Coordination chemistry of a calix[4]arene-based NHC ligand: dinuclear complexes and comparison to I super(i)Pr sub(2)Me sub(2)
The preparation and coordination chemistry of 5,17-bis(3-methyl-1-imidazol-2-ylidene)-25,26,27,28-tetrapropoxyca l ix[4]arene (1) is described. Starting from the bis(imidazolium) pro-ligand 1.2HI, the free carbene 1 was readily generated in solution through deprotonation using K[O super()tu] and its...
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| Veröffentlicht in: | Dalton transactions : an international journal of inorganic chemistry 2016-05, Vol.45 (21), p.8945-8955 |
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| container_title | Dalton transactions : an international journal of inorganic chemistry |
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| creator | Patchett, Ruth Chaplin, Adrian B |
| description | The preparation and coordination chemistry of 5,17-bis(3-methyl-1-imidazol-2-ylidene)-25,26,27,28-tetrapropoxyca l ix[4]arene (1) is described. Starting from the bis(imidazolium) pro-ligand 1.2HI, the free carbene 1 was readily generated in solution through deprotonation using K[O super()tu] and its reactivity with rhodium(i) dimers [Rh(COD)Cl] sub(2) (COD = 1,5-cyclooctadiene) and [Rh(CO) sub(2)Cl] sub(2) investigated. Dinuclear complexes were isolated in both cases, where the calix[4]arene-based NHC ligand adopts a bridging mu super(2)-coordination mode, and in one case characterised in the solid-state by X-ray diffraction. Using instead an isolated and well-defined (mononuclear) silver transfer agent, generated by reaction of 1.2HI with Ag sub(2)O in the presence of a halide extractor, reactions with [Rh(COD)Cl] sub(2) and [Rh(CO) sub(2)Cl] sub(2) produced cationic dinuclear complexes bearing mu super(2)-1 and mu super(2)-Cl bridging ligands. The structural formulation of the novel dinuclear adducts of 1 was aided through spectroscopic congruence with model complexes, containing monodentate 1,3-diisopropyl-4,5-dimethylimidazol-2-ylidene (I super(i)Pr sub(2)Me sub(2)). |
| doi_str_mv | 10.1039/c6dt01001f |
| format | Article |
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Starting from the bis(imidazolium) pro-ligand 1.2HI, the free carbene 1 was readily generated in solution through deprotonation using K[O super()tu] and its reactivity with rhodium(i) dimers [Rh(COD)Cl] sub(2) (COD = 1,5-cyclooctadiene) and [Rh(CO) sub(2)Cl] sub(2) investigated. Dinuclear complexes were isolated in both cases, where the calix[4]arene-based NHC ligand adopts a bridging mu super(2)-coordination mode, and in one case characterised in the solid-state by X-ray diffraction. Using instead an isolated and well-defined (mononuclear) silver transfer agent, generated by reaction of 1.2HI with Ag sub(2)O in the presence of a halide extractor, reactions with [Rh(COD)Cl] sub(2) and [Rh(CO) sub(2)Cl] sub(2) produced cationic dinuclear complexes bearing mu super(2)-1 and mu super(2)-Cl bridging ligands. The structural formulation of the novel dinuclear adducts of 1 was aided through spectroscopic congruence with model complexes, containing monodentate 1,3-diisopropyl-4,5-dimethylimidazol-2-ylidene (I super(i)Pr sub(2)Me sub(2)).</description><identifier>ISSN: 1477-9226</identifier><identifier>EISSN: 1477-9234</identifier><identifier>DOI: 10.1039/c6dt01001f</identifier><language>eng</language><subject>Bridging ; Carbenes ; Cationic ; Diffraction ; Dimers ; Ligands ; Mathematical models ; X-rays</subject><ispartof>Dalton transactions : an international journal of inorganic chemistry, 2016-05, Vol.45 (21), p.8945-8955</ispartof><lds50>peer_reviewed</lds50><woscitedreferencessubscribed>false</woscitedreferencessubscribed></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><link.rule.ids>314,777,781,27905,27906</link.rule.ids></links><search><creatorcontrib>Patchett, Ruth</creatorcontrib><creatorcontrib>Chaplin, Adrian B</creatorcontrib><title>Coordination chemistry of a calix[4]arene-based NHC ligand: dinuclear complexes and comparison to I super(i)Pr sub(2)Me sub(2)</title><title>Dalton transactions : an international journal of inorganic chemistry</title><description>The preparation and coordination chemistry of 5,17-bis(3-methyl-1-imidazol-2-ylidene)-25,26,27,28-tetrapropoxyca l ix[4]arene (1) is described. Starting from the bis(imidazolium) pro-ligand 1.2HI, the free carbene 1 was readily generated in solution through deprotonation using K[O super()tu] and its reactivity with rhodium(i) dimers [Rh(COD)Cl] sub(2) (COD = 1,5-cyclooctadiene) and [Rh(CO) sub(2)Cl] sub(2) investigated. Dinuclear complexes were isolated in both cases, where the calix[4]arene-based NHC ligand adopts a bridging mu super(2)-coordination mode, and in one case characterised in the solid-state by X-ray diffraction. Using instead an isolated and well-defined (mononuclear) silver transfer agent, generated by reaction of 1.2HI with Ag sub(2)O in the presence of a halide extractor, reactions with [Rh(COD)Cl] sub(2) and [Rh(CO) sub(2)Cl] sub(2) produced cationic dinuclear complexes bearing mu super(2)-1 and mu super(2)-Cl bridging ligands. 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Starting from the bis(imidazolium) pro-ligand 1.2HI, the free carbene 1 was readily generated in solution through deprotonation using K[O super()tu] and its reactivity with rhodium(i) dimers [Rh(COD)Cl] sub(2) (COD = 1,5-cyclooctadiene) and [Rh(CO) sub(2)Cl] sub(2) investigated. Dinuclear complexes were isolated in both cases, where the calix[4]arene-based NHC ligand adopts a bridging mu super(2)-coordination mode, and in one case characterised in the solid-state by X-ray diffraction. Using instead an isolated and well-defined (mononuclear) silver transfer agent, generated by reaction of 1.2HI with Ag sub(2)O in the presence of a halide extractor, reactions with [Rh(COD)Cl] sub(2) and [Rh(CO) sub(2)Cl] sub(2) produced cationic dinuclear complexes bearing mu super(2)-1 and mu super(2)-Cl bridging ligands. The structural formulation of the novel dinuclear adducts of 1 was aided through spectroscopic congruence with model complexes, containing monodentate 1,3-diisopropyl-4,5-dimethylimidazol-2-ylidene (I super(i)Pr sub(2)Me sub(2)).</abstract><doi>10.1039/c6dt01001f</doi></addata></record> |
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| source | Royal Society Of Chemistry Journals 2008-; Alma/SFX Local Collection |
| subjects | Bridging Carbenes Cationic Diffraction Dimers Ligands Mathematical models X-rays |
| title | Coordination chemistry of a calix[4]arene-based NHC ligand: dinuclear complexes and comparison to I super(i)Pr sub(2)Me sub(2) |
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