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A new mixed-valent Rh2II,III dimer, [Rh2(espn)2Cl] (espn2− = α,α,α′,α′-tetramethyl-1,3-benzenedipropanamidate), is reported. This compound readily dissociates Cl− at low concentrations in solution to form the active [Rh2(espn)2]+ catalyst, which performs intramolecular C–H amination with TONs > 1400. This work expands the scope of Rh2II,III dimers to nitrenoid chemistry.
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