Four new complexes, [Zn(TIBTC)(DMA)]center dot[NH2(CH3)(2)] (1), [Cd(TIBTC)(H2O)]center dot[NH2(CH3)(2)]center dot DMA (2), [Cd-2(TIBTC)(2,2'-bipy)(2)(HCOO)] (3), and [Cd-2(DIBTC)(2,2'-bipy)(2)(HCOO)] (4) (H3TIBTC = 2,4,6-triiodo-1,3,5-benzenetricarboxylic acid, H3DIBTC = 2,4-diiodo-1,3,5-benzenetricarboxylic acid, 2,2'-bipy = 2,2'-bipyridine, and DMA = dimethylacetamide), were successfully synthesized and characterized by elemental analysis, powder X-ray diffraction, infrared spectroscopy, ultraviolet- visible spectroscopy, and thermogravimetric analysis. Complexes 1 and 2 are three-dimensional supramolecular network structures, while complex 4 has a two-dimensional network structure. We preliminarily studied the fluorescence properties of the complexes and found that complexes 1 - 3 can detect thiamine hydrochloride, NACs, and Fe3+/Zn2+ with high sensitivity and selectivity.