Synthesis and H-1-, N-15-, P-31-, W-183-multinuclear magnetic resonance study of the cyclotriphosphazenes [N3P3(dobp)2(OC5H4N-4)(2)] and [N3P3(dobp)(OC5H4N-4)(4)] and their W(CO)(5) complexes (dobp=2,2 '-dioxybiphenyl)

Citation
Ga. Carriedo et al., Synthesis and H-1-, N-15-, P-31-, W-183-multinuclear magnetic resonance study of the cyclotriphosphazenes [N3P3(dobp)2(OC5H4N-4)(2)] and [N3P3(dobp)(OC5H4N-4)(4)] and their W(CO)(5) complexes (dobp=2,2 '-dioxybiphenyl), EUR J INORG, (6), 1999, pp. 1015-1020
Citations number
34
Categorie Soggetti
Inorganic & Nuclear Chemistry
Journal title
EUROPEAN JOURNAL OF INORGANIC CHEMISTRY
ISSN journal
14341948 → ACNP
Issue
6
Year of publication
1999
Pages
1015 - 1020
Database
ISI
SICI code
1434-1948(199906):6<1015:SAHNPW>2.0.ZU;2-9
Abstract
The reactions of [N3P3(dobp)(2)Cl-2] and [N3P3(dobp)Cl-4] with a mixture of HOC5H4N-4 and K2CO3 in acetone give the cyclotriphosphazenes [N3P3 (dobp)( 2)(OC5H4N-4)(2)] and [N3P3 (dobp)(OC5H4N-4)(4)], respectively. These compou nds react with [W(MeDH)(CO)(5)] in methanol to give mixtures of the polymet allic complexes [N3P3(dobp)(2)(OC5H4N-4)(2){W (CO)(5)}(x)] (x = 1, 2) and [ N3P3(dobp)(OC5H4N-4)(4){W(CO)(5)}(x)] (x = 1-4), which are unstable in solu tion, slowly undergoing loss of the pentacarbonyl moiety. A complete charac terization by H-1, N-15, P-31, W-183 magnetic resonance has revealed that t he complexation of the N atom of one 4-oxypyridine ligand by the W(CO)(5) f ragment has a measurable effect on other parts of the phosphazene molecule very far away from the coordination site. The changes observed in delta(183 )W have been used to identify the components in mixtures of compounds incor porating different numbers of tungsten atoms in the molecule. The character ization of less sensitive nuclei has been accomplished by means of indirect detection methods.