Isolation of an Arsenic Diradicaloid with a Cyclic C(2) As(2) -Core

分离具有环状 C(2)As(2) 核心的砷双自由基化合物

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Abstract

Herein, we report on the synthesis, characterization, and reactivity studies of the first cyclic C(2) As(2) -diradicaloid {(IPr)CAs}(2) (6) (IPr = C{N(Dipp)CH}(2) ; Dipp = 2,6-iPr(2) C(6) H(3) ). Treatment of (IPr)CH(2) (1) with AsCl(3) affords the Lewis adduct {(IPr)CH(2) }AsCl(3) (2). Compound 2 undergoes stepwise dehydrochlorination to yield {(IPr)CH}AsCl(2) (3) and {(IPr)CAsCl}(2) (5 a) or [{(IPr)CAs}(2) Cl]OTf (5 b). Reduction of 5 a (or 5 b) with magnesium turnings gives 6 as a red crystalline solid in 90% yield. Compound 6 featuring a planar C(2) As(2) ring is diamagnetic and exhibits well resolved NMR signals. DFT calculations reveal a singlet ground state for 6 with a small singlet-triplet energy gap of 8.7 kcal mol(-1) . The diradical character of 6 amounts to 20% (CASSCF, complete active space self consistent field) and 28% (DFT). Treatments of 6 with (PhSe)(2) and Fe(2) (CO)(9) give rise to {(IPr)CAs(SePh)}(2) (7) and {(IPr)CAs}(2) Fe(CO)(4) (8), respectively.

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