Tris(pyrazolyl)methanesulfonate (Tpms) − A Versatile Alternative to Tris(pyrazolyl)borate in Rhodium(I) Chemistry
Identifieur interne : 003009 ( Istex/Curation ); précédent : 003008; suivant : 003010Tris(pyrazolyl)methanesulfonate (Tpms) − A Versatile Alternative to Tris(pyrazolyl)borate in Rhodium(I) Chemistry
Auteurs : Wolfgang Kl Ui [Allemagne] ; Daniel Schramm [Allemagne] ; Wilfried Peters [Allemagne] ; Gerd Rheinwald [Allemagne] ; Heinrich Lang [Allemagne]Source :
- European Journal of Inorganic Chemistry [ 1434-1948 ] ; 2001-06.
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Abstract
Thallium(I) tris(pyrazol‐1‐yl)methanesulfonate (TlTpms) has been prepared as a new versatile precursor for Tpms complexes. TlTpms readily reacts with the rhodium(I) complexes [Rh(LL)Cl]2 [LL = (CO)2, cod, nbd] to give the corresponding TpmsRh(LL) complexes [LL = (CO)2 (2a), cod (3), and nbd (4)]. In solution, 2a reversibly forms the binuclear complex TpmsRh(µ‐CO)3RhTpms (2b). 3 and 4 react with CO to form 2a. TpmsRh(CO)(PR3) complexes [PR3 = PPh3 (5a), PMe3 (5b), PCy3 (5d), P(Ph)2(PhSO3K) (5e)] have been obtained by reaction of 2a with the corresponding phosphanes. The solid‐state structures of 2a, 3, 4, and 5a have been determined by X‐ray analysis. 2a, 3, and 5a have square‐planar geometries with the Tpms ligand coordinating in a κ2 mode. The non‐coordinating pyrazole ring faces either away from (structure 2a) or towards the rhodium atom (structures 3 and 5a). 4 has a trigonal‐bipyramidal coordination geometry with a genuine κ3‐bonded Tpms ligand. The non‐rigid behaviour of the (Tpms)rhodium complexes has been followed by variable‐temperature NMR studies. IR studies on 2a and 5a−e show that Tpms is a weakly donating ligand, comparable to the Tp CF 3,Me and Tp CF 3,CF 3 ligands. Compound 5e is soluble and stable in dilute acids, showing that Tpms, unlike the Tp ligand, is hydrolytically stable.
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DOI: 10.1002/1099-0682(200106)2001:6<1415::AID-EJIC1415>3.0.CO;2-Z
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Düsseldorf</wicri:regionArea></affiliation></author><author><name sortKey="Peters, Wilfried" sort="Peters, Wilfried" uniqKey="Peters W" first="Wilfried" last="Peters">Wilfried Peters</name><affiliation wicri:level="1"><mods:affiliation>Institut für Anorganische Chemie und Strukturchemie der Universität Düsseldorf, Universitätsstraße 1, 40225 Düsseldorf, Germany</mods:affiliation><country xml:lang="fr">Allemagne</country><wicri:regionArea>Institut für Anorganische Chemie und Strukturchemie der Universität Düsseldorf, Universitätsstraße 1, 40225 Düsseldorf</wicri:regionArea></affiliation></author><author><name sortKey="Rheinwald, Gerd" sort="Rheinwald, Gerd" uniqKey="Rheinwald G" first="Gerd" last="Rheinwald">Gerd Rheinwald</name><affiliation wicri:level="1"><mods:affiliation>Lehrstuhl für Anorganische Chemie, Technische Universität Chemnitz, Straße der Nationen 62, 09107 Chemnitz, Germany</mods:affiliation><country xml:lang="fr">Allemagne</country><wicri:regionArea>Lehrstuhl für 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J. Inorg. Chem.</title><idno type="ISSN">1434-1948</idno><idno type="eISSN">1099-0682</idno><imprint><publisher>WILEY‐VCH Verlag GmbH</publisher><pubPlace>Weinheim</pubPlace><date type="published" when="2001-06">2001-06</date><biblScope unit="volume">2001</biblScope><biblScope unit="issue">6</biblScope><biblScope unit="page" from="1415">1415</biblScope><biblScope unit="page" to="1424">1424</biblScope></imprint><idno type="ISSN">1434-1948</idno></series><idno type="istex">D5FD470FAE7A0384FBF653138DFE310233E9029D</idno><idno type="DOI">10.1002/1099-0682(200106)2001:6<1415::AID-EJIC1415>3.0.CO;2-Z</idno><idno type="ArticleID">EJIC1415</idno></biblStruct></sourceDesc><seriesStmt><idno type="ISSN">1434-1948</idno></seriesStmt></fileDesc><profileDesc><textClass><keywords scheme="KwdEn" xml:lang="en"><term>Carbonyl complexes</term><term>Fluxionality</term><term>N ligands</term><term>Rhodium</term><term>Tripodal ligands</term></keywords></textClass><langUsage><language ident="en">en</language></langUsage></profileDesc></teiHeader><front><div type="abstract" xml:lang="en">Thallium(I) tris(pyrazol‐1‐yl)methanesulfonate (TlTpms) has been prepared as a new versatile precursor for Tpms complexes. TlTpms readily reacts with the rhodium(I) complexes [Rh(LL)Cl]2 [LL = (CO)2, cod, nbd] to give the corresponding TpmsRh(LL) complexes [LL = (CO)2 (2a), cod (3), and nbd (4)]. In solution, 2a reversibly forms the binuclear complex TpmsRh(µ‐CO)3RhTpms (2b). 3 and 4 react with CO to form 2a. TpmsRh(CO)(PR3) complexes [PR3 = PPh3 (5a), PMe3 (5b), PCy3 (5d), P(Ph)2(PhSO3K) (5e)] have been obtained by reaction of 2a with the corresponding phosphanes. The solid‐state structures of 2a, 3, 4, and 5a have been determined by X‐ray analysis. 2a, 3, and 5a have square‐planar geometries with the Tpms ligand coordinating in a κ2 mode. The non‐coordinating pyrazole ring faces either away from (structure 2a) or towards the rhodium atom (structures 3 and 5a). 4 has a trigonal‐bipyramidal coordination geometry with a genuine κ3‐bonded Tpms ligand. The non‐rigid behaviour of the (Tpms)rhodium complexes has been followed by variable‐temperature NMR studies. IR studies on 2a and 5a−e show that Tpms is a weakly donating ligand, comparable to the Tp CF 3,Me and Tp CF 3,CF 3 ligands. Compound 5e is soluble and stable in dilute acids, showing that Tpms, unlike the Tp ligand, is hydrolytically stable.</div></front></TEI></record>Pour manipuler ce document sous Unix (Dilib)
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