Thio-, seleno- and telluro-ether complexes of aluminium(III) halides: synthesis, structures and properties.
Identifieur interne : 000022 ( Main/Exploration ); précédent : 000021; suivant : 000023Thio-, seleno- and telluro-ether complexes of aluminium(III) halides: synthesis, structures and properties.
Auteurs : RBID : pubmed:24413529Abstract
The reaction of AlCl3 with Me2E (E = S, Se or Te) or (n)Bu2E (E = Se or Te) in CH2Cl2 under rigorously anhydrous conditions gave the pseudo-tetrahedral complexes [AlCl3(R2E)]. The [AlX3(Me2E)] (X = Br or I, E = S; X = Br, E = Te) were made from toluene solution since attempted syntheses in CH2Cl2 resulted in substantial chloride incorporation. The synthesis of [(AlCl3)2{o-C6H4(CH2SEt)2}], in which the ligand bridges two tetrahedral aluminium centres, and of the six-coordinate trans-[AlX2{MeE(CH2)2EMe}2][AlX4] (X = Cl or Br, E = S, and X = Cl, E = Se) and cis-[AlI2{MeS(CH2)2SMe}2][AlI4] are reported. The tripodal thioether forms [AlCl3{MeC(CH2SMe)3}], which is a chain polymer with κ(2)-coordinated ligand and a tbp arrangement at Al(iii). Chalcogenoether macrocycle complexes [AlCl3([9]aneS3)], [AlCl2([14]aneS4)][AlCl4] and [AlCl2([16]aneSe4)] [AlCl4] are also described. All complexes were characterised by microanalysis, IR and multinuclear NMR ((1)H, (27)Al, (77)Se or (125)Te) spectroscopy as appropriate. In CH2Cl2 solution [AlCl3(Me2S)] with added Me2S forms [AlCl3(Me2S)2], and the [AlX2{MeS(CH2)2SMe}2][AlX4] exist as mixtures of cis and trans isomers which undergo rapid exchange at ambient temperatures. X-Ray crystal structures are reported for [AlCl3(Me2Se], [AlX3(Me2Te)] (X = Cl or Br), trans-[AlCl2{MeE(CH2)2EMe}2][AlCl4] (E = S or Se), cis-[AlI2{MeS(CH2)2SMe}2][AlI4], [AlCl3{MeC(CH2SMe)3}], and for the sulfonium salt [Me2SH][AlCl4]. The aluminium halide chalcogenoether chemistry is compared with the corresponding gallium and indium systems, and the relative Lewis acidities of the metals discussed. Attempts to use [AlCl3((n)Bu2E)] (E = Se or Te) as LPCVD reagents to form aluminium chalcogenide films were unsuccessful.
DOI: 10.1039/c3dt52991f
PubMed: 24413529
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<record><TEI><teiHeader><fileDesc><titleStmt><title xml:lang="en">Thio-, seleno- and telluro-ether complexes of aluminium(III) halides: synthesis, structures and properties.</title><author><name sortKey="George, Kathryn" uniqKey="George K">Kathryn George</name><affiliation wicri:level="1"><nlm:affiliation>School of Chemistry, University of Southampton, Highfield, Southampton SO17 1BJ, UK. wxl@soton.ac.uk.</nlm:affiliation><country xml:lang="fr">Royaume-Uni</country><wicri:regionArea>School of Chemistry, University of Southampton, Highfield, Southampton SO17 1BJ</wicri:regionArea></affiliation></author><author><name sortKey="Jura, Marek" uniqKey="Jura M">Marek Jura</name></author><author><name sortKey="Levason, William" uniqKey="Levason W">William Levason</name></author><author><name sortKey="Light, Mark E" uniqKey="Light M">Mark E Light</name></author><author><name sortKey="Reid, Gillian" uniqKey="Reid G">Gillian Reid</name></author></titleStmt><publicationStmt><date when="2014">2014</date><idno type="doi">10.1039/c3dt52991f</idno><idno type="RBID">pubmed:24413529</idno><idno type="pmid">24413529</idno><idno type="wicri:Area/Main/Corpus">000214</idno><idno type="wicri:Area/Main/Curation">000214</idno><idno type="wicri:Area/Main/Exploration">000022</idno></publicationStmt></fileDesc><profileDesc><textClass></textClass></profileDesc></teiHeader><front><div type="abstract" xml:lang="en">The reaction of AlCl3 with Me2E (E = S, Se or Te) or (n)Bu2E (E = Se or Te) in CH2Cl2 under rigorously anhydrous conditions gave the pseudo-tetrahedral complexes [AlCl3(R2E)]. The [AlX3(Me2E)] (X = Br or I, E = S; X = Br, E = Te) were made from toluene solution since attempted syntheses in CH2Cl2 resulted in substantial chloride incorporation. The synthesis of [(AlCl3)2{o-C6H4(CH2SEt)2}], in which the ligand bridges two tetrahedral aluminium centres, and of the six-coordinate trans-[AlX2{MeE(CH2)2EMe}2][AlX4] (X = Cl or Br, E = S, and X = Cl, E = Se) and cis-[AlI2{MeS(CH2)2SMe}2][AlI4] are reported. The tripodal thioether forms [AlCl3{MeC(CH2SMe)3}], which is a chain polymer with κ(2)-coordinated ligand and a tbp arrangement at Al(iii). Chalcogenoether macrocycle complexes [AlCl3([9]aneS3)], [AlCl2([14]aneS4)][AlCl4] and [AlCl2([16]aneSe4)] [AlCl4] are also described. All complexes were characterised by microanalysis, IR and multinuclear NMR ((1)H, (27)Al, (77)Se or (125)Te) spectroscopy as appropriate. In CH2Cl2 solution [AlCl3(Me2S)] with added Me2S forms [AlCl3(Me2S)2], and the [AlX2{MeS(CH2)2SMe}2][AlX4] exist as mixtures of cis and trans isomers which undergo rapid exchange at ambient temperatures. X-Ray crystal structures are reported for [AlCl3(Me2Se], [AlX3(Me2Te)] (X = Cl or Br), trans-[AlCl2{MeE(CH2)2EMe}2][AlCl4] (E = S or Se), cis-[AlI2{MeS(CH2)2SMe}2][AlI4], [AlCl3{MeC(CH2SMe)3}], and for the sulfonium salt [Me2SH][AlCl4]. The aluminium halide chalcogenoether chemistry is compared with the corresponding gallium and indium systems, and the relative Lewis acidities of the metals discussed. Attempts to use [AlCl3((n)Bu2E)] (E = Se or Te) as LPCVD reagents to form aluminium chalcogenide films were unsuccessful.</div></front></TEI><pubmed><MedlineCitation Owner="NLM" Status="In-Process"><PMID Version="1">24413529</PMID><DateCreated><Year>2014</Year><Month>02</Month><Day>05</Day></DateCreated><Article PubModel="Print"><Journal><ISSN IssnType="Electronic">1477-9234</ISSN><JournalIssue CitedMedium="Internet"><Volume>43</Volume><Issue>9</Issue><PubDate><Year>2014</Year><Month>Mar</Month><Day>7</Day></PubDate></JournalIssue><Title>Dalton transactions (Cambridge, England : 2003)</Title><ISOAbbreviation>Dalton Trans</ISOAbbreviation></Journal><ArticleTitle>Thio-, seleno- and telluro-ether complexes of aluminium(III) halides: synthesis, structures and properties.</ArticleTitle><Pagination><MedlinePgn>3637-48</MedlinePgn></Pagination><ELocationID EIdType="doi" ValidYN="Y">10.1039/c3dt52991f</ELocationID><Abstract><AbstractText>The reaction of AlCl3 with Me2E (E = S, Se or Te) or (n)Bu2E (E = Se or Te) in CH2Cl2 under rigorously anhydrous conditions gave the pseudo-tetrahedral complexes [AlCl3(R2E)]. The [AlX3(Me2E)] (X = Br or I, E = S; X = Br, E = Te) were made from toluene solution since attempted syntheses in CH2Cl2 resulted in substantial chloride incorporation. The synthesis of [(AlCl3)2{o-C6H4(CH2SEt)2}], in which the ligand bridges two tetrahedral aluminium centres, and of the six-coordinate trans-[AlX2{MeE(CH2)2EMe}2][AlX4] (X = Cl or Br, E = S, and X = Cl, E = Se) and cis-[AlI2{MeS(CH2)2SMe}2][AlI4] are reported. The tripodal thioether forms [AlCl3{MeC(CH2SMe)3}], which is a chain polymer with κ(2)-coordinated ligand and a tbp arrangement at Al(iii). Chalcogenoether macrocycle complexes [AlCl3([9]aneS3)], [AlCl2([14]aneS4)][AlCl4] and [AlCl2([16]aneSe4)] [AlCl4] are also described. All complexes were characterised by microanalysis, IR and multinuclear NMR ((1)H, (27)Al, (77)Se or (125)Te) spectroscopy as appropriate. In CH2Cl2 solution [AlCl3(Me2S)] with added Me2S forms [AlCl3(Me2S)2], and the [AlX2{MeS(CH2)2SMe}2][AlX4] exist as mixtures of cis and trans isomers which undergo rapid exchange at ambient temperatures. X-Ray crystal structures are reported for [AlCl3(Me2Se], [AlX3(Me2Te)] (X = Cl or Br), trans-[AlCl2{MeE(CH2)2EMe}2][AlCl4] (E = S or Se), cis-[AlI2{MeS(CH2)2SMe}2][AlI4], [AlCl3{MeC(CH2SMe)3}], and for the sulfonium salt [Me2SH][AlCl4]. The aluminium halide chalcogenoether chemistry is compared with the corresponding gallium and indium systems, and the relative Lewis acidities of the metals discussed. Attempts to use [AlCl3((n)Bu2E)] (E = Se or Te) as LPCVD reagents to form aluminium chalcogenide films were unsuccessful.</AbstractText></Abstract><AuthorList CompleteYN="Y"><Author ValidYN="Y"><LastName>George</LastName><ForeName>Kathryn</ForeName><Initials>K</Initials><Affiliation>School of Chemistry, University of Southampton, Highfield, Southampton SO17 1BJ, UK. wxl@soton.ac.uk.</Affiliation></Author><Author ValidYN="Y"><LastName>Jura</LastName><ForeName>Marek</ForeName><Initials>M</Initials></Author><Author ValidYN="Y"><LastName>Levason</LastName><ForeName>William</ForeName><Initials>W</Initials></Author><Author ValidYN="Y"><LastName>Light</LastName><ForeName>Mark E</ForeName><Initials>ME</Initials></Author><Author ValidYN="Y"><LastName>Reid</LastName><ForeName>Gillian</ForeName><Initials>G</Initials></Author></AuthorList><Language>eng</Language><PublicationTypeList><PublicationType>Journal Article</PublicationType></PublicationTypeList></Article><MedlineJournalInfo><Country>England</Country><MedlineTA>Dalton Trans</MedlineTA><NlmUniqueID>101176026</NlmUniqueID><ISSNLinking>1477-9226</ISSNLinking></MedlineJournalInfo></MedlineCitation><PubmedData><History><PubMedPubDate PubStatus="entrez"><Year>2014</Year><Month>1</Month><Day>14</Day><Hour>6</Hour><Minute>0</Minute></PubMedPubDate><PubMedPubDate PubStatus="pubmed"><Year>2014</Year><Month>1</Month><Day>15</Day><Hour>6</Hour><Minute>0</Minute></PubMedPubDate><PubMedPubDate PubStatus="medline"><Year>2014</Year><Month>1</Month><Day>15</Day><Hour>6</Hour><Minute>0</Minute></PubMedPubDate></History><PublicationStatus>ppublish</PublicationStatus><ArticleIdList><ArticleId IdType="doi">10.1039/c3dt52991f</ArticleId><ArticleId IdType="pubmed">24413529</ArticleId></ArticleIdList></PubmedData></pubmed></record>Pour manipuler ce document sous Unix (Dilib)
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