Synthesis and Characterization of Cyclopentadienyl Sulfur Niobium Complexes
A trimetallic sulfide cluster [Nb3(η5-C5Me5)3Cl3(μ3-Cl)(μ-S)3(μ3-S)] (2) has been synthesized from the reaction of [Nb(η5-C5Me5)Cl4] (1) with (Me3Si)2S in a 4:3 ratio by the release of SiClMe3. The trinuclear nature of complex 2 has been established by single crystal X-ray diffraction analysis. Ther...
| Autores: | , , , , |
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| Formato: | artículo |
| Fecha de publicación: | 2019 |
| País: | España |
| Recursos: | Universidad de Alcalá (UAH) |
| Repositorio: | e_Buah Biblioteca Digital Universidad de Alcalá |
| Idioma: | inglés |
| OAI Identifier: | oai:ebuah.uah.es:10017/38634 |
| Acesso em linha: | http://hdl.handle.net/10017/38634 https://dx.doi.org/10.1016/j.jorganchem.2019.06.022 |
| Access Level: | acceso abierto |
| Palavra-chave: | Sulfur complexes cyclopentadienyl ligand niobium metathesis reactions Química Chemistry |
| Resumo: | A trimetallic sulfide cluster [Nb3(η5-C5Me5)3Cl3(μ3-Cl)(μ-S)3(μ3-S)] (2) has been synthesized from the reaction of [Nb(η5-C5Me5)Cl4] (1) with (Me3Si)2S in a 4:3 ratio by the release of SiClMe3. The trinuclear nature of complex 2 has been established by single crystal X-ray diffraction analysis. Thermal treatment of 2 with SiH3Ph generated the dinuclear niobium(IV) complex [Nb2(η5-C5Me5)2Cl2(μ-S)2] (3) in a quantitative way. Likewise, one-pot syntheses of 3 has been developed from reaction of 1, (Me3Si)2S, and SiH3Ph in toluene. A series of dinuclear sulfide niobium(IV) derivatives [Nb2(η5-C5Me5)2R2(μ-S)2] (R = Me 4, Et 5, CH2SiMe3 6, C3H5 7, CH2Ph 8, nBu 9) can easily be obtained from the reaction of 3 with 2 equiv of the corresponding alkylating reagents. Single crystal X-ray diffraction analyses of 6 and 7 showed in all cases a trans disposition of the substituents. |
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