Reactions of monocyclopentadienylniobium(III) complexes with α-diketones. Crystal-structure of the phosphonium salt [P{C(OH)MeC(O)Me}Me2Ph]Cl
The reactions of Nb(η5-C5H5)Cl2(CO)L2 (= PMe3, PMe2Ph) with α-diketones RCOCOR (R = Me, Ph) and 3,5-di-t-butyl-o-quinone have been studied. When L = PMe2Ph and R = Ph the reaction in a molar ratio 1/1 gives Nb(η5-C5H5)Cl2(O2C2Ph2)(PMe2Ph)2 (I) whereas the same reaction for R = Me gives the phosphoni...
| Autores: | , , , , , |
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| Tipo de recurso: | artículo |
| Fecha de publicación: | 1987 |
| País: | España |
| Institución: | Universidad de Alcalá (UAH) |
| Repositorio: | e_Buah Biblioteca Digital Universidad de Alcalá |
| Idioma: | inglés |
| OAI Identifier: | oai:ebuah.uah.es:10017/4660 |
| Acceso en línea: | http://hdl.handle.net/10017/4660 https://dx.doi.org/10.1016/0022-328X(87)85096-9 |
| Access Level: | acceso abierto |
| Palabra clave: | Niobium Crystal structure Ciencia Química inorgánica Science Chemistry, inorganic |
| Sumario: | The reactions of Nb(η5-C5H5)Cl2(CO)L2 (= PMe3, PMe2Ph) with α-diketones RCOCOR (R = Me, Ph) and 3,5-di-t-butyl-o-quinone have been studied. When L = PMe2Ph and R = Ph the reaction in a molar ratio 1/1 gives Nb(η5-C5H5)Cl2(O2C2Ph2)(PMe2Ph)2 (I) whereas the same reaction for R = Me gives the phosphonium salt [P{C(OH)MeC(O)Me}Me2Ph]Cl (VII). When L = PMe3 only the phosphonium salts [P{C(OH)RC(O)R}Me3]Cl are obtained for R = Me (V) and Ph (VI), but the complex Nb(η5-C5H5)Cl2(O2C2Ph2)PMe3 (II) can be isolated by previous addition of MeI. Similar reactions with 3,5-di-t-butyl-o-quinone give Nb(η5-C5H5)Cl2(o-O2C6H2But)L, L = PMe3 (III), PMe2Ph (IV). All the compounds have been characterized by IR, 1H, 13C, 31P NMR spectroscopy and the crystal structure of VII has been determined by X-ray diffraction. VII crystallizes in the monoclinic space group P21/c with a 7.440(2), b 10.377(3), c 17.644(4) Å, β 96.94(2)° and Dcal 1.039 g cm−3 for Z = 4. A final R value of 0.046 (Rw = 0.049) based on 2309 observed reflections was obtained. The geometry around the P atom is tetrahedral. |
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