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Reaction of p-Toluenesulfonylamide and M(NMe2)4 (M = Ti, V): Generation of Electron-Deficient Imido Complexes of Early Transition Metals
p-Toluenesulfonamide (p-TsNH2) was succesfully employed as an imido ligand precursor in the synthesis of highly air- and moisture-sensitive titanium(IV) and vanadium(IV) complexes. Reaction of M(NMe2)4 (M = Ti, V) with TsNH2 in toluene afforded [M(μ-NTs)(NMe2)2]2 dimer complexes (M = Ti (1), V (2))....
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Published in: | Inorganic chemistry 2007-04, Vol.46 (8), p.3192-3202 |
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description | p-Toluenesulfonamide (p-TsNH2) was succesfully employed as an imido ligand precursor in the synthesis of highly air- and moisture-sensitive titanium(IV) and vanadium(IV) complexes. Reaction of M(NMe2)4 (M = Ti, V) with TsNH2 in toluene afforded [M(μ-NTs)(NMe2)2]2 dimer complexes (M = Ti (1), V (2)). By contrast, the reaction carried out in dichloromethane led to [Ti{μ-N,O-NTs}Cl(NMe2)(NHMe2)2]2 (3) and [Ti{μ-N,O-NTs}Cl2(NHMe2)2] n (4) through solvent activation. The same reaction of M(NMe2)4/TsNH2 conducted in the presence of an excess of trimethylchlorosilane produced [V(NTs)Cl2(NHMe2)2] (5) and [(Me2HN)Cl2Ti(μ2-N-NTs-κ2 N,O)2TiCl2(NHMe2)2] (6). Alternatively, compound 6 has also been prepared from TiCl2(NMe2)2 and TsNH2. 1 was reacted with trimethylchlorosilane to afford the amide complex [Ti{μ-N,O‘-N(SiMe3)Ts-κ3 N,O,O‘}Cl2(NMe2)]2 (7) in which the tosylimide bond has been silylated. Compounds 1 − 6 represents the first examples of sulfonylimido complexes for titanium and vanadium. |
doi_str_mv | 10.1021/ic062404j |
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Reaction of M(NMe2)4 (M = Ti, V) with TsNH2 in toluene afforded [M(μ-NTs)(NMe2)2]2 dimer complexes (M = Ti (1), V (2)). By contrast, the reaction carried out in dichloromethane led to [Ti{μ-N,O-NTs}Cl(NMe2)(NHMe2)2]2 (3) and [Ti{μ-N,O-NTs}Cl2(NHMe2)2] n (4) through solvent activation. The same reaction of M(NMe2)4/TsNH2 conducted in the presence of an excess of trimethylchlorosilane produced [V(NTs)Cl2(NHMe2)2] (5) and [(Me2HN)Cl2Ti(μ2-N-NTs-κ2 N,O)2TiCl2(NHMe2)2] (6). Alternatively, compound 6 has also been prepared from TiCl2(NMe2)2 and TsNH2. 1 was reacted with trimethylchlorosilane to afford the amide complex [Ti{μ-N,O‘-N(SiMe3)Ts-κ3 N,O,O‘}Cl2(NMe2)]2 (7) in which the tosylimide bond has been silylated. Compounds 1 − 6 represents the first examples of sulfonylimido complexes for titanium and vanadium.</description><identifier>ISSN: 0020-1669</identifier><identifier>EISSN: 1520-510X</identifier><identifier>DOI: 10.1021/ic062404j</identifier><identifier>PMID: 17362000</identifier><language>eng</language><publisher>United States: American Chemical Society</publisher><subject>Crystallography, X-Ray ; Electrons ; Imides - chemistry ; Models, Molecular ; Molecular Conformation ; Organometallic Compounds - chemical synthesis ; Organometallic Compounds - chemistry ; Stereoisomerism ; Sulfonamides - chemistry ; Toluene - analogs & derivatives ; Toluene - chemistry ; Transition Elements - chemistry</subject><ispartof>Inorganic chemistry, 2007-04, Vol.46 (8), p.3192-3202</ispartof><rights>Copyright © 2007 American Chemical Society</rights><lds50>peer_reviewed</lds50><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-a266t-ab226eea8487a573e8222a99cf38ef5e83ee5804a0ece470c2a7edaf5fa5859a3</citedby><cites>FETCH-LOGICAL-a266t-ab226eea8487a573e8222a99cf38ef5e83ee5804a0ece470c2a7edaf5fa5859a3</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/17362000$$D View this record in MEDLINE/PubMed$$Hfree_for_read</backlink></links><search><creatorcontrib>Lorber, Christian</creatorcontrib><creatorcontrib>Choukroun, Robert</creatorcontrib><creatorcontrib>Vendier, Laure</creatorcontrib><title>Reaction of p-Toluenesulfonylamide and M(NMe2)4 (M = Ti, V): Generation of Electron-Deficient Imido Complexes of Early Transition Metals</title><title>Inorganic chemistry</title><addtitle>Inorg. Chem</addtitle><description>p-Toluenesulfonamide (p-TsNH2) was succesfully employed as an imido ligand precursor in the synthesis of highly air- and moisture-sensitive titanium(IV) and vanadium(IV) complexes. Reaction of M(NMe2)4 (M = Ti, V) with TsNH2 in toluene afforded [M(μ-NTs)(NMe2)2]2 dimer complexes (M = Ti (1), V (2)). By contrast, the reaction carried out in dichloromethane led to [Ti{μ-N,O-NTs}Cl(NMe2)(NHMe2)2]2 (3) and [Ti{μ-N,O-NTs}Cl2(NHMe2)2] n (4) through solvent activation. The same reaction of M(NMe2)4/TsNH2 conducted in the presence of an excess of trimethylchlorosilane produced [V(NTs)Cl2(NHMe2)2] (5) and [(Me2HN)Cl2Ti(μ2-N-NTs-κ2 N,O)2TiCl2(NHMe2)2] (6). Alternatively, compound 6 has also been prepared from TiCl2(NMe2)2 and TsNH2. 1 was reacted with trimethylchlorosilane to afford the amide complex [Ti{μ-N,O‘-N(SiMe3)Ts-κ3 N,O,O‘}Cl2(NMe2)]2 (7) in which the tosylimide bond has been silylated. Compounds 1 − 6 represents the first examples of sulfonylimido complexes for titanium and vanadium.</description><subject>Crystallography, X-Ray</subject><subject>Electrons</subject><subject>Imides - chemistry</subject><subject>Models, Molecular</subject><subject>Molecular Conformation</subject><subject>Organometallic Compounds - chemical synthesis</subject><subject>Organometallic Compounds - chemistry</subject><subject>Stereoisomerism</subject><subject>Sulfonamides - chemistry</subject><subject>Toluene - analogs & derivatives</subject><subject>Toluene - chemistry</subject><subject>Transition Elements - chemistry</subject><issn>0020-1669</issn><issn>1520-510X</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2007</creationdate><recordtype>article</recordtype><recordid>eNpt0MFu1DAQBmALgei2cOAFkC-grkTAdmInQeJQLWVbqSkIAurNmnonkhcnXuxE6t64It6SJ8F0l3LhNLb8-R_pJ-QJZy85E_yVNUyJghXre2TGpWCZ5OzqPpkxls5cqfqAHMa4ZozVeaEekgNe5kqk64z8_IhgRusH6ju6yVrvJhwwTq7zw9ZBb1dIYVjR5viyQTEv6HFD39DWvqBf5q9_ff9Bl4kH-Jtw6tCMwQ_ZW-yssTiM9DxleLrw_cbhDcZbBcFtaRtgiPb2Z4MjuPiIPOjSwMf7eUQ-vzttF2fZxfvl-eLkIgOh1JjBtRAKEaqiKkGWOVZCCKhr0-UVdhKrHFFWrACGBouSGQElrqCTHchK1pAfkee73E3w3yaMo-5tNOgcDOinqEuWSykrnuB8B03wMQbs9CbYHsJWc6b_NK_vmk_26T50uu5x9U_uq04g2wEbR7y5e4fwVasyL6VuP3zSV5fNslicVbpO_tnOg4l67acwpE7-s_g32CWZ7Q</recordid><startdate>20070416</startdate><enddate>20070416</enddate><creator>Lorber, Christian</creator><creator>Choukroun, Robert</creator><creator>Vendier, Laure</creator><general>American Chemical Society</general><scope>BSCLL</scope><scope>CGR</scope><scope>CUY</scope><scope>CVF</scope><scope>ECM</scope><scope>EIF</scope><scope>NPM</scope><scope>AAYXX</scope><scope>CITATION</scope><scope>7X8</scope></search><sort><creationdate>20070416</creationdate><title>Reaction of p-Toluenesulfonylamide and M(NMe2)4 (M = Ti, V): Generation of Electron-Deficient Imido Complexes of Early Transition Metals</title><author>Lorber, Christian ; Choukroun, Robert ; Vendier, Laure</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-a266t-ab226eea8487a573e8222a99cf38ef5e83ee5804a0ece470c2a7edaf5fa5859a3</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>2007</creationdate><topic>Crystallography, X-Ray</topic><topic>Electrons</topic><topic>Imides - chemistry</topic><topic>Models, Molecular</topic><topic>Molecular Conformation</topic><topic>Organometallic Compounds - chemical synthesis</topic><topic>Organometallic Compounds - chemistry</topic><topic>Stereoisomerism</topic><topic>Sulfonamides - chemistry</topic><topic>Toluene - analogs & derivatives</topic><topic>Toluene - chemistry</topic><topic>Transition Elements - chemistry</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Lorber, Christian</creatorcontrib><creatorcontrib>Choukroun, Robert</creatorcontrib><creatorcontrib>Vendier, Laure</creatorcontrib><collection>Istex</collection><collection>Medline</collection><collection>MEDLINE</collection><collection>MEDLINE (Ovid)</collection><collection>MEDLINE</collection><collection>MEDLINE</collection><collection>PubMed</collection><collection>CrossRef</collection><collection>MEDLINE - Academic</collection><jtitle>Inorganic chemistry</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Lorber, Christian</au><au>Choukroun, Robert</au><au>Vendier, Laure</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Reaction of p-Toluenesulfonylamide and M(NMe2)4 (M = Ti, V): Generation of Electron-Deficient Imido Complexes of Early Transition Metals</atitle><jtitle>Inorganic chemistry</jtitle><addtitle>Inorg. Chem</addtitle><date>2007-04-16</date><risdate>2007</risdate><volume>46</volume><issue>8</issue><spage>3192</spage><epage>3202</epage><pages>3192-3202</pages><issn>0020-1669</issn><eissn>1520-510X</eissn><abstract>p-Toluenesulfonamide (p-TsNH2) was succesfully employed as an imido ligand precursor in the synthesis of highly air- and moisture-sensitive titanium(IV) and vanadium(IV) complexes. Reaction of M(NMe2)4 (M = Ti, V) with TsNH2 in toluene afforded [M(μ-NTs)(NMe2)2]2 dimer complexes (M = Ti (1), V (2)). By contrast, the reaction carried out in dichloromethane led to [Ti{μ-N,O-NTs}Cl(NMe2)(NHMe2)2]2 (3) and [Ti{μ-N,O-NTs}Cl2(NHMe2)2] n (4) through solvent activation. The same reaction of M(NMe2)4/TsNH2 conducted in the presence of an excess of trimethylchlorosilane produced [V(NTs)Cl2(NHMe2)2] (5) and [(Me2HN)Cl2Ti(μ2-N-NTs-κ2 N,O)2TiCl2(NHMe2)2] (6). Alternatively, compound 6 has also been prepared from TiCl2(NMe2)2 and TsNH2. 1 was reacted with trimethylchlorosilane to afford the amide complex [Ti{μ-N,O‘-N(SiMe3)Ts-κ3 N,O,O‘}Cl2(NMe2)]2 (7) in which the tosylimide bond has been silylated. Compounds 1 − 6 represents the first examples of sulfonylimido complexes for titanium and vanadium.</abstract><cop>United States</cop><pub>American Chemical Society</pub><pmid>17362000</pmid><doi>10.1021/ic062404j</doi><tpages>11</tpages></addata></record> |
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subjects | Crystallography, X-Ray Electrons Imides - chemistry Models, Molecular Molecular Conformation Organometallic Compounds - chemical synthesis Organometallic Compounds - chemistry Stereoisomerism Sulfonamides - chemistry Toluene - analogs & derivatives Toluene - chemistry Transition Elements - chemistry |
title | Reaction of p-Toluenesulfonylamide and M(NMe2)4 (M = Ti, V): Generation of Electron-Deficient Imido Complexes of Early Transition Metals |
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