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Synthesis, Characterization, and Structure Determination of a New Heterometallic Oxoalkoxide: Er2Ti4O2(OC2H5)18(HOC2H5)2

✍ Scribed by G. Westin; R. Norrestam; M. Nygren; M. Wijk


Publisher
Elsevier Science
Year
1998
Tongue
English
Weight
411 KB
Volume
135
Category
Article
ISSN
0022-4596

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✦ Synopsis


Different synthesis routes have been studied for the preparation of a new oxoalkoxide, Er 2 Ti 4 O 2 (OEt) 18 (HOEt) 2 (Et‫؍‬ C 2 H 5 ). The compound was best prepared by reacting KOEt and Ti(OEt) 4 first with water and then with ErCl 3 . The structure was determined by single-crystal X-ray diffraction, showing the unit cell to have the monoclinic space group symmetry, P 2 1 /n, and the lattice constants a ‫؍‬ 15.180(2) A > , b ‫؍‬ 12.693(2) A > , c ‫؍‬ 16.602(3) A > and ‫؍‬ 98.91(1)Β°and to contain two formula units. The final R value was 0.053 (wR ‫؍‬ 0.077). The molecule contains three of the most commonly found structure fragments of alkoxides, namely the C 2h fragment of Ti 4 (OEt) 16 (Er 2 Ti 2 O 6 ), the M 4 ( 4 -O) fragment (Er 2 Ti 2 O), and the face-sharing MO 6 octahedra, with M ‫؍‬ Ti 4Ψ‰ . IR studies revealed that the molecular structure of the alkoxide was retained to a large extent when the alkoxide was dissolved in 4 : 1 ethanol : toluene and hexane solvents.


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The title compound (named MU-~) is a new layered aluminophosphate with a unusual Al/P ratio for this kind of materials. Mu-4 was obtained From a quasi nonaqueous mixture involving mainly diethylfonnamide (DEF) as solvent, in addition to limited amounts of water. DEF is decomposed during the synthesi