Synthesis and characterization of HC[C(Me)N(C(6)H(3)-2,6-i-Pr(2))](2)MX(2) (M = Al, X = Cl, I; M = Ga, In, X = Me, Cl, I): sterically encumbered beta-diketiminate group 13 metal derivatives.
Identifieur interne : 003672 ( Main/Exploration ); précédent : 003671; suivant : 003673Synthesis and characterization of HC[C(Me)N(C(6)H(3)-2,6-i-Pr(2))](2)MX(2) (M = Al, X = Cl, I; M = Ga, In, X = Me, Cl, I): sterically encumbered beta-diketiminate group 13 metal derivatives.
Auteurs : RBID : pubmed:11375697Abstract
A series of group 13 metal complexes featuring the beta-diketiminate ligand [[(C(6)H(3)-2,6-i-Pr(2))NC(Me)](2)CH](-) (i.e., [Dipp(2)nacnac](-), Dipp = C(6)H(3)-2,6-i-Pr(2)) have been prepared and spectroscopically and structurally characterized. The chloride derivatives Dipp(2)nacnacMCl(2) (M = Al (3), Ga (5), In (8)) were isolated in good yield by the reaction of 1 equiv of Dipp(2)nacnacLi.Et(2)O (2) and the respective metal halides. The iodide derivatives Dipp(2)nacnacMI(2) (M = Al (4), Ga (6), In (9)), which are useful for reduction to afford M(I) species, were made by a variety of routes. Thus, 4 was obtained by treatment of the previously reported Dipp(2)nacnacAlMe(2) with I(2), whereas the gallium analogue 6 was obtained as a product of the reaction of "GaI" with Dipp(2)nacnacLi.Et(2)O, and 9 was obtained by direct reaction of InI(3) and the lithium salt. The methyl derivatives Dipp(2)nacnacMMe(2) (M = Ga (7), In (10)), which are analogous to the previously reported Dipp(2)nacnacAlMe(2), were synthesized by the reaction of GaMe(3) with Dipp(2)nacnacH (1) or by reaction of the indium chloride derivative 8 with 2 equiv of MeMgBr in diethyl ether. The compounds 3-10 exist as colorless, air- and moisture-sensitive crystalline solids. Their X-ray crystal structures feature nearly planar C(3)N(2) arrays in the Dipp(2)nacnac ligand backbone with short C-C and C-N distances that are consistent with a delocalized structure. However, there are large dihedral angles between the C(3)N(2) plane and the N(2)M metal coordination plane which have been attributed mainly to steric effects. The relatively short M-N distances are consistent with the coordination numbers of the metals and the normal/dative character of the nitrogen ligands. The compounds were also characterized by (1)H and (13)C NMR spectroscopy. (1)H NMR data for 7 revealed equivalent methyl groups whereas the spectrum of 10 displayed two In-Me signals which indicated that ring wagging was slow on the (1)H NMR time scale.
PubMed: 11375697
Links toward previous steps (curation, corpus...)
Le document en format XML
<record><TEI><teiHeader><fileDesc><titleStmt><title xml:lang="en">Synthesis and characterization of HC[C(Me)N(C(6)H(3)-2,6-i-Pr(2))](2)MX(2) (M = Al, X = Cl, I; M = Ga, In, X = Me, Cl, I): sterically encumbered beta-diketiminate group 13 metal derivatives.</title><author><name sortKey="Stender, M" uniqKey="Stender M">M Stender</name><affiliation wicri:level="3"><nlm:affiliation>Institut für Anorganische Chemie der Universität Göttingen, Tammannstrasse 4, D-37077 Göttingen, Germany.</nlm:affiliation><country xml:lang="fr">Allemagne</country><wicri:regionArea>Institut für Anorganische Chemie der Universität Göttingen, Tammannstrasse 4, D-37077 Göttingen</wicri:regionArea><placeName><region type="land" nuts="2">Basse-Saxe</region><settlement type="city">Göttingen</settlement></placeName></affiliation></author><author><name sortKey="Eichler, B E" uniqKey="Eichler B">B E Eichler</name></author><author><name sortKey="Hardman, N J" uniqKey="Hardman N">N J Hardman</name></author><author><name sortKey="Power, P P" uniqKey="Power P">P P Power</name></author><author><name sortKey="Prust, J" uniqKey="Prust J">J Prust</name></author><author><name sortKey="Noltemeyer, M" uniqKey="Noltemeyer M">M Noltemeyer</name></author><author><name sortKey="Roesky, H W" uniqKey="Roesky H">H W Roesky</name></author></titleStmt><publicationStmt><date when="2001">2001</date><idno type="RBID">pubmed:11375697</idno><idno type="pmid">11375697</idno><idno type="wicri:Area/Main/Corpus">003A15</idno><idno type="wicri:Area/Main/Curation">003A15</idno><idno type="wicri:Area/Main/Exploration">003672</idno></publicationStmt></fileDesc><profileDesc><textClass></textClass></profileDesc></teiHeader><front><div type="abstract" xml:lang="en">A series of group 13 metal complexes featuring the beta-diketiminate ligand [[(C(6)H(3)-2,6-i-Pr(2))NC(Me)](2)CH](-) (i.e., [Dipp(2)nacnac](-), Dipp = C(6)H(3)-2,6-i-Pr(2)) have been prepared and spectroscopically and structurally characterized. The chloride derivatives Dipp(2)nacnacMCl(2) (M = Al (3), Ga (5), In (8)) were isolated in good yield by the reaction of 1 equiv of Dipp(2)nacnacLi.Et(2)O (2) and the respective metal halides. The iodide derivatives Dipp(2)nacnacMI(2) (M = Al (4), Ga (6), In (9)), which are useful for reduction to afford M(I) species, were made by a variety of routes. Thus, 4 was obtained by treatment of the previously reported Dipp(2)nacnacAlMe(2) with I(2), whereas the gallium analogue 6 was obtained as a product of the reaction of "GaI" with Dipp(2)nacnacLi.Et(2)O, and 9 was obtained by direct reaction of InI(3) and the lithium salt. The methyl derivatives Dipp(2)nacnacMMe(2) (M = Ga (7), In (10)), which are analogous to the previously reported Dipp(2)nacnacAlMe(2), were synthesized by the reaction of GaMe(3) with Dipp(2)nacnacH (1) or by reaction of the indium chloride derivative 8 with 2 equiv of MeMgBr in diethyl ether. The compounds 3-10 exist as colorless, air- and moisture-sensitive crystalline solids. Their X-ray crystal structures feature nearly planar C(3)N(2) arrays in the Dipp(2)nacnac ligand backbone with short C-C and C-N distances that are consistent with a delocalized structure. However, there are large dihedral angles between the C(3)N(2) plane and the N(2)M metal coordination plane which have been attributed mainly to steric effects. The relatively short M-N distances are consistent with the coordination numbers of the metals and the normal/dative character of the nitrogen ligands. The compounds were also characterized by (1)H and (13)C NMR spectroscopy. (1)H NMR data for 7 revealed equivalent methyl groups whereas the spectrum of 10 displayed two In-Me signals which indicated that ring wagging was slow on the (1)H NMR time scale.</div></front></TEI><pubmed><MedlineCitation Owner="NLM" Status="PubMed-not-MEDLINE"><PMID Version="1">11375697</PMID><DateCreated><Year>2001</Year><Month>05</Month><Day>28</Day></DateCreated><DateCompleted><Year>2001</Year><Month>08</Month><Day>02</Day></DateCompleted><DateRevised><Year>2003</Year><Month>10</Month><Day>31</Day></DateRevised><Article PubModel="Print"><Journal><ISSN IssnType="Print">0020-1669</ISSN><JournalIssue CitedMedium="Print"><Volume>40</Volume><Issue>12</Issue><PubDate><Year>2001</Year><Month>Jun</Month><Day>4</Day></PubDate></JournalIssue><Title>Inorganic chemistry</Title><ISOAbbreviation>Inorg Chem</ISOAbbreviation></Journal><ArticleTitle>Synthesis and characterization of HC[C(Me)N(C(6)H(3)-2,6-i-Pr(2))](2)MX(2) (M = Al, X = Cl, I; M = Ga, In, X = Me, Cl, I): sterically encumbered beta-diketiminate group 13 metal derivatives.</ArticleTitle><Pagination><MedlinePgn>2794-9</MedlinePgn></Pagination><Abstract><AbstractText>A series of group 13 metal complexes featuring the beta-diketiminate ligand [[(C(6)H(3)-2,6-i-Pr(2))NC(Me)](2)CH](-) (i.e., [Dipp(2)nacnac](-), Dipp = C(6)H(3)-2,6-i-Pr(2)) have been prepared and spectroscopically and structurally characterized. The chloride derivatives Dipp(2)nacnacMCl(2) (M = Al (3), Ga (5), In (8)) were isolated in good yield by the reaction of 1 equiv of Dipp(2)nacnacLi.Et(2)O (2) and the respective metal halides. The iodide derivatives Dipp(2)nacnacMI(2) (M = Al (4), Ga (6), In (9)), which are useful for reduction to afford M(I) species, were made by a variety of routes. Thus, 4 was obtained by treatment of the previously reported Dipp(2)nacnacAlMe(2) with I(2), whereas the gallium analogue 6 was obtained as a product of the reaction of "GaI" with Dipp(2)nacnacLi.Et(2)O, and 9 was obtained by direct reaction of InI(3) and the lithium salt. The methyl derivatives Dipp(2)nacnacMMe(2) (M = Ga (7), In (10)), which are analogous to the previously reported Dipp(2)nacnacAlMe(2), were synthesized by the reaction of GaMe(3) with Dipp(2)nacnacH (1) or by reaction of the indium chloride derivative 8 with 2 equiv of MeMgBr in diethyl ether. The compounds 3-10 exist as colorless, air- and moisture-sensitive crystalline solids. Their X-ray crystal structures feature nearly planar C(3)N(2) arrays in the Dipp(2)nacnac ligand backbone with short C-C and C-N distances that are consistent with a delocalized structure. However, there are large dihedral angles between the C(3)N(2) plane and the N(2)M metal coordination plane which have been attributed mainly to steric effects. The relatively short M-N distances are consistent with the coordination numbers of the metals and the normal/dative character of the nitrogen ligands. The compounds were also characterized by (1)H and (13)C NMR spectroscopy. (1)H NMR data for 7 revealed equivalent methyl groups whereas the spectrum of 10 displayed two In-Me signals which indicated that ring wagging was slow on the (1)H NMR time scale.</AbstractText></Abstract><AuthorList CompleteYN="Y"><Author ValidYN="Y"><LastName>Stender</LastName><ForeName>M</ForeName><Initials>M</Initials><Affiliation>Institut für Anorganische Chemie der Universität Göttingen, Tammannstrasse 4, D-37077 Göttingen, Germany.</Affiliation></Author><Author ValidYN="Y"><LastName>Eichler</LastName><ForeName>B E</ForeName><Initials>BE</Initials></Author><Author ValidYN="Y"><LastName>Hardman</LastName><ForeName>N J</ForeName><Initials>NJ</Initials></Author><Author ValidYN="Y"><LastName>Power</LastName><ForeName>P P</ForeName><Initials>PP</Initials></Author><Author ValidYN="Y"><LastName>Prust</LastName><ForeName>J</ForeName><Initials>J</Initials></Author><Author ValidYN="Y"><LastName>Noltemeyer</LastName><ForeName>M</ForeName><Initials>M</Initials></Author><Author ValidYN="Y"><LastName>Roesky</LastName><ForeName>H W</ForeName><Initials>HW</Initials></Author></AuthorList><Language>eng</Language><PublicationTypeList><PublicationType>Journal Article</PublicationType></PublicationTypeList></Article><MedlineJournalInfo><Country>United States</Country><MedlineTA>Inorg Chem</MedlineTA><NlmUniqueID>0366543</NlmUniqueID><ISSNLinking>0020-1669</ISSNLinking></MedlineJournalInfo></MedlineCitation><PubmedData><History><PubMedPubDate PubStatus="pubmed"><Year>2001</Year><Month>5</Month><Day>29</Day><Hour>10</Hour><Minute>0</Minute></PubMedPubDate><PubMedPubDate PubStatus="medline"><Year>2001</Year><Month>5</Month><Day>29</Day><Hour>10</Hour><Minute>1</Minute></PubMedPubDate><PubMedPubDate PubStatus="entrez"><Year>2001</Year><Month>5</Month><Day>29</Day><Hour>10</Hour><Minute>0</Minute></PubMedPubDate></History><PublicationStatus>ppublish</PublicationStatus><ArticleIdList><ArticleId IdType="pubmed">11375697</ArticleId><ArticleId IdType="pii">ic001311d</ArticleId></ArticleIdList></PubmedData></pubmed></record>Pour manipuler ce document sous Unix (Dilib)
EXPLOR_STEP=IndiumV2/Data/Main/Exploration
HfdSelect -h $EXPLOR_STEP/biblio.hfd -nk 003672 | SxmlIndent | more
Ou
HfdSelect -h $EXPLOR_AREA/Data/Main/Exploration/biblio.hfd -nk 003672 | SxmlIndent | more
Pour mettre un lien sur cette page dans le réseau Wicri
{{Explor lien
|wiki= *** parameter Area/wikiCode missing ***
|area= IndiumV2
|flux= Main
|étape= Exploration
|type= RBID
|clé= pubmed:11375697
|texte= Synthesis and characterization of HC[C(Me)N(C(6)H(3)-2,6-i-Pr(2))](2)MX(2) (M = Al, X = Cl, I; M = Ga, In, X = Me, Cl, I): sterically encumbered beta-diketiminate group 13 metal derivatives.
}}
Pour générer des pages wiki
HfdIndexSelect -h $EXPLOR_AREA/Data/Main/Exploration/RBID.i -Sk "pubmed:11375697" \
| HfdSelect -Kh $EXPLOR_AREA/Data/Main/Exploration/biblio.hfd \
| NlmPubMed2Wicri -a IndiumV2
| This area was generated with Dilib version V0.5.76. |  |