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]

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

doi:10.1039/DT9950001357

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Journal of the Chemical Society, Dalton Transactions

Issue 8, 1995

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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]

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

J. Chem. Soc., Dalton Trans., 1995, 1357-1361

DOI: 10.1039/DT9950001357

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Abstract
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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.

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Journal of the Chemical Society, Dalton Transactions

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]

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