Synthesis, Crystal Structure and Spectroscopic Characterisation of Mono‐ and Dinuclear 5,5‐Diethylbarbiturato Complexes of Chromium(0) and Rhenium(I)
Identifieur interne : 000532 ( Main/Exploration ); précédent : 000531; suivant : 000533Synthesis, Crystal Structure and Spectroscopic Characterisation of Mono‐ and Dinuclear 5,5‐Diethylbarbiturato Complexes of Chromium(0) and Rhenium(I)
Auteurs : Nadera Haque [Allemagne] ; J. Nicolas Roedel [Allemagne] ; Ingo-Peter Lorenz [Allemagne]Source :
- ZAAC ‐ Journal of Inorganic and General Chemistry [ 0044-2313 ] ; 2009-03.
Descripteurs français
- Wicri :
- topic : Chrome.
English descriptors
- KwdEn :
- Teeft :
- Acta, Acta crystallogr, Agotf, Allg, Anorg, Barbiturate, Bond angle, Bond angles, Bond lengths, Carbonyl, Carbonyl groups, Carbonyl ligands, Chcl3, Chem, Chemical shifts, Cohdebarb, Colourless crystals, Crystal data, Crystal structure, Disordered protons, Elemental analysis, Ethyl groups, Gmbh, Good agreement, Hdebarb, Hdebarb ligand, Hydrogen atoms, Kgaa, Ligand, Mass spectra, Mass spectrum, Metal atom, Metal complexes, Mmol, Molecular structure, Pph3, Pph3 ligand, Reco, Rhenium, Rhenium complexes, Room temperature, Show multiplets, Spectroscopic characterisation, Structural refinement, Structure analysis, Thermal ellipsoids, Verlag, Verlag gmbh, Weinheim.
Abstract
Addition of 5,5‐diethylbarbituric acid (H2debarb, 1) to [CpCr(NO)2Cl], [Re(CO)5Br] or [(PPh3)Re(CO)4Br] in the presence of triethylamine and AgO3SCF3 (= AgOTf) resulted in the mono‐barbiturato complexes [CpCr(NO)2(Hdebarb)] (2), [PPh3Re(CO)4(Hdebarb)] (3) and [Re(CO)5(Hdebarb)] (4), respectively. Bis‐barbiturato complex [{(CO)5Re}2(debarb)] (5) with a doubly deprotonated barbiturate dianion formed when a molar ratio of metal complex to ligand of 2:1 was used. In the case of the rhenium complexes, AgO3SCF3 must be used additionally to cleave off bromide. All of the complexes were fully characterised by means of IR, mass and 1H, 13C and 31P NMR spectra and elemental analysis. In addition, their solid‐state structures were determined by single‐crystal X‐ray diffraction studies. The complexes exhibit distorted pseudo‐tetrahedral (2) or pseudo‐octahedral (3–5) configuration around the metal atom. In all complexes the ring system of the Hdebarb ligand is essentially planar.
Url:
DOI: 10.1002/zaac.200801342
Affiliations:
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Chem.</title><idno type="ISSN">0044-2313</idno><idno type="eISSN">1521-3749</idno><imprint><publisher>WILEY‐VCH Verlag</publisher><pubPlace>Weinheim</pubPlace><date type="published" when="2009-03">2009-03</date><biblScope unit="volume">635</biblScope><biblScope unit="issue">3</biblScope><biblScope unit="page" from="496">496</biblScope><biblScope unit="page" to="502">502</biblScope></imprint><idno type="ISSN">0044-2313</idno></series><idno type="istex">6B892EBA05B0440F2230A6F3AF0D521BACC6FF6F</idno><idno type="DOI">10.1002/zaac.200801342</idno><idno type="ArticleID">ZAAC200801342</idno></biblStruct></sourceDesc><seriesStmt><idno type="ISSN">0044-2313</idno></seriesStmt></fileDesc><profileDesc><textClass><keywords scheme="KwdEn" xml:lang="en"><term>Barbiturates</term><term>Chromium</term><term>N ligands</term><term>Rhenium</term><term>Solid‐state structures</term></keywords><keywords scheme="Teeft" xml:lang="en"><term>Acta</term><term>Acta crystallogr</term><term>Agotf</term><term>Allg</term><term>Anorg</term><term>Barbiturate</term><term>Bond angle</term><term>Bond angles</term><term>Bond lengths</term><term>Carbonyl</term><term>Carbonyl groups</term><term>Carbonyl ligands</term><term>Chcl3</term><term>Chem</term><term>Chemical shifts</term><term>Cohdebarb</term><term>Colourless crystals</term><term>Crystal data</term><term>Crystal structure</term><term>Disordered protons</term><term>Elemental analysis</term><term>Ethyl groups</term><term>Gmbh</term><term>Good agreement</term><term>Hdebarb</term><term>Hdebarb ligand</term><term>Hydrogen atoms</term><term>Kgaa</term><term>Ligand</term><term>Mass spectra</term><term>Mass spectrum</term><term>Metal atom</term><term>Metal complexes</term><term>Mmol</term><term>Molecular structure</term><term>Pph3</term><term>Pph3 ligand</term><term>Reco</term><term>Rhenium</term><term>Rhenium complexes</term><term>Room temperature</term><term>Show multiplets</term><term>Spectroscopic characterisation</term><term>Structural refinement</term><term>Structure analysis</term><term>Thermal ellipsoids</term><term>Verlag</term><term>Verlag gmbh</term><term>Weinheim</term></keywords><keywords scheme="Wicri" type="topic" xml:lang="fr"><term>Chrome</term></keywords></textClass><langUsage><language ident="en">en</language></langUsage></profileDesc></teiHeader><front><div type="abstract">Addition of 5,5‐diethylbarbituric acid (H2debarb, 1) to [CpCr(NO)2Cl], [Re(CO)5Br] or [(PPh3)Re(CO)4Br] in the presence of triethylamine and AgO3SCF3 (= AgOTf) resulted in the mono‐barbiturato complexes [CpCr(NO)2(Hdebarb)] (2), [PPh3Re(CO)4(Hdebarb)] (3) and [Re(CO)5(Hdebarb)] (4), respectively. Bis‐barbiturato complex [{(CO)5Re}2(debarb)] (5) with a doubly deprotonated barbiturate dianion formed when a molar ratio of metal complex to ligand of 2:1 was used. In the case of the rhenium complexes, AgO3SCF3 must be used additionally to cleave off bromide. All of the complexes were fully characterised by means of IR, mass and 1H, 13C and 31P NMR spectra and elemental analysis. In addition, their solid‐state structures were determined by single‐crystal X‐ray diffraction studies. The complexes exhibit distorted pseudo‐tetrahedral (2) or pseudo‐octahedral (3–5) configuration around the metal atom. In all complexes the ring system of the Hdebarb ligand is essentially planar.</div></front></TEI><affiliations><list><country><li>Allemagne</li></country><region><li>Bavière</li><li>District de Haute-Bavière</li></region><settlement><li>Munich</li></settlement><orgName><li>Université Louis-et-Maximilien de Munich</li></orgName></list><tree><country name="Allemagne"><region name="Bavière"><name sortKey="Haque, Nadera" sort="Haque, Nadera" uniqKey="Haque N" first="Nadera" last="Haque">Nadera Haque</name></region><name sortKey="Lorenz, Ingo Eter" sort="Lorenz, Ingo Eter" uniqKey="Lorenz I" first="Ingo-Peter" last="Lorenz">Ingo-Peter Lorenz</name><name sortKey="Lorenz, Ingo Eter" sort="Lorenz, Ingo Eter" uniqKey="Lorenz I" first="Ingo-Peter" last="Lorenz">Ingo-Peter Lorenz</name><name sortKey="Roedel, J Nicolas" sort="Roedel, J Nicolas" uniqKey="Roedel J" first="J. Nicolas" last="Roedel">J. Nicolas Roedel</name></country></tree></affiliations></record>Pour manipuler ce document sous Unix (Dilib)
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