Pf. Kelly et al., USE OF SE4N4 AND SE(NSO)(2) IN THE PREPARATION OF PALLADIUM ADDUCTS OF DISELENIUM DINITRIDE, SE2N2 - CRYSTAL-STRUCTURE OF [PPH(4)](2)[PD2BR6(SE2N2)], Journal of the Chemical Society. Dalton transactions, (4), 1997, pp. 559-562
Reaction of Se4N4 with [NBu(4)(n)](2)[Pd2Br6] at 100 degrees C in CH2C
l2 resulted in [NBu(4)(n)](2)[Pd2Br6(Se2N2)] 1a in high yield (67%). I
n contrast to the reaction of [PPh(4)](2)[Pd2Br6] with S4N4, which gen
erates a number of products, the tetrabutylammonium salt generated onl
y [NBu(4)(n)](2)[Pd2Br6(S2N2)] 1b; comparison of the IR spectra of la
and Ib allows unambiguous identification of the two bands due to E(2)N
(2) vibrations: While reaction of S(NSO)(2) with [Pt(PPh(3))(3)] leads
to a mixture of [Pt(S2N2)(PPh(3))(2)] and [Pt(NSO)(2)(PPh(3))(2)], on
ly the latter species forms in the analogous reaction of Se(NSO)(2). T
wo different results were also found in-reactions with [PPh(4)](2)[Pd2
Br6]; while S(NSO)(2) appeals surprisingly inert to this reagent, Se(N
SO)(2) reacts, when-present in excess, to give the unexpected product
[PPh(4)](2)[Pd2Br6(Se2N2)] 1c. The crystal structure of the latter con
firms the presence of the adducted diselenium dinitride unit.