Hydrothermal reactions of Zn(II) or Pb(II) ions with 4-pyridyl-CH2N(CH2COOH)(CH2PO3H2) (H3L) afforded two metal phosphonates, namely, [Zn3(L)2]·2H2O (1) and [Pb3(L)2(H2O)2]·H2O (2). Compound 1 is a 3D pillared framework in which [ZnO4] tetrahedra and [ZnO3N2] trigonal-bipyramids are connected by L3− anions with heptadentate modes. In 2, L3− anions exhibit pentadentate modes to combine Pb(II) ions into a complicated 2D hybrid layer, resulting in the non-coordinated pyridine rings being sandwiched between the layers. Solid 1 is thermally stable up to 350 °C under an air atmosphere and displays bright purple–blue luminescence, and the luminescent intensity of the hydrated solid 1 can be weakened by nitrobenzene.
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