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THE ALKOXIDES OF ZIRCONIUM AND HAFNIUM - DIRECT ELECTROCHEMICAL SYNTHESIS AND MASS-SPECTRAL STUDY - DO M(OR)(4), WHERE M=ZR, HF, SN, REALLY EXISTстатья
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Статья опубликована в журнале из списка Web of Science и/или Scopus
Дата последнего поиска статьи во внешних источниках: 29 мая 2015 г.
- Авторы: TUREVSKAYA EP, KOZLOVA NI, TUROVA NY, BELOKON AI, BERDYEV DV, KESSLER VG, GRISHIN YK
- Журнал: Russian Chemical Bulletin
- Том: 44
- Номер: 4
- Год издания: 1995
- Издательство: Springer Nature
- Местоположение издательства: Switzerland
- Первая страница: 734
- Последняя страница: 742
- DOI: 10.1007/BF00698513
- Аннотация: The direct electrochemical synthesis of zirconium (la) and hafnium (Ib) alkoxides, M(OPri)(4) . (PrOH)-O-i, Zr(OBu(i))(4) . Bu(i)OH (4a) and M(OR)(4), where R = Et (2a,b), Bu(n) (3a), Bu(S) (5a), C(2)H(4)OMe (6a,b) has been carried out by anodic oxidation of metals in anhydrous alcohols in the presence of LiCl as a conductive additive to give quantitative yields. The solubility polytherms and dissociation pressure of la,b have been investigated. It has been proved by means of chemical analysis, X-ray powder, and IR spectral studies that the desolvation of 1a,b and Sn(OPri)(4) . (PrOH)-O-i (1c) is accompanied by the formation of amorphous oxocompounds M(3)O(OPri)(10). On the basis of H-1 NMR data it has been proved that the structure of the latter is analogous to that of known triangular cluster molecules M(3)(mu(3)-O)(mu(3)-OR)(mu-OR)(3)(OR)(6), where M = Mo, W, U. Mass-spectral data and the determined physicochemical characteristics of 1-5 permit to conclude that the samples of composition M(OR)(4), where M = Zr, Hf, and 2, 3, 5 contain tri- and tetranuclear oxocomplexes M(3)O(OR)(10) and M(4)O(OR)(14), respectively, along with Zr(OR)(4) oligomers of different molecular complexity.
- Добавил в систему: Гришин Юрий Константинович