Bisstibane-distibane conversion via consecutive single-electron oxidation and reduction reaction.

peri -Substituted naphthalene complexes (Trip 2 Pn) 2 Naph (Pn = Sb 1, Bi 2) were synthesised and their redox behaviour investigated. Oxidation of 1 with [Fc][BAr F ] (BAr F = B(C 6 F 5 ) 4 ) yielded [(Trip 2 Sb)(TripSb)Naph][BAr F ] (3) containing the stibane-coordinated stibenium cation [(Trip 2 Sb)(TripSb)Naph] + . Subsequent reduction of 3 with KC 8 yielded distibane (TripSb) 2 Naph (4). 1-4 were characterised by NMR ( 1 H, 13 C) and IR spectroscopy as well as single-crystal X-ray diffraction (sc-XRD), while their electronic structures were analysed by quantum chemical computations.