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Rhenium complex of a triply deprotonated chelated thiosemicarbazide and its conversion to a nitride complex via a hydrazide intermediate. Crystal structure of [ReCl2(NH)(NHNH2)(PPh3)2]

1995; Royal Society of Chemistry; Issue: 8 Linguagem: Inglês

10.1039/dt9950001357

2050-5671

Jonathan R. Dilworth, Jason S. Lewis, John R. Miller, Yifan Zheng,

Radiopharmaceutical Chemistry and Applications

Reaction of [Re(O)X3(PPh3)2](X = Cl or Br) with thiosemicarbazides RNHCSNHNH2(R = Me or Ph) in ethanol under reflux in the presence of aqueous HX and PPh3 gave the rhenium(V) S,N-chelated thiosemicarbazide(3–) complexes [ReX2(NNCSNHR)(PPh3)2]. On extended reflux for X = Cl the purple imide–hydrazide [ReCl2(NH)(NHNH2)(PPh3)2] was formed, and a crystal structure determination showed a pseudo-octahedral geometry with trans PPh3 and nitrogen ligands and a significantly bent M–N–N system (145.5°). Further reflux gave the known nitride complex [Re(N)Cl2(PPh3)2] in good yield.