Synthesis, Crystal Structure and Spectroscopic Characterisation of Mono‐ and Dinuclear 5,5‐Diethylbarbiturato Complexes of Chromium(0) and Rhenium(I)
Identifieur interne : 000B34 ( Istex/Corpus ); précédent : 000B33; suivant : 000B35Synthesis, Crystal Structure and Spectroscopic Characterisation of Mono‐ and Dinuclear 5,5‐Diethylbarbiturato Complexes of Chromium(0) and Rhenium(I)
Auteurs : Nadera Haque ; J. Nicolas Roedel ; Ingo-Peter LorenzSource :
- ZAAC ‐ Journal of Inorganic and General Chemistry [ 0044-2313 ] ; 2009-03.
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.
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DOI: 10.1002/zaac.200801342
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ISTEX:6B892EBA05B0440F2230A6F3AF0D521BACC6FF6FLe document en format XML
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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. 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Nicolas Roedel</name><affiliations><json:string>Department Chemie und Biochemie, Ludwig‐Maximilians‐Universität München, Butenandtstraóe 5–13 (Haus D), 81377 München, Germany, Fax: +49‐89‐2180‐77867</json:string></affiliations></json:item><json:item><name>Ingo‐Peter Lorenz Prof. Dr.</name><affiliations><json:string>Department Chemie und Biochemie, Ludwig‐Maximilians‐Universität München, Butenandtstraóe 5–13 (Haus D), 81377 München, Germany, Fax: +49‐89‐2180‐77867</json:string><json:string>E-mail: ipl@cup.uni‐muenchen.de</json:string></affiliations></json:item></author><subject><json:item><lang><json:string>eng</json:string></lang><value>Barbiturates</value></json:item><json:item><lang><json:string>eng</json:string></lang><value>Chromium</value></json:item><json:item><lang><json:string>eng</json:string></lang><value>N ligands</value></json:item><json:item><lang><json:string>eng</json:string></lang><value>Rhenium</value></json:item><json:item><lang><json:string>eng</json:string></lang><value>Solid‐state structures</value></json:item></subject><articleId><json:string>ZAAC200801342</json:string></articleId><language><json:string>eng</json:string></language><originalGenre><json:string>article</json:string></originalGenre><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. 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KGaA, Weinheim</p></availability><date>2009</date></publicationStmt><sourceDesc><biblStruct type="inbook"><analytic><title level="a" type="main" xml:lang="en">Synthesis, Crystal Structure and Spectroscopic Characterisation of Mono‐ and Dinuclear 5,5‐Diethylbarbiturato Complexes of Chromium(0) and Rhenium(I)</title><author xml:id="author-1"><persName><forename type="first">Nadera</forename><surname>Haque</surname></persName><affiliation>Department Chemie und Biochemie, Ludwig‐Maximilians‐Universität München, Butenandtstraóe 5–13 (Haus D), 81377 München, Germany, Fax: +49‐89‐2180‐77867</affiliation></author><author xml:id="author-2"><persName><forename type="first">J. 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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. 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Chem.</title></titleGroup></publicationMeta><publicationMeta level="part" position="30"><doi origin="wiley" registered="yes">10.1002/zaac.v635:3</doi><numberingGroup><numbering type="journalVolume" number="635">635</numbering><numbering type="journalIssue">3</numbering></numberingGroup><coverDate startDate="2009-03">March 2009</coverDate></publicationMeta><publicationMeta level="unit" type="article" position="19" status="forIssue"><doi origin="wiley" registered="yes">10.1002/zaac.200801342</doi><idGroup><id type="unit" value="ZAAC200801342"></id></idGroup><countGroup><count type="pageTotal" number="7"></count></countGroup><titleGroup><title type="articleCategory">Article</title><title type="tocHeading1">Articles</title></titleGroup><copyright ownership="publisher">Copyright © 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim</copyright><eventGroup><event type="manuscriptReceived" date="2008-10-30"></event><event type="firstOnline" date="2009-01-20"></event><event type="publishedOnlineFinalForm" date="2009-03-09"></event><event type="publishedOnlineAcceptedOrEarlyUnpaginated" date="2009-01-20"></event><event type="xmlConverted" agent="Converter:JWSART34_TO_WML3G version:2.4.7 mode:FullText source:HeaderRef result:HeaderRef" date="2011-02-24"></event><event type="xmlConverted" agent="Converter:WILEY_ML3G_TO_WILEY_ML3GV2 version:3.8.8" date="2014-02-11"></event><event type="xmlConverted" agent="Converter:WML3G_To_WML3G version:4.1.7 mode:FullText,remove_FC" date="2014-11-04"></event></eventGroup><numberingGroup><numbering type="pageFirst">496</numbering><numbering type="pageLast">502</numbering></numberingGroup><linkGroup><link type="toTypesetVersion" href="file:ZAAC.ZAAC200801342.pdf"></link></linkGroup></publicationMeta><contentMeta><countGroup><count type="figureTotal" number="4"></count><count type="tableTotal" number="1"></count><count type="referenceTotal" number="24"></count></countGroup><titleGroup><title type="main" xml:lang="en">Synthesis, Crystal Structure and Spectroscopic Characterisation of Mono‐ and Dinuclear 5,5‐Diethylbarbiturato Complexes of Chromium(0) and Rhenium(I)</title></titleGroup><creators><creator xml:id="au1" creatorRole="author" affiliationRef="#a1"><personName><givenNames>Nadera</givenNames><familyName>Haque</familyName></personName></creator><creator xml:id="au2" creatorRole="author" affiliationRef="#a1"><personName><givenNames>J. Nicolas</givenNames><familyName>Roedel</familyName></personName></creator><creator xml:id="au3" creatorRole="author" affiliationRef="#a1"><personName><givenNames>Ingo‐Peter</givenNames><familyName>Lorenz</familyName><degrees>Prof. Dr.</degrees></personName><contactDetails><email normalForm="ipl@cup.uni-muenchen.de">ipl@cup.uni‐muenchen.de</email></contactDetails></creator></creators><affiliationGroup><affiliation xml:id="a1" countryCode="DE" type="organization"><unparsedAffiliation>Department Chemie und Biochemie, Ludwig‐Maximilians‐Universität München, Butenandtstraóe 5–13 (Haus D), 81377 München, Germany, Fax: +49‐89‐2180‐77867</unparsedAffiliation></affiliation></affiliationGroup><keywordGroup xml:lang="en" type="author"><keyword xml:id="kwd1">Barbiturates</keyword><keyword xml:id="kwd2">Chromium</keyword><keyword xml:id="kwd3">N ligands</keyword><keyword xml:id="kwd4">Rhenium</keyword><keyword xml:id="kwd5">Solid‐state structures</keyword></keywordGroup><abstractGroup><abstract type="main" xml:lang="en"><title type="main">Abstract</title><p>Addition of 5,5‐diethylbarbituric acid (H<sub>2</sub>debarb, <b>1</b>) to [CpCr(NO)<sub>2</sub>Cl], [Re(CO)<sub>5</sub>Br] or [(PPh<sub>3</sub>)Re(CO)<sub>4</sub>Br] in the presence of triethylamine and AgO<sub>3</sub>SCF<sub>3</sub> (= AgOTf) resulted in the mono‐barbiturato complexes [CpCr(NO)<sub>2</sub>(Hdebarb)] (<b>2</b>), [PPh<sub>3</sub>Re(CO)<sub>4</sub>(Hdebarb)] (<b>3</b>) and [Re(CO)<sub>5</sub>(Hdebarb)] (<b>4</b>), respectively. Bis‐barbiturato complex [{(CO)<sub>5</sub>Re}<sub>2</sub>(debarb)] (<b>5</b>) 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, AgO<sub>3</sub>SCF<sub>3</sub> must be used additionally to cleave off bromide. All of the complexes were fully characterised by means of IR, mass and <sup>1</sup>H, <sup>13</sup>C and <sup>31</sup>P 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 (<b>2</b>) or pseudo‐octahedral (<b>3</b>–<b>5</b>) configuration around the metal atom. In all complexes the ring system of the Hdebarb ligand is essentially planar.</p></abstract></abstractGroup></contentMeta></header></component></istex:document></istex:metadataXml><mods version="3.6"><titleInfo lang="en"><title>Synthesis, Crystal Structure and Spectroscopic Characterisation of Mono‐ and Dinuclear 5,5‐Diethylbarbiturato Complexes of Chromium(0) and Rhenium(I)</title></titleInfo><titleInfo type="alternative" contentType="CDATA" lang="en"><title>Synthesis, Crystal Structure and Spectroscopic Characterisation of Mono‐ and Dinuclear 5,5‐Diethylbarbiturato Complexes of Chromium(0) and Rhenium(I)</title></titleInfo><name type="personal"><namePart type="given">Nadera</namePart><namePart type="family">Haque</namePart><affiliation>Department Chemie und Biochemie, Ludwig‐Maximilians‐Universität München, Butenandtstraóe 5–13 (Haus D), 81377 München, Germany, Fax: +49‐89‐2180‐77867</affiliation><role><roleTerm type="text">author</roleTerm></role></name><name type="personal"><namePart type="given">J. Nicolas</namePart><namePart type="family">Roedel</namePart><affiliation>Department Chemie und Biochemie, Ludwig‐Maximilians‐Universität München, Butenandtstraóe 5–13 (Haus D), 81377 München, Germany, Fax: +49‐89‐2180‐77867</affiliation><role><roleTerm type="text">author</roleTerm></role></name><name type="personal"><namePart type="given">Ingo‐Peter</namePart><namePart type="family">Lorenz</namePart><namePart type="termsOfAddress">Prof. Dr.</namePart><affiliation>Department Chemie und Biochemie, Ludwig‐Maximilians‐Universität München, Butenandtstraóe 5–13 (Haus D), 81377 München, Germany, Fax: +49‐89‐2180‐77867</affiliation><affiliation>E-mail: ipl@cup.uni‐muenchen.de</affiliation><role><roleTerm type="text">author</roleTerm></role></name><typeOfResource>text</typeOfResource><genre type="article" displayLabel="article"></genre><originInfo><publisher>WILEY‐VCH Verlag</publisher><place><placeTerm type="text">Weinheim</placeTerm></place><dateIssued encoding="w3cdtf">2009-03</dateIssued><dateCaptured encoding="w3cdtf">2008-10-30</dateCaptured><copyrightDate encoding="w3cdtf">2009</copyrightDate></originInfo><language><languageTerm type="code" authority="rfc3066">en</languageTerm><languageTerm type="code" authority="iso639-2b">eng</languageTerm></language><physicalDescription><internetMediaType>text/html</internetMediaType><extent unit="figures">4</extent><extent unit="tables">1</extent><extent unit="references">24</extent></physicalDescription><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.</abstract><subject lang="en"><genre>keywords</genre><topic>Barbiturates</topic><topic>Chromium</topic><topic>N ligands</topic><topic>Rhenium</topic><topic>Solid‐state structures</topic></subject><relatedItem type="host"><titleInfo><title>ZAAC ‐ Journal of Inorganic and General Chemistry</title></titleInfo><titleInfo type="abbreviated"><title>Z. anorg. allg. Chem.</title></titleInfo><genre type="journal">journal</genre><subject><genre>article-category</genre><topic>Article</topic></subject><identifier type="ISSN">0044-2313</identifier><identifier type="eISSN">1521-3749</identifier><identifier type="DOI">10.1002/(ISSN)1521-3749</identifier><identifier type="PublisherID">ZAAC</identifier><part><date>2009</date><detail type="volume"><caption>vol.</caption><number>635</number></detail><detail type="issue"><caption>no.</caption><number>3</number></detail><extent unit="pages"><start>496</start><end>502</end><total>7</total></extent></part></relatedItem><identifier type="istex">6B892EBA05B0440F2230A6F3AF0D521BACC6FF6F</identifier><identifier type="DOI">10.1002/zaac.200801342</identifier><identifier type="ArticleID">ZAAC200801342</identifier><accessCondition type="use and reproduction" contentType="copyright">Copyright © 2009 WILEY‐VCH Verlag GmbH & Co. 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