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Two hexanuclear paddlewheel-like clusters appending six carboxylic-acid pendants have been isolated with the inclusion of polar solvent guests: [Cu 6 (Hmna) 6 ]·7DMF ( 1 ·7DMF) and [Ag 6 (Hmna) 6 ]·8DMSO ( 2 ·8DMSO), where H 2 mna = 2-mercaptonicotininc acid, DMF =  N , N ’-dimethylformamide, and DMSO = dimethyl sulfoxide. The solvated clusters, together with their fully desolvated forms  1  and  2 , have been characterized by FTIR, UV–Vis diffuse reflectance spectroscopy, TG-DTA analysis, and DFT calculations. Crystal structures of two solvated clusters  1 ·7DMF and  2 ·8DMSO have been unambiguously determined by single-crystal X-ray diffraction analysis. Six carboxylic groups appended on the clusters trap solvent guests, DMF or DMSO, through H-bonds. As a result, alternately stacked lamellar architectures comprising of a paddlewheel cluster layer and H-bonded solvent layer are formed. Upon UV illumination ( λ  ex  = 365 nm), the solvated hexasilver(I) cluster  2 ·8DMSO gives intense greenish-yellow photoluminescence in the solid state ( λ  PL  = 545 nm,  Φ  PL  = 0.17 at 298 K), whereas the solvated hexacopper(I) cluster  1 ·7DMF displays PL in the near-IR region ( λ  PL  = 765 nm,  Φ  PL  = 0.38 at 298 K). Upon complete desolvation, a substantial bleach in the PL intensity ( Φ  PL  < 0.01) is observed. The desorption–sorption response was studied by the solid-state PL spectroscopy. Non-covalent interactions in the crystal including intermolecular H-bonds, CH⋯π interactions, and π⋯π stack were found to play decisive roles in the creation of the lamellar architectures, small-molecule trap-and-release behavior, and guest-induced luminescence enhancement.

Solid-State Structures and Photoluminescence of Lamellar Architectures of Cu(I) and Ag(I) Paddlewheel Clusters with Hydrogen-Bonded Polar Guests