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The reaction of the organometallic diarsene complex [Cp 2 Mo 2 (CO) 4 (η 2 ‐As 2 )] ( 1 ) with Ag[Al{OC(CF 3 ) 3 } 4 ] (Ag[TEF]) yielded the Ag I  monomer [Ag(η 2 ‐ 1 ) 3 ][TEF] ( 2 ). This compound exhibits dynamic behavior in solution, which allows directed selective synthesis of unprecedented organometallic–organic hybrid assemblies upon its reaction with N‐donor organic molecules by a stepwise pathway, which is supported by DFT calculations. Accordingly, the reaction of  2  with 2,2′‐bipyrimidine ( L1 ) yielded the dicationic molecular compound [{(η 2 ‐ 1 ) 2 Ag} 2 (μ‐ L1 )][TEF] 2  ( 3 ) or the 1D polymer [{(η 2 ‐ 1 )Ag}(μ‐ L1 )]  n  [TEF]  n   ( 4 ) depending on the ratio of the reactants. However, its reactions with the pyridine‐based linkers 4,4′‐bipyridine ( L2 ), 1,2‐bis(4‐pyridyl)ethylene ( L3 ) and 1,2‐bis(4‐pyridyl)ethyne ( L4 ) allowed the formation of the 2D polymers [{(η 2 ‐ 1 )Ag} 2 (μ‐ L x  ) 3 ]  n  [TEF] 2 n   [ L x =L2  ( 5 ),  L3  ( 6 ),  L4  ( 7 ), respectively]. Additionally, this concept was extended to step‐by‐step one‐pot reactions of  1 , [Ag(CH 3 CN) 3 ][Al{OC(CF 3 ) 2 (CCl 3 )} 4 ] ([Ag(CH 3 CN) 3 ][TEF Cl ]) and linkers  L2 – L4  to produce the 2D polymers [{(η 2 ‐ 1 )Ag} 2 (μ, L x  ) 3 ]  n  [TEF Cl ] 2 n   [ Lx = L2  ( 8 ),  L3  ( 9 ),  L4  ( 10 ), respectively].

chemistry – a european journal

Mixed Organometallic–Organic Hybrid Assemblies Based on the Diarsene Complex [Cp 2 Mo 2 (CO) 4 (μ,η 2 ‐As 2 )], Ag I  Salts and N‐Donor Organic Molecules