Synthesis, structure and characterisation of Ln5O(OPri)13 with Ln = Nd, Gd or Er
| Autor: | Gunnar Westin, Maria Wijk, Marat Moustiakimov, Mikael Kritikos |
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| Rok vydání: | 2001 |
| Předmět: | |
| Zdroj: | Journal of the Chemical Society, Dalton Transactions. :1931-1938 |
| ISSN: | 1364-5447 1472-7773 |
| DOI: | 10.1039/b102798k |
| Popis: | The molecular and basically isostructural oxo-alkoxides Ln5O(OPri)13 (Pri = 2-propyl) with Ln = Nd (1) and Gd (2) were synthesized by metathesis of LnCl3 and KOPri, in combination with stoichiometric hydrolysis, in 2-propanol-containing solvents. Er5O(OPri)133 was obtained as co-product to an erbium aluminium 2-propoxide with an Er ∶ Al ratio of ca. 3 ∶ 1, from the reaction of 15KOPri + H2O + Al(OPri)3 with 5ErCl3, in toluene–2-propanol. The solid state structures of 1–3 were obtained by single-crystal X-ray diffraction. The characterisations were made with differential scanning calorimetric measurements, UV-Vis and FT-IR spectroscopy. The molecule contains an M5O fragment with the configuration of a square pyramid and the oxo-oxygen atom slightly above the basal plane. FT-IR measurements showed that the molecular structure of the alkoxide was retained, to a large extent, when dissolved in toluene–2-propanol (2 ∶ 1) or hexane. Investigations by UV-Vis and FT-IR spectroscopy showed that Ln5O(OPri)13 reacted with Al4(OPri)12 (Ln ∶ Al = 1 ∶ 3) in toluene–2-propanol to form LnAl3(OPri)12 within 2 hours at 80 °C. |
| Databáze: | OpenAIRE |
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