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The reaction of the organometallic diarsene complex [Cp 2 Mo 2 (CO) 4 (μ,η 2 ‐As 2 )] ( B ) (Cp = C 5 H 5 ) with Ag[FAl{OC 6 F 10 (C 6 F 5 )} 3 ] (Ag[FAl]) and Ag[Al{OC(CF 3 ) 3 } 4 ] (Ag[TEF]), respectively, yields three unprecedented supramolecular assemblies [(η 2 ‐ B ) 4 Ag 2 ][FAl] 2  ( 4 ), [(μ,η 1 :η 2 ‐ B ) 3 (η 2 ‐ B ) 2 Ag 3 ][TEF] 3  ( 5 ) and [(μ,η 1 :η 2 ‐ B ) 4 Ag 3 ][TEF] 3  ( 6 ). These products are only composed of the complexes  B  and Ag I . Moreover, compounds  5  and  6  are the only supramolecular assemblies featuring  B  as a linking unit, and the first examples of [Ag I ] 3  units stabilized by organometallic bichelating ligands. According to DFT calculations, complex  B  coordinates to metal centers through both the As lone pair and the As−As σ‐bond thus showing this unique feature of this diarsene ligand.

The Potential of the Diarsene Complex [(C 5 H 5 ) 2 Mo 2 (CO) 4 (μ,η 2 ‐As 2 )] as a Connector Between Silver Ions