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)
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
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.