Preparation and Characterization of the Triflate Complex [Cp(dppe)FeOSO2CF3]: A Convenient Access to Labile Five‐ and Six‐Coordinate Iron(I) and Iron(II) Complexes
Treatment of the iron hydride [Cp*(dppe)FeH] (1) with methyl triflate (CH3OSO2CF3) yielded the iron triflate adduct [Cp*(dppe)FeOSO2CF3] (4, 85 %). In the solid state, the triflate is coordinated at the iron center as shown by XRD (dFe–O = 2.118(4) Å) and IR spectroscopy (νSO = 1305 cm–1). In soluti...
Gespeichert in:
| Veröffentlicht in: | European journal of inorganic chemistry 2020-01, Vol.2020 (1), p.84-93 |
|---|---|
| Hauptverfasser: | , , , , |
| Format: | Artikel |
| Sprache: | eng |
| Schlagworte: | |
| Online-Zugang: | Volltext |
| Tags: |
Tag hinzufügen
Keine Tags, Fügen Sie den ersten Tag hinzu!
|
| container_end_page | 93 |
|---|---|
| container_issue | 1 |
| container_start_page | 84 |
| container_title | European journal of inorganic chemistry |
| container_volume | 2020 |
| creator | Hamon, Paul Toupet, Loic Roisnel, Thierry Hamon, Jean‐René Lapinte, Claude |
| description | Treatment of the iron hydride [Cp*(dppe)FeH] (1) with methyl triflate (CH3OSO2CF3) yielded the iron triflate adduct [Cp*(dppe)FeOSO2CF3] (4, 85 %). In the solid state, the triflate is coordinated at the iron center as shown by XRD (dFe–O = 2.118(4) Å) and IR spectroscopy (νSO = 1305 cm–1). In solution, 4 is in equilibrium with the 16‐electron species [Cp*(dppe)Fe]OSO2CF3 (5(OSO2CF3)), 4/5(OSO2CF3) = 2:1). The CV of 4 displays two waves (E1 = –0.74 V, E2 = 0.24 V vs. SCE) assigned to the [Cp*(dppe)Fe(I)]/[Cp*(dppe)Fe(II)]+ and [Cp*(dppe)Fe(II)]+/[Cp*(dppe)Fe(III)]2+ redox couples. Reduction of 4 with Cp2Co provided the complex [Cp*(dppe)Fe(I)] (6, 95 %) and oxidation of 6 with [Cp2Fe]PF6 gave [Cp*(dppe)Fe]PF6 (5(PF6), 98 %). XRD established the pseudo‐trigonal bipyramidal geometry for the five‐coordinated cation 5+. The reactivity of 5(PF6) and 6 toward small molecules (CH2Cl2, H2O, CO, H2, N2) is reported.
The new complex [Cp*(dppe)FeOSO2CF3] was prepared by treatment of hydride [Cp*(dppe)FeH] with CH3OSO2CF3 (85 % yield). This compound dissociates in THF, opening the route to the five‐coordinated complexes [Cp*(dppe)Fe] and [Cp*(dppe)Fe]PF6, and to the six‐coordinated derivatives [Cp*(dppe)Fe‐L]PF6 (L = CO, H2, N2, H2O) |
| doi_str_mv | 10.1002/ejic.201901086 |
| format | Article |
| fullrecord | <record><control><sourceid>proquest_hal_p</sourceid><recordid>TN_cdi_hal_primary_oai_HAL_hal_02434627v1</recordid><sourceformat>XML</sourceformat><sourcesystem>PC</sourcesystem><sourcerecordid>2345499571</sourcerecordid><originalsourceid>FETCH-LOGICAL-c4576-f91bf16ae9cb616c10d57e2a9a381a4dbc82258df583c57d57499f9084919c503</originalsourceid><addsrcrecordid>eNqFUctO5DAQjNAiwQJXzpa4MIcMbedpbqOIgUEjDRJwQsjyOB2NRyEOdhgep_2E_Qv-iy_BIYg97snVXdXVVlcQHFIYUwB2gmutxgwoBwp5uhXsUuA8hDRnvzyOozikPM53gt_OrQEggijdDd6vLLbSyk6bhsimJMXKV6pDq9-GpqlIt0JyY3VVyw5JYR7aGl_IXdEel22LoykurhesmEb3p2Ti6WaDjcamIxOl0DnSGTKXS10jmeoNfvz5-7XnWr94WBhjS930vjNrmuPZ6IscsC--l6HbD7YrWTs8-H73gtvp2U1xEc4X57NiMg9VnGRpWHG6rGgqkatlSlNFoUwyZJLLKKcyLpcqZyzJyyrJI5Vknow5rzjkMadcJRDtBaPBdyVr0Vr9IO2rMFKLi8lc9D1g_pIpyzbUa48GbWvN4xO6TqzNk2389wSL4sQ7J1mvGg8qZY1zFqsfWwqiD070wYmf4PwAHwae_c1e_6MWZ5ez4t_sJ-99nMM</addsrcrecordid><sourcetype>Open Access Repository</sourcetype><iscdi>true</iscdi><recordtype>article</recordtype><pqid>2345499571</pqid></control><display><type>article</type><title>Preparation and Characterization of the Triflate Complex [Cp(dppe)FeOSO2CF3]: A Convenient Access to Labile Five‐ and Six‐Coordinate Iron(I) and Iron(II) Complexes</title><source>Access via Wiley Online Library</source><creator>Hamon, Paul ; Toupet, Loic ; Roisnel, Thierry ; Hamon, Jean‐René ; Lapinte, Claude</creator><creatorcontrib>Hamon, Paul ; Toupet, Loic ; Roisnel, Thierry ; Hamon, Jean‐René ; Lapinte, Claude</creatorcontrib><description>Treatment of the iron hydride [Cp*(dppe)FeH] (1) with methyl triflate (CH3OSO2CF3) yielded the iron triflate adduct [Cp*(dppe)FeOSO2CF3] (4, 85 %). In the solid state, the triflate is coordinated at the iron center as shown by XRD (dFe–O = 2.118(4) Å) and IR spectroscopy (νSO = 1305 cm–1). In solution, 4 is in equilibrium with the 16‐electron species [Cp*(dppe)Fe]OSO2CF3 (5(OSO2CF3)), 4/5(OSO2CF3) = 2:1). The CV of 4 displays two waves (E1 = –0.74 V, E2 = 0.24 V vs. SCE) assigned to the [Cp*(dppe)Fe(I)]/[Cp*(dppe)Fe(II)]+ and [Cp*(dppe)Fe(II)]+/[Cp*(dppe)Fe(III)]2+ redox couples. Reduction of 4 with Cp2Co provided the complex [Cp*(dppe)Fe(I)] (6, 95 %) and oxidation of 6 with [Cp2Fe]PF6 gave [Cp*(dppe)Fe]PF6 (5(PF6), 98 %). XRD established the pseudo‐trigonal bipyramidal geometry for the five‐coordinated cation 5+. The reactivity of 5(PF6) and 6 toward small molecules (CH2Cl2, H2O, CO, H2, N2) is reported.
The new complex [Cp*(dppe)FeOSO2CF3] was prepared by treatment of hydride [Cp*(dppe)FeH] with CH3OSO2CF3 (85 % yield). This compound dissociates in THF, opening the route to the five‐coordinated complexes [Cp*(dppe)Fe] and [Cp*(dppe)Fe]PF6, and to the six‐coordinated derivatives [Cp*(dppe)Fe‐L]PF6 (L = CO, H2, N2, H2O)</description><identifier>ISSN: 1434-1948</identifier><identifier>EISSN: 1099-0682</identifier><identifier>DOI: 10.1002/ejic.201901086</identifier><language>eng</language><publisher>Weinheim: Wiley Subscription Services, Inc</publisher><subject>Chemical Sciences ; Coordination chemistry ; Coordination compounds ; Coordination modes ; Dichloromethane ; Infrared spectroscopy ; Inorganic chemistry ; Iron ; N,O ligands ; Oxidation ; Structure elucidation ; Triflate adducts</subject><ispartof>European journal of inorganic chemistry, 2020-01, Vol.2020 (1), p.84-93</ispartof><rights>2020 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim</rights><rights>Distributed under a Creative Commons Attribution 4.0 International License</rights><lds50>peer_reviewed</lds50><oa>free_for_read</oa><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-c4576-f91bf16ae9cb616c10d57e2a9a381a4dbc82258df583c57d57499f9084919c503</citedby><cites>FETCH-LOGICAL-c4576-f91bf16ae9cb616c10d57e2a9a381a4dbc82258df583c57d57499f9084919c503</cites><orcidid>0000-0003-4630-4096 ; 0000-0003-2647-8240 ; 0000-0002-6088-4472</orcidid></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><linktopdf>$$Uhttps://onlinelibrary.wiley.com/doi/pdf/10.1002%2Fejic.201901086$$EPDF$$P50$$Gwiley$$H</linktopdf><linktohtml>$$Uhttps://onlinelibrary.wiley.com/doi/full/10.1002%2Fejic.201901086$$EHTML$$P50$$Gwiley$$H</linktohtml><link.rule.ids>230,314,780,784,885,1417,27924,27925,45574,45575</link.rule.ids><backlink>$$Uhttps://univ-rennes.hal.science/hal-02434627$$DView record in HAL$$Hfree_for_read</backlink></links><search><creatorcontrib>Hamon, Paul</creatorcontrib><creatorcontrib>Toupet, Loic</creatorcontrib><creatorcontrib>Roisnel, Thierry</creatorcontrib><creatorcontrib>Hamon, Jean‐René</creatorcontrib><creatorcontrib>Lapinte, Claude</creatorcontrib><title>Preparation and Characterization of the Triflate Complex [Cp(dppe)FeOSO2CF3]: A Convenient Access to Labile Five‐ and Six‐Coordinate Iron(I) and Iron(II) Complexes</title><title>European journal of inorganic chemistry</title><description>Treatment of the iron hydride [Cp*(dppe)FeH] (1) with methyl triflate (CH3OSO2CF3) yielded the iron triflate adduct [Cp*(dppe)FeOSO2CF3] (4, 85 %). In the solid state, the triflate is coordinated at the iron center as shown by XRD (dFe–O = 2.118(4) Å) and IR spectroscopy (νSO = 1305 cm–1). In solution, 4 is in equilibrium with the 16‐electron species [Cp*(dppe)Fe]OSO2CF3 (5(OSO2CF3)), 4/5(OSO2CF3) = 2:1). The CV of 4 displays two waves (E1 = –0.74 V, E2 = 0.24 V vs. SCE) assigned to the [Cp*(dppe)Fe(I)]/[Cp*(dppe)Fe(II)]+ and [Cp*(dppe)Fe(II)]+/[Cp*(dppe)Fe(III)]2+ redox couples. Reduction of 4 with Cp2Co provided the complex [Cp*(dppe)Fe(I)] (6, 95 %) and oxidation of 6 with [Cp2Fe]PF6 gave [Cp*(dppe)Fe]PF6 (5(PF6), 98 %). XRD established the pseudo‐trigonal bipyramidal geometry for the five‐coordinated cation 5+. The reactivity of 5(PF6) and 6 toward small molecules (CH2Cl2, H2O, CO, H2, N2) is reported.
The new complex [Cp*(dppe)FeOSO2CF3] was prepared by treatment of hydride [Cp*(dppe)FeH] with CH3OSO2CF3 (85 % yield). This compound dissociates in THF, opening the route to the five‐coordinated complexes [Cp*(dppe)Fe] and [Cp*(dppe)Fe]PF6, and to the six‐coordinated derivatives [Cp*(dppe)Fe‐L]PF6 (L = CO, H2, N2, H2O)</description><subject>Chemical Sciences</subject><subject>Coordination chemistry</subject><subject>Coordination compounds</subject><subject>Coordination modes</subject><subject>Dichloromethane</subject><subject>Infrared spectroscopy</subject><subject>Inorganic chemistry</subject><subject>Iron</subject><subject>N,O ligands</subject><subject>Oxidation</subject><subject>Structure elucidation</subject><subject>Triflate adducts</subject><issn>1434-1948</issn><issn>1099-0682</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2020</creationdate><recordtype>article</recordtype><recordid>eNqFUctO5DAQjNAiwQJXzpa4MIcMbedpbqOIgUEjDRJwQsjyOB2NRyEOdhgep_2E_Qv-iy_BIYg97snVXdXVVlcQHFIYUwB2gmutxgwoBwp5uhXsUuA8hDRnvzyOozikPM53gt_OrQEggijdDd6vLLbSyk6bhsimJMXKV6pDq9-GpqlIt0JyY3VVyw5JYR7aGl_IXdEel22LoykurhesmEb3p2Ti6WaDjcamIxOl0DnSGTKXS10jmeoNfvz5-7XnWr94WBhjS930vjNrmuPZ6IscsC--l6HbD7YrWTs8-H73gtvp2U1xEc4X57NiMg9VnGRpWHG6rGgqkatlSlNFoUwyZJLLKKcyLpcqZyzJyyrJI5Vknow5rzjkMadcJRDtBaPBdyVr0Vr9IO2rMFKLi8lc9D1g_pIpyzbUa48GbWvN4xO6TqzNk2389wSL4sQ7J1mvGg8qZY1zFqsfWwqiD070wYmf4PwAHwae_c1e_6MWZ5ez4t_sJ-99nMM</recordid><startdate>20200109</startdate><enddate>20200109</enddate><creator>Hamon, Paul</creator><creator>Toupet, Loic</creator><creator>Roisnel, Thierry</creator><creator>Hamon, Jean‐René</creator><creator>Lapinte, Claude</creator><general>Wiley Subscription Services, Inc</general><general>Wiley-VCH Verlag</general><scope>AAYXX</scope><scope>CITATION</scope><scope>7SR</scope><scope>7U5</scope><scope>8BQ</scope><scope>8FD</scope><scope>JG9</scope><scope>L7M</scope><scope>1XC</scope><scope>VOOES</scope><orcidid>https://orcid.org/0000-0003-4630-4096</orcidid><orcidid>https://orcid.org/0000-0003-2647-8240</orcidid><orcidid>https://orcid.org/0000-0002-6088-4472</orcidid></search><sort><creationdate>20200109</creationdate><title>Preparation and Characterization of the Triflate Complex [Cp(dppe)FeOSO2CF3]: A Convenient Access to Labile Five‐ and Six‐Coordinate Iron(I) and Iron(II) Complexes</title><author>Hamon, Paul ; Toupet, Loic ; Roisnel, Thierry ; Hamon, Jean‐René ; Lapinte, Claude</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-c4576-f91bf16ae9cb616c10d57e2a9a381a4dbc82258df583c57d57499f9084919c503</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>2020</creationdate><topic>Chemical Sciences</topic><topic>Coordination chemistry</topic><topic>Coordination compounds</topic><topic>Coordination modes</topic><topic>Dichloromethane</topic><topic>Infrared spectroscopy</topic><topic>Inorganic chemistry</topic><topic>Iron</topic><topic>N,O ligands</topic><topic>Oxidation</topic><topic>Structure elucidation</topic><topic>Triflate adducts</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Hamon, Paul</creatorcontrib><creatorcontrib>Toupet, Loic</creatorcontrib><creatorcontrib>Roisnel, Thierry</creatorcontrib><creatorcontrib>Hamon, Jean‐René</creatorcontrib><creatorcontrib>Lapinte, Claude</creatorcontrib><collection>CrossRef</collection><collection>Engineered Materials Abstracts</collection><collection>Solid State and Superconductivity Abstracts</collection><collection>METADEX</collection><collection>Technology Research Database</collection><collection>Materials Research Database</collection><collection>Advanced Technologies Database with Aerospace</collection><collection>Hyper Article en Ligne (HAL)</collection><collection>Hyper Article en Ligne (HAL) (Open Access)</collection><jtitle>European journal of inorganic chemistry</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Hamon, Paul</au><au>Toupet, Loic</au><au>Roisnel, Thierry</au><au>Hamon, Jean‐René</au><au>Lapinte, Claude</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Preparation and Characterization of the Triflate Complex [Cp(dppe)FeOSO2CF3]: A Convenient Access to Labile Five‐ and Six‐Coordinate Iron(I) and Iron(II) Complexes</atitle><jtitle>European journal of inorganic chemistry</jtitle><date>2020-01-09</date><risdate>2020</risdate><volume>2020</volume><issue>1</issue><spage>84</spage><epage>93</epage><pages>84-93</pages><issn>1434-1948</issn><eissn>1099-0682</eissn><abstract>Treatment of the iron hydride [Cp*(dppe)FeH] (1) with methyl triflate (CH3OSO2CF3) yielded the iron triflate adduct [Cp*(dppe)FeOSO2CF3] (4, 85 %). In the solid state, the triflate is coordinated at the iron center as shown by XRD (dFe–O = 2.118(4) Å) and IR spectroscopy (νSO = 1305 cm–1). In solution, 4 is in equilibrium with the 16‐electron species [Cp*(dppe)Fe]OSO2CF3 (5(OSO2CF3)), 4/5(OSO2CF3) = 2:1). The CV of 4 displays two waves (E1 = –0.74 V, E2 = 0.24 V vs. SCE) assigned to the [Cp*(dppe)Fe(I)]/[Cp*(dppe)Fe(II)]+ and [Cp*(dppe)Fe(II)]+/[Cp*(dppe)Fe(III)]2+ redox couples. Reduction of 4 with Cp2Co provided the complex [Cp*(dppe)Fe(I)] (6, 95 %) and oxidation of 6 with [Cp2Fe]PF6 gave [Cp*(dppe)Fe]PF6 (5(PF6), 98 %). XRD established the pseudo‐trigonal bipyramidal geometry for the five‐coordinated cation 5+. The reactivity of 5(PF6) and 6 toward small molecules (CH2Cl2, H2O, CO, H2, N2) is reported.
The new complex [Cp*(dppe)FeOSO2CF3] was prepared by treatment of hydride [Cp*(dppe)FeH] with CH3OSO2CF3 (85 % yield). This compound dissociates in THF, opening the route to the five‐coordinated complexes [Cp*(dppe)Fe] and [Cp*(dppe)Fe]PF6, and to the six‐coordinated derivatives [Cp*(dppe)Fe‐L]PF6 (L = CO, H2, N2, H2O)</abstract><cop>Weinheim</cop><pub>Wiley Subscription Services, Inc</pub><doi>10.1002/ejic.201901086</doi><tpages>10</tpages><orcidid>https://orcid.org/0000-0003-4630-4096</orcidid><orcidid>https://orcid.org/0000-0003-2647-8240</orcidid><orcidid>https://orcid.org/0000-0002-6088-4472</orcidid><oa>free_for_read</oa></addata></record> |
| fulltext | fulltext |
| identifier | ISSN: 1434-1948 |
| ispartof | European journal of inorganic chemistry, 2020-01, Vol.2020 (1), p.84-93 |
| issn | 1434-1948 1099-0682 |
| language | eng |
| recordid | cdi_hal_primary_oai_HAL_hal_02434627v1 |
| source | Access via Wiley Online Library |
| subjects | Chemical Sciences Coordination chemistry Coordination compounds Coordination modes Dichloromethane Infrared spectroscopy Inorganic chemistry Iron N,O ligands Oxidation Structure elucidation Triflate adducts |
| title | Preparation and Characterization of the Triflate Complex [Cp(dppe)FeOSO2CF3]: A Convenient Access to Labile Five‐ and Six‐Coordinate Iron(I) and Iron(II) Complexes |
| url | https://sfx.bib-bvb.de/sfx_tum?ctx_ver=Z39.88-2004&ctx_enc=info:ofi/enc:UTF-8&ctx_tim=2025-01-02T01%3A28%3A26IST&url_ver=Z39.88-2004&url_ctx_fmt=infofi/fmt:kev:mtx:ctx&rfr_id=info:sid/primo.exlibrisgroup.com:primo3-Article-proquest_hal_p&rft_val_fmt=info:ofi/fmt:kev:mtx:journal&rft.genre=article&rft.atitle=Preparation%20and%20Characterization%20of%20the%20Triflate%20Complex%20%5BCp(dppe)FeOSO2CF3%5D:%20A%20Convenient%20Access%20to%20Labile%20Five%E2%80%90%20and%20Six%E2%80%90Coordinate%20Iron(I)%20and%20Iron(II)%20Complexes&rft.jtitle=European%20journal%20of%20inorganic%20chemistry&rft.au=Hamon,%20Paul&rft.date=2020-01-09&rft.volume=2020&rft.issue=1&rft.spage=84&rft.epage=93&rft.pages=84-93&rft.issn=1434-1948&rft.eissn=1099-0682&rft_id=info:doi/10.1002/ejic.201901086&rft_dat=%3Cproquest_hal_p%3E2345499571%3C/proquest_hal_p%3E%3Curl%3E%3C/url%3E&disable_directlink=true&sfx.directlink=off&sfx.report_link=0&rft_id=info:oai/&rft_pqid=2345499571&rft_id=info:pmid/&rfr_iscdi=true |