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A family of 3D lanthanide metal–organic frameworks, [La(HTADIP)(H2O)4]·xH2O (2 < x < 2.5) (1), [Eu(HTADIP)(H2O)4]·H2O (2), [Tb(HTADIP)(H2O)3]·2H2O (3), and [Er(HTADIP)(H2O)3]·2H2O (4) (H4TADIP = 5,5′-(1H-1,2,3-triazole-1,4-diyl)diisophthalic acid), have been hydrothermally synthesized and characterized. The unsymmetrical 1,2,3-triazole-containing tetracarboxylate ligand was synthesized through the copper-catalyzed azide–alkyne cycloaddition (CuAAC) reaction of diethyl-5-azidoisophthalate (M1) and diethyl-5-ethynylisophthalate (M2). Single-crystal X-ray diffraction analyses for 1–4 reveal that they are isostructural. These compounds crystallize in the monoclinic P21/c space group with the rutile topology. The luminescent properties of compounds 2 and 3 were investigated and characteristic Eu(III) and Tb(III) emissions are observed. Compound 3 exhibits selective luminescent sensing behavior for Cu2+ ions in aqueous solution. The magnetic properties of compounds 3 and 4 were studied.
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