Copper(II) and triphenylphosphine copper(I) ethylene glycol carboxylates: synthesis, characterisation and copper nanoparticle generation
Ethylene glycol-functionalised copper(II) carboxylates Cu[O2CCR2(OC2H4)nOCH3]2 (n = 0-3; R = H, Me) (2a-e) have been prepared by the reaction of [Cu2(OAc)4·2H2O] with CH3O(C2H4O)nCR2CO2H (1a-e). Upon reduction of 2a-e with triphenylphosphine, the corresponding tris(triphenylphosphine)copper(I) compl...
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| Veröffentlicht in: | Dalton transactions : an international journal of inorganic chemistry 2013-01, Vol.42 (44), p.15599-15609 |
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| container_title | Dalton transactions : an international journal of inorganic chemistry |
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| creator | Adner, David Möckel, Stefan Korb, Marcus Buschbeck, Roy Rüffer, Tobias Schulze, Steffen Mertens, Lutz Hietschold, Michael Mehring, Michael Lang, Heinrich |
| description | Ethylene glycol-functionalised copper(II) carboxylates Cu[O2CCR2(OC2H4)nOCH3]2 (n = 0-3; R = H, Me) (2a-e) have been prepared by the reaction of [Cu2(OAc)4·2H2O] with CH3O(C2H4O)nCR2CO2H (1a-e). Upon reduction of 2a-e with triphenylphosphine, the corresponding tris(triphenylphosphine)copper(I) complexes 3a-e were obtained, which could be converted to the bis(triphenylphosphine)copper(I) complexes 4a-e by removal of one phosphine ligand. Based on IR spectroscopy and single crystal X-ray structure analysis the binding motif of the carboxylato group on the copper ion is discussed. DSC, TG and TG-MS experiments were performed to analyse the thermal decomposition mechanism of 2-4. Complex 4c was used as a precursor for the generation of copper nanoparticles by thermal decomposition in hexadecylamine without the need of any further reactants. Depending on the precursor concentration, spherical copper nanoparticles with a mean diameter ranging from 10 to 85 nm as well as nanorods with a length of up to 1.3 μm (aspect ratios ranging between 2 and 32) were obtained. Electron diffraction analysis of the rods suggested that they consist of five domains which are arranged around a fivefold rotational axis. |
| doi_str_mv | 10.1039/c3dt51913a |
| format | Article |
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Upon reduction of 2a-e with triphenylphosphine, the corresponding tris(triphenylphosphine)copper(I) complexes 3a-e were obtained, which could be converted to the bis(triphenylphosphine)copper(I) complexes 4a-e by removal of one phosphine ligand. Based on IR spectroscopy and single crystal X-ray structure analysis the binding motif of the carboxylato group on the copper ion is discussed. DSC, TG and TG-MS experiments were performed to analyse the thermal decomposition mechanism of 2-4. Complex 4c was used as a precursor for the generation of copper nanoparticles by thermal decomposition in hexadecylamine without the need of any further reactants. Depending on the precursor concentration, spherical copper nanoparticles with a mean diameter ranging from 10 to 85 nm as well as nanorods with a length of up to 1.3 μm (aspect ratios ranging between 2 and 32) were obtained. Electron diffraction analysis of the rods suggested that they consist of five domains which are arranged around a fivefold rotational axis.</description><identifier>ISSN: 1477-9226</identifier><identifier>EISSN: 1477-9234</identifier><identifier>DOI: 10.1039/c3dt51913a</identifier><identifier>PMID: 24030202</identifier><language>eng</language><publisher>England</publisher><subject>Carboxylates ; Copper ; COPPER IONS ; DECOMPOSITION ; ETHYLENE ; ETHYLENE GLYCOL ; MICROSTRUCTURES ; Nanoparticles ; Nanorods ; Nanostructure ; PARTICLES ; Phosphines ; Precursors ; SINGLE CRYSTALS ; Thermal decomposition</subject><ispartof>Dalton transactions : an international journal of inorganic chemistry, 2013-01, Vol.42 (44), p.15599-15609</ispartof><lds50>peer_reviewed</lds50><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-c353t-29113403a36fcf5acdf957bd5f201b1257892e3bdcdf1c7f95e039b1813dd4eb3</citedby><cites>FETCH-LOGICAL-c353t-29113403a36fcf5acdf957bd5f201b1257892e3bdcdf1c7f95e039b1813dd4eb3</cites></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><link.rule.ids>314,780,784,27924,27925</link.rule.ids><backlink>$$Uhttps://www.ncbi.nlm.nih.gov/pubmed/24030202$$D View this record in MEDLINE/PubMed$$Hfree_for_read</backlink></links><search><creatorcontrib>Adner, David</creatorcontrib><creatorcontrib>Möckel, Stefan</creatorcontrib><creatorcontrib>Korb, Marcus</creatorcontrib><creatorcontrib>Buschbeck, Roy</creatorcontrib><creatorcontrib>Rüffer, Tobias</creatorcontrib><creatorcontrib>Schulze, Steffen</creatorcontrib><creatorcontrib>Mertens, Lutz</creatorcontrib><creatorcontrib>Hietschold, Michael</creatorcontrib><creatorcontrib>Mehring, Michael</creatorcontrib><creatorcontrib>Lang, Heinrich</creatorcontrib><title>Copper(II) and triphenylphosphine copper(I) ethylene glycol carboxylates: synthesis, characterisation and copper nanoparticle generation</title><title>Dalton transactions : an international journal of inorganic chemistry</title><addtitle>Dalton Trans</addtitle><description>Ethylene glycol-functionalised copper(II) carboxylates Cu[O2CCR2(OC2H4)nOCH3]2 (n = 0-3; R = H, Me) (2a-e) have been prepared by the reaction of [Cu2(OAc)4·2H2O] with CH3O(C2H4O)nCR2CO2H (1a-e). Upon reduction of 2a-e with triphenylphosphine, the corresponding tris(triphenylphosphine)copper(I) complexes 3a-e were obtained, which could be converted to the bis(triphenylphosphine)copper(I) complexes 4a-e by removal of one phosphine ligand. Based on IR spectroscopy and single crystal X-ray structure analysis the binding motif of the carboxylato group on the copper ion is discussed. DSC, TG and TG-MS experiments were performed to analyse the thermal decomposition mechanism of 2-4. Complex 4c was used as a precursor for the generation of copper nanoparticles by thermal decomposition in hexadecylamine without the need of any further reactants. Depending on the precursor concentration, spherical copper nanoparticles with a mean diameter ranging from 10 to 85 nm as well as nanorods with a length of up to 1.3 μm (aspect ratios ranging between 2 and 32) were obtained. Electron diffraction analysis of the rods suggested that they consist of five domains which are arranged around a fivefold rotational axis.</description><subject>Carboxylates</subject><subject>Copper</subject><subject>COPPER IONS</subject><subject>DECOMPOSITION</subject><subject>ETHYLENE</subject><subject>ETHYLENE GLYCOL</subject><subject>MICROSTRUCTURES</subject><subject>Nanoparticles</subject><subject>Nanorods</subject><subject>Nanostructure</subject><subject>PARTICLES</subject><subject>Phosphines</subject><subject>Precursors</subject><subject>SINGLE CRYSTALS</subject><subject>Thermal decomposition</subject><issn>1477-9226</issn><issn>1477-9234</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2013</creationdate><recordtype>article</recordtype><recordid>eNqNkc9OwzAMhyMEYjC48ACoR4YYJHGzEm5o4s-kSVzgXKWpS4uypiSZRN-AxyZsYxzhZMv-9Mnyj5ATRi8ZBXmloQyCSQZqhxywNMvGkkO6u-35ZEAOvX-jlHMq-D4Z8JQC5ZQfkM-p7Tp0Z7PZKFFtmQTXdDW2velq67u6aTHRG2KUYKh7g3H0anptTaKVK-xHb1RAf5P4vg01-sZfJLpWTumArvEqNLZdqdeepFWt7ZQLjTZRFG1uhRyRvUoZj8ebOiQv93fP08fx_OlhNr2djzUICGMuGYN4vYJJpSuhdFlJkRWlqDhlBeMiu5YcoSjjguksLjG-qGDXDMoyxQKG5Gzt7Zx9X6IP-aLxGo1RLdqlz1kGlGYy_vNvNJ2kYgIS6D_QNAXJmeARPV-j2lnvHVZ555qFcn3OaP6dZ_6bZ4RPN95lscByi_4ECF8LOZ2T</recordid><startdate>20130101</startdate><enddate>20130101</enddate><creator>Adner, David</creator><creator>Möckel, Stefan</creator><creator>Korb, Marcus</creator><creator>Buschbeck, Roy</creator><creator>Rüffer, Tobias</creator><creator>Schulze, Steffen</creator><creator>Mertens, Lutz</creator><creator>Hietschold, Michael</creator><creator>Mehring, Michael</creator><creator>Lang, Heinrich</creator><scope>NPM</scope><scope>AAYXX</scope><scope>CITATION</scope><scope>7X8</scope><scope>7U5</scope><scope>8FD</scope><scope>H8G</scope><scope>JG9</scope><scope>L7M</scope><scope>7SR</scope><scope>8BQ</scope></search><sort><creationdate>20130101</creationdate><title>Copper(II) and triphenylphosphine copper(I) ethylene glycol carboxylates: synthesis, characterisation and copper nanoparticle generation</title><author>Adner, David ; 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Upon reduction of 2a-e with triphenylphosphine, the corresponding tris(triphenylphosphine)copper(I) complexes 3a-e were obtained, which could be converted to the bis(triphenylphosphine)copper(I) complexes 4a-e by removal of one phosphine ligand. Based on IR spectroscopy and single crystal X-ray structure analysis the binding motif of the carboxylato group on the copper ion is discussed. DSC, TG and TG-MS experiments were performed to analyse the thermal decomposition mechanism of 2-4. Complex 4c was used as a precursor for the generation of copper nanoparticles by thermal decomposition in hexadecylamine without the need of any further reactants. Depending on the precursor concentration, spherical copper nanoparticles with a mean diameter ranging from 10 to 85 nm as well as nanorods with a length of up to 1.3 μm (aspect ratios ranging between 2 and 32) were obtained. Electron diffraction analysis of the rods suggested that they consist of five domains which are arranged around a fivefold rotational axis.</abstract><cop>England</cop><pmid>24030202</pmid><doi>10.1039/c3dt51913a</doi><tpages>11</tpages></addata></record> |
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| source | Royal Society Of Chemistry Journals 2008-; Alma/SFX Local Collection |
| subjects | Carboxylates Copper COPPER IONS DECOMPOSITION ETHYLENE ETHYLENE GLYCOL MICROSTRUCTURES Nanoparticles Nanorods Nanostructure PARTICLES Phosphines Precursors SINGLE CRYSTALS Thermal decomposition |
| title | Copper(II) and triphenylphosphine copper(I) ethylene glycol carboxylates: synthesis, characterisation and copper nanoparticle generation |
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