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Complexes {Ln(TDA)(H2O)2} and {NMe2H2[Ln(TDA)(HCOO)} (Ln=Eu, Gd, Tb, H3TDA=1,2,3-Triazole-4,5-dicarboxylic acid) with the MOF structure can be obtained by solvothermal synthesis, depending on the solvent selected. Crystal structures of {Eu(TDA)(H2O)2} and {NMe2H2[Ln(TDA)(HCOO)} (Ln=Eu, Tb) were determined by X-ray diffraction. If a mixture of salts of two lanthanides is used in the synthesis, the corresponding mixed metal derivatives can be obtained. Such derivatives of terbium and europium were used as sensory materials, and the ratio of luminescence intensities of terbium and europium transitions served as an analytical signal. The sensory response to traces of water in aprotic solvents and D2O, as well as with respect to cations, was studied.