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Synthesis and properties of new ditertiary stibines based upon o-, m- or p-xylyl and m- or p-phenylene backbones and their complexes with tungsten, iron and nickel carbonyls

Synthesis and properties of new ditertiary stibines based upon o-, m- or p-xylyl and m- or p-phenylene backbones and their complexes with tungsten, iron and nickel carbonyls
Synthesis and properties of new ditertiary stibines based upon o-, m- or p-xylyl and m- or p-phenylene backbones and their complexes with tungsten, iron and nickel carbonyls
High yield syntheses for 1,2-, 1,3-, and 1,4-xylyl distibines (1,2-C6H4(CH2SbMe2)(2), 1,3-C6H4(CH2SbMe2)(2), 1,4-C6H4(CH2SbMe2)(2), respectively) from Me2SbCl (conveniently made in situ from Me2PhSb and HClgas) and the appropriate di-Grignard are reported. The 1,3- and 1,4-phenylene distibines, 1,3-C6H4(SbMe2)(2) and 1,4-C6H4(SbMe2)(2), were made similarly. The new ligands have been characterised by mass spectrometry, H-1 and C-13{H-1} NMR spectroscopy, and by the preparation of methiodide derivatives. The crystal structures of 1,4-C6H4(CH2SbMe2)(2) and [1,3-C6H4(CH2SbMe3)(2)] I-2 have been determined. The synthesis of 1,2-C6H4( CH2SbPh2)(2) has been achieved similarly in modest yield and the distibine converted into the tetra-iodo-derivative 1,2-C6H4(CH2SbPh2I2)(2). The coordination modes available to these ligands have been probed by the synthesis and characterisation of complexes with nickel, iron and tungsten carbonyls. The crystal structure of [{Fe(CO)(4)}(2){ {mu-1,3-C6H4(CH2SbMe2)(2)}] has been determined. The spectroscopic properties of these carbonyl derivatives have been compared with those of complexes of other antimony ligands, and in some cases with diphosphine and diarsine complexes, to probe the electronic properties of the new ligands.
distibinomethane ligands, crystal-structures, proprietes vibrationnelles, coordination chemistry, molybdene carbonyle, tertiary, derivatives, halides, sb, di
1477-9226
51-58
Levason, William
e7f6d7c7-643c-49f5-8b57-0ebbe1bb52cd
Matthews, Melissa L.
48114504-dd8b-4879-b428-f31fada714e7
Reid, Gillian
37d35b11-40ce-48c5-a68e-f6ce04cd4037
Webster, Michael
f26c6e36-cb2e-486e-b2ed-b0d25a3a71f7
Levason, William
e7f6d7c7-643c-49f5-8b57-0ebbe1bb52cd
Matthews, Melissa L.
48114504-dd8b-4879-b428-f31fada714e7
Reid, Gillian
37d35b11-40ce-48c5-a68e-f6ce04cd4037
Webster, Michael
f26c6e36-cb2e-486e-b2ed-b0d25a3a71f7

Levason, William, Matthews, Melissa L., Reid, Gillian and Webster, Michael (2004) Synthesis and properties of new ditertiary stibines based upon o-, m- or p-xylyl and m- or p-phenylene backbones and their complexes with tungsten, iron and nickel carbonyls. Dalton Transactions, 2004 (1), 51-58. (doi:10.1039/b312083j).

Record type: Article

Abstract

High yield syntheses for 1,2-, 1,3-, and 1,4-xylyl distibines (1,2-C6H4(CH2SbMe2)(2), 1,3-C6H4(CH2SbMe2)(2), 1,4-C6H4(CH2SbMe2)(2), respectively) from Me2SbCl (conveniently made in situ from Me2PhSb and HClgas) and the appropriate di-Grignard are reported. The 1,3- and 1,4-phenylene distibines, 1,3-C6H4(SbMe2)(2) and 1,4-C6H4(SbMe2)(2), were made similarly. The new ligands have been characterised by mass spectrometry, H-1 and C-13{H-1} NMR spectroscopy, and by the preparation of methiodide derivatives. The crystal structures of 1,4-C6H4(CH2SbMe2)(2) and [1,3-C6H4(CH2SbMe3)(2)] I-2 have been determined. The synthesis of 1,2-C6H4( CH2SbPh2)(2) has been achieved similarly in modest yield and the distibine converted into the tetra-iodo-derivative 1,2-C6H4(CH2SbPh2I2)(2). The coordination modes available to these ligands have been probed by the synthesis and characterisation of complexes with nickel, iron and tungsten carbonyls. The crystal structure of [{Fe(CO)(4)}(2){ {mu-1,3-C6H4(CH2SbMe2)(2)}] has been determined. The spectroscopic properties of these carbonyl derivatives have been compared with those of complexes of other antimony ligands, and in some cases with diphosphine and diarsine complexes, to probe the electronic properties of the new ligands.

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Published date: 2004
Keywords: distibinomethane ligands, crystal-structures, proprietes vibrationnelles, coordination chemistry, molybdene carbonyle, tertiary, derivatives, halides, sb, di

Identifiers

Local EPrints ID: 20272
URI: http://eprints.soton.ac.uk/id/eprint/20272
ISSN: 1477-9226
PURE UUID: 1299cd6a-682b-4f4e-90a5-0d3c1afc0ee1
ORCID for William Levason: ORCID iD orcid.org/0000-0003-3540-0971
ORCID for Gillian Reid: ORCID iD orcid.org/0000-0001-5349-3468

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Date deposited: 20 Feb 2006
Last modified: 16 Mar 2024 02:43

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Contributors

Author: William Levason ORCID iD
Author: Melissa L. Matthews
Author: Gillian Reid ORCID iD
Author: Michael Webster

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