Abstract
Interaction of [Ru(Co)H(Et 2dtc)with triflic acid (HOTf) afforded [Ru(Co)H(Et 2dtc)(PPh 3) 2(OTf) ( 1), which has been characterized by X-ray crystallography. The RuC, RuO, average RuS and average RuP distances in 1 are 1.811(5), 2.216(3), 2.433 and 2.423 Å, respectively. Reaction of 1 with amines L results in the formation of adducts trans-[Ru(CO)(Et 2dtc)(PPh 3) 2L](OTf) (L=N 2H 4 ( 2) and NH 2OH ( 3)). The RuC, RuN, average RuS and average RuP distance in 3 are 1.85(1), 2.179(8), 2.433 and 2.393, respectively; the RuNO angle being 119.7(5)°. Treatment of 1 with [N nBu 4][OsN(C 7H 6S 2) 2] ([C 7H 6S 2] 2−=3,4-toluenedithiolate(2−)), and [ReN(Et 2dtc) 2] (Et 2dtc= N, N-diethyldithiocarbamate) gave the corresponding μ-nitrido complexes [Ru(CO)(Et 2dtc)(PPh 3) 2(NOsO 3)] ( 4), [Ru(CO)(Et 2dtc)(PPh 3) 2{NOs(C 7H 6S 2) 2}] ( 5) and [Ru(CO)(Et 2dtc)(PPh 3) 2{NRe(Et 2dtc) 2}] ( 6). The structures of complexes 4– 6 have been established by X-ray crystallography. The OsN and RuN distances, and OsNRu angle in 4 are 1.719(7) and 2.075(7) Å, and 155.1(4)°, respectively. The OsN and RuN distances and OsNRu angle in 5 are 1.680(6) and 2.068(6) Å, and 166.2(3)°, respectively. The ReN and RuN distances, and ReNRu angle for 6 are 1.670(3) and 2.108(3) Å, and 170.9(2)°, respectively. The bond lengths and angles for these μ-nitrido complexes are indicative of asymmetric bridging mode of nitride, i.e. MN→Ru(II) (M=Os(VIII), Os(VI), Re(V)).
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