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The synthesis of the first unsupported dicationic arene complexes of calcium and strontium [(η6-HMAE(oDF4]2+ is reported (HMB = hexamethylbenzene; AE = alkaline earth metal; oDFB = ortho-difluorobenzene). They were prepared by direct oxidation of the elemental metals employing the ligand-forming radical cation salt [HMB][WCA] as an oxidant (WCA = [Al(ORF)4] or [μF-Al(ORF)32]; RF = C(CF3)3). In addition, monocationic η6-HMB complexes of calcium, strontium and barium supported by coordination of the monodentate anion [F-Al(ORF)3]- ar
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