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Two new complexes with composition {[Ni(L1)(mip)(H 2 O)]·3.6H 2 O} n (1) and {[Co(L2) 2 (npht)]·H 2 O} n (2) [H 2 mip = 5-methylphthalic acid, H 2 npht = 5-nitrophthalic acid, L1 = 1,3-bis(thiabendazol-1-ylmethyl)benzene, L2 = 1,4-bis(thiabendazol-1-ylmethyl)benzene)] were hydrothermally synthesized and characterized by physicochemical and spectroscopic methods. 1 displays a binuclear [Ni 2 L1 2 (mip) 2 structure and further extends into a 2D layer via O–H⋯O hydrogen bond interactions, 2 holds a 1D zigzag linear chain which is further packed via C–H⋯O hydrogen bond interactions into a 3D supramolecular network. Sensing experiments indicate that both complexes can be as high selectivity and sensitivity fluorescent chemosensors for ethylene glycol and Fe3+/Cu2+. Two new complexes were synthesized under hydrothermal condition. The complex 1 displays a binuclear [Ni 2 L1 2 (mip) 2 structure and further extends into a 2D layer via O–H⋯O hydrogen bond. 2 holds a 1D zigzag linear chain which is further linked through C–H⋯O hydrogen bond into a 3D supramolecular network. Sensing experiments indicate that both compounds can be used as highly selective and sensitive fluorescent chemosensors for ethylene glycol and Fe3+/Cu2+. Image 1 • Two bis(thiabendazole) complexes were synthesized and characterized. • 1 and 2 are packed into 2D/3D supramolecular networks by hydrogen bonding. • 1 and 2 exhibit highly sensitive and selective for detection of ethylene glycol. • 1 and 2 could as good fluorescent chemosensors for Fe3+/Cu2+. [ABSTRACT FROM AUTHOR]