Ac ombination of ab ent bis(naphthalene) and hydroxy-basedd icarboxylate linker and af lexible bis(tridentate)polypyridyl ligand has been employed to self-assemble with two different d 10 metal centers, Zn II and Cd II ,t of orm structurally diversifiedl uminescent metal-organic frameworks, [Zn 2 (tpbn)(mbhna) 2 (H 2 O) 2 ]·4 H 2 O·1.5DMF (1)a nd {[Cd 2 (tpbn)(mbhna) 2 ]·2DMF} n (2), respectively (where, tpbn = N,N',N'',N'''-tetrakis(pyridine-2-ylmethyl)butane-1,4-diamine and H 2 mbhna = 4,4'-methylene-bis[3-hydroxy-2-naphthalene carboxylic acid]). Both 1 and 2 are characterizeda nd analyzed by various analytical techniques includings ingle-crys-tal X-ray diffractometry.T heire xcellent emissive nature is studied in different solvents andf urtheru tilized to selectively detect aromatica mines,p articularly 4-nitroaniline in water with detection limits at sub-ppm level. The difference in sensing activity of 1 and 2 toward 4-NA is corroborated well with their structures. The mechanism of action has been established through Stern-Volmer plot, spectral overlap, timeresolved lifetime studies and HOMO-LUMO energy calculations. In addition, 1 and 2 are found to be recyclable and display good stability after sensing experiments.[a] Dr.Figure 4. Effect of solvents on the emissionspectra of 1 (a) and 2 (b).