Abstract
Abstract For a more extensive 31P NMR spectroscopic study several new sulfides of unsymmetrically substituted bis(diorganylphosphinyl) sulfur diimides, tBU2(S)P(NSN)P(S)RR1 (R = R1 = iPr (3b), Cy (3c), Ph (3d); R = Ph, R1 = tBu (3e)), were prepared. These compounds, together with the symmetrically substituted chalcogenides tBu2(E)P(NSN)P(E)tBu2 (E = S (3a), Se (4a)) and carbonylmetal complexes of the type [(C0)5M]tBu2P(NSN)PRR1[M(C0)5] (R = R1 = tBu, M = Cr (1a); R = R1 = Ph, M = Mo(1b); R = Ph, R1 = tBu, M = Cr (lc), Mo (1d) and W (le)) as well as tBu2 P(NSN)PPhtBu-Mo(CO)4 (2) were studied by 31P NMR in solution and in the solid state (CP/MAS). Hahn-echo extended (HEED) pulse sequences were used to determine coupling constants 1J(31P15N) and one-bond isotope shifts 1Δ15/14N(31P) for all compounds. The sign and magnitude of 1J(31P15N) appear to be dominated by the electronic structure of the NSN system, in contrast with other P(III)-N and P(V)-N compounds. The 1Δ15/14N(31P) data (all negative) reflect the...
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