| Summary: | A new strategy for the easy polymerization of anionic [Ln(Q<sup>cy</sup>)<sub>4</sub>]<sup>−</sup> (HQ<sup>cy</sup>-4-(cyclohexanecarbonyl)-5-methyl-2-phenyl-2,4-dihydro-3H-pyrazol-3-one) into two-dimensional layers of [AgLn(Q<sup>cy</sup>)<sub>4</sub>]<sub>n</sub> (Ln = Sm, Eu, Gd, Tb and Dy) is proposed by binding the single molecular anions [Ln(Q<sup>cy</sup>)<sub>4</sub>]<sup>−</sup> to silver cations through the coordination of the pyridinic nitrogen atoms of the pyrazolonate rings. The luminescent properties of [AgLn(Q<sup>cy</sup>)<sub>4</sub>]<sub>n</sub> have been studied in detail, and it was shown that the previously described low photoluminescence quantum yield (PLQY) of [Eu(Q<sup>cy</sup>)<sub>4</sub>]<sup>−</sup> is due to Ligand-To-Metal Charge Transfer (LMCT) quenching, which is effectively suppressed in the heterometallic [AgEu(Q<sup>cy</sup>)<sub>4</sub>]<sub>n</sub> polymer. Sensibilization coefficients for H<sub>3</sub>O[Eu(Q<sup>cy</sup>)<sub>4</sub>], [AgEu(Q<sup>cy</sup>)<sub>4</sub>]<sub>n</sub>, and H<sub>3</sub>O[Sm(Q<sup>cy</sup>)<sub>4</sub>] complexes (n ≈ 1) were estimated via theoretical analysis (also by using Judd-Ofelt theory for Sm<sup>3+</sup>) and PLQY measurements.
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