Two series of twelve polycarboxylate lanthanide coordination polymers (CPs), namely, [Ln(cpida)(H2O)]n{Ln=La (1), Ce (2), Pr (3) and Nd (4)} and {[Ln(cpida)(H2O)]⋅2H2O}n {Ln=Sm (5), Eu (6), Gd (7), Tb (8), Dy (9), Ho (10), Er (11) and Yb (12)} {H3cpida=N‐(4‐carboxyphenyl) iminodiacetic acid}, have been synthesized by self‐assembly and characterized by IR, TGA, X‐ray crystallography, powder XRD and elemental analysis. CPs 1–4 and 5–12 are isomorphic respectively, featuring 2D double layer structures. In CPs 1‐4, each metal atom connects five [cpida]3− anions and each ligand is bound to five metal cations. However, in 5‐12 each [cpida]3− anion only connects four metal cations due to the lanthanide contraction. Further, PL spectra of CPs 6, 8 and 12 show the strong characteristic luminescence of Eu(III), Tb(III) and Yb(III) ions, respectively, suggesting that [cpida]3‐ is able to sensitize the luminescence of lanthanide ions efficiently. The magnetic properties of Gd (7) and Dy (9) complexes have also been investigated.

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