Abstract

Four crystalline one‐dimensional (1‐D) silver alkynyl assemblies, namely, [Ag11(tBuC≡C)7(CH3COO)4]n (1), [Ag21(tBuC≡C)11(PhCOO)10]n (2), [Ag16(m‐F‐PhC≡C)12(CF3COO)4(CH3CN)4]n (3) and [Cl@Ag14(PhC≡C)10(CF3SO3)3]n (4). have been obtained by reacting polymeric [AgC≡CR]n with silver salts under mild solvothermal conditions. Compound 1 and 3 are coordination polymer of irregular silver alkynyl clusters. Compound 2 consists of well‐defined parallel Ag3 triangles columns. Compound 4 is chains of chloride templated cage‐like silver clusters. Compound 2–4 show temperature‐sensitive luminescent behaviors. Amongst, compound 2 and 3 display dual‐emissive characteristic at low temperature. By correlating the structures and properties of four silver compounds, we found that the non‐emissive behavior of compound 1 could be tentatively assigned to the absence of any aryl groups on the ligands.

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