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Preparation of N(SeCl)2 +X- (X = SbCl6 or FeCl4), F3CCSeNSeCCF3 +SbCl6 -, F3CCSeNSeCCF3, F3CCSeNSeCCF3 and F3CCSeSeC(CF3)C(CF3)SeSeCCF3. Electron diffraction studyстатья
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Статья опубликована в журнале из списка Web of Science и/или Scopus
Дата последнего поиска статьи во внешних источниках: 14 февраля 2019 г.
- Авторы: Borisenko K.B., Broschag M., Hargittai I., Klapötke T.M., Schröder D, Schulz A., Schwarz H., Tornieporth-Oetting I.C., White P.S.
- Журнал: JOURNAL OF THE CHEMICAL SOCIETY-DALTON TRANSACTIONS
- Номер: 18
- Год издания: 1994
- Первая страница: 2705
- Последняя страница: 2712
- DOI: 10.1039/DT9940002705
- Аннотация: Full title: Preparation of N(SeCl)2 +X- (X = SbCl6 or FeCl4), F3CCSeNSeCCF3 +SbCl6 -, F3CCSeNSeCCF3, F3CCSeNSeCCF3 and F3CCSeSeC(CF3)C(CF3)SeSeCCF3. Electron diffraction study of F3CCSeSeCCF3 and crystal structure of the eight-membered heterocycle F3CCSeSeC(CF3)C(CF3)SeSeCCF3. The salts N(SeCl)2 +SbCl6 - 1 and N(SeCl)2 +FeCl4 - 2 were synthesized by reaction of SeCl3 + X-(X = SbCl6 or FeCl) with N(SiMe3)3; 1 was also formed by reaction of Se2NCl3 with SbCl5. Reaction of 1 with SnCl2 and F3CCCCF3 led to the formation of F3CCSeNSeCCF3 + SbCl6 - 3. In this reaction the Se2N + cation is a likely intermediate because SnCl2 seems to be essential for chloride abstraction in the first reaction step to generate Se2N+ in situ which then adds F3CCCCF3 to yield 3. Compound 3 is a useful building block to generate selenium compounds such as F3CCSeNSeCCF3 4, F3CCSeSeCCF3 5 and F3CCSeSeC(CF3)C(CF3)SeSeCCF3 6. The heterocycle 5 was shown by electron diffraction to have an approximately planar four-membered ring structure. The structure of compound 6 was determined by X-ray crystallography: orthorhombic, space group Pbca, a = 10.1920(21), b = 13.0615(20) and c = 22.050(5) Å. In order to rationalize the structures of 5 and the cation F3CCSeNSeCCF3 +, ab initio calculations were made on model compounds in which the CF3 groups were replaced by a fluorine atom (i.e. FCSeSeCF for 5and FCSeNSeCF+ for the cation in 3). In addition, mass spectrometric experiments were performed in order to examine the structures and stabilities of the unligated cation F3CCSeNSeCCF3 + as well as its neutral counterpart. The existence of the neutral radical 4 was established by means of neutralization-reionization mass spectrometry.
- Добавил в систему: Borisenko Konstantin B.