A new silver(I) compound, namely [Ag(MA)(FA)0.5] n ( 1) (MA = melamine, H2FA = fumaric acid), was synthesized via the reactions of AgNO3, MA, and H2FA. Single crystal X-ray diffraction analysis reveals that compound 1 is 2D undulated layer, which further extended into a 2D→3D interdigitated supramolecular framework by intermolecular hydrogen bonds. In addition, the catalytic property on degradation of methyl orange for compound 1 in a Fenton-like process was also investigated. [ABSTRACT FROM AUTHOR]