant H.; Babich, John W. et al.
In: Inorganica Chimica Acta, Vol. 284, No. 2, 30.01.1999, p. 252-257.

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

Maresca, KP, Bonavia, GH, Babich, JW & Zubieta, J 1999, 'Synthesis and characterization of oxorhenium-'3 + 1' mixed-thiolate complexes. Crystal and molecular structures of [ReO{η³-(SCH₂CH₂)₂S}(C ₆H₄X-4-CH₂S)] (X = F, Cl, Br, OMe) and of the pendant thiolate compounds', Inorganica Chimica Acta, vol. 284, no. 2, pp. 252-257. https://doi.org/10.1016/s0020-1693(98)00296-5

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title = "Synthesis and characterization of oxorhenium-'3 + 1' mixed-thiolate complexes. Crystal and molecular structures of [ReO{η3-(SCH2CH2)2S}(C 6H4X-4-CH2S)] (X = F, Cl, Br, OMe) and of the pendant thiolate compounds",

abstract = "The reaction of [(n-C4H9)4N][ReOBr4(OPPh 3)] with bis(2-mercaptoethyl) sulfide produces [ReOBr{η3-(SCH2CH2)2S}] (1), which can be reacted in turn to replace the labile bromine atom with various monodentate thiolate ligands. The reactions of [ReOBr{η3-(SCH2CH2)2S}] (1) with (C6H4X-4-CH2S) where X = Br, Cl, F and OMe in alcohol treated with triethylamine has led to the isolation of a series of rhenium complexes of the type [ReO{(SCH2CH2)2S}(C6H 4X-4-CH2S)]. The reaction of [ReOCl3(DMS) (OPPh3)] with 2-mercaptoethyl sulfide and base results in the isolation of [ReO{η3-(SCH2CH2)2S}(η 1-SCH2CH2SCH2CH2SH)] (6) while the reaction of 1 with dithioerythritol and triethylamine results in the formation of [ReO{η3-(SCH2CH2)2S}{η 1-SCH2CH(OH)CH(OH)CH2SH}] (7), unusual examples of '3 + 1' coordination chemistry with a pendant thiol arm. The X-ray structures of [ReO{η3-(SCH2CH2)2S}(C 6H4X-4-CH2S)] (X = Br (2), Cl (3), F (4), and OMe (5)), [ReO(η3-(SCH2(CH2)2S}{η 1-SCH2CH2SCH2CH2SH)] (6) and [ReO{η3-(SCH2CH2)2S}{η 1-SCH2CH(OH)CH2CH(OH)CH2SH}] (7) have been determined.",

keywords = "Crystal structures, Oxo complexes, Rhenium complexes, Thiolate complexes",

author = "Maresca, {Kevin P.} and Bonavia, {Grant H.} and Babich, {John W.} and Jon Zubieta",

note = "Funding Information: This work was supported by a grant from the Department of Energy Office of Health and Environmental Research DE-FG02-93RG1571.",

year = "1999",

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doi = "10.1016/s0020-1693(98)00296-5",

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TY - JOUR

T1 - Synthesis and characterization of oxorhenium-'3 + 1' mixed-thiolate complexes. Crystal and molecular structures of [ReO{η3-(SCH2CH2)2S}(C 6H4X-4-CH2S)] (X = F, Cl, Br, OMe) and of the pendant thiolate compounds

AU - Maresca, Kevin P.

AU - Bonavia, Grant H.

AU - Babich, John W.

AU - Zubieta, Jon

N1 - Funding Information: This work was supported by a grant from the Department of Energy Office of Health and Environmental Research DE-FG02-93RG1571.

PY - 1999/1/30

Y1 - 1999/1/30

N2 - The reaction of [(n-C4H9)4N][ReOBr4(OPPh 3)] with bis(2-mercaptoethyl) sulfide produces [ReOBr{η3-(SCH2CH2)2S}] (1), which can be reacted in turn to replace the labile bromine atom with various monodentate thiolate ligands. The reactions of [ReOBr{η3-(SCH2CH2)2S}] (1) with (C6H4X-4-CH2S) where X = Br, Cl, F and OMe in alcohol treated with triethylamine has led to the isolation of a series of rhenium complexes of the type [ReO{(SCH2CH2)2S}(C6H 4X-4-CH2S)]. The reaction of [ReOCl3(DMS) (OPPh3)] with 2-mercaptoethyl sulfide and base results in the isolation of [ReO{η3-(SCH2CH2)2S}(η 1-SCH2CH2SCH2CH2SH)] (6) while the reaction of 1 with dithioerythritol and triethylamine results in the formation of [ReO{η3-(SCH2CH2)2S}{η 1-SCH2CH(OH)CH(OH)CH2SH}] (7), unusual examples of '3 + 1' coordination chemistry with a pendant thiol arm. The X-ray structures of [ReO{η3-(SCH2CH2)2S}(C 6H4X-4-CH2S)] (X = Br (2), Cl (3), F (4), and OMe (5)), [ReO(η3-(SCH2(CH2)2S}{η 1-SCH2CH2SCH2CH2SH)] (6) and [ReO{η3-(SCH2CH2)2S}{η 1-SCH2CH(OH)CH2CH(OH)CH2SH}] (7) have been determined.

AB - The reaction of [(n-C4H9)4N][ReOBr4(OPPh 3)] with bis(2-mercaptoethyl) sulfide produces [ReOBr{η3-(SCH2CH2)2S}] (1), which can be reacted in turn to replace the labile bromine atom with various monodentate thiolate ligands. The reactions of [ReOBr{η3-(SCH2CH2)2S}] (1) with (C6H4X-4-CH2S) where X = Br, Cl, F and OMe in alcohol treated with triethylamine has led to the isolation of a series of rhenium complexes of the type [ReO{(SCH2CH2)2S}(C6H 4X-4-CH2S)]. The reaction of [ReOCl3(DMS) (OPPh3)] with 2-mercaptoethyl sulfide and base results in the isolation of [ReO{η3-(SCH2CH2)2S}(η 1-SCH2CH2SCH2CH2SH)] (6) while the reaction of 1 with dithioerythritol and triethylamine results in the formation of [ReO{η3-(SCH2CH2)2S}{η 1-SCH2CH(OH)CH(OH)CH2SH}] (7), unusual examples of '3 + 1' coordination chemistry with a pendant thiol arm. The X-ray structures of [ReO{η3-(SCH2CH2)2S}(C 6H4X-4-CH2S)] (X = Br (2), Cl (3), F (4), and OMe (5)), [ReO(η3-(SCH2(CH2)2S}{η 1-SCH2CH2SCH2CH2SH)] (6) and [ReO{η3-(SCH2CH2)2S}{η 1-SCH2CH(OH)CH2CH(OH)CH2SH}] (7) have been determined.

KW - Crystal structures

KW - Oxo complexes

KW - Rhenium complexes

KW - Thiolate complexes

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