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Solvothermal reaction of 1,3,5-benzenetribenzoic acid (H3btb) with metal salts yielded two compounds with chemical formulas {(Me2NH2)[Zn(btb)(DMA)]·DMA}n (1) and [Mn3(btb)2(DMA)4·4DMA] (2) (DMA = N,N′-dimethylacetamide). 1 shows a 3D 4-fold interpenetrating (6,3) topological net, which has 1-D channels with counter anion and guest DMA molecules. 2 contains a two-dimensional bilayer structure based on a carboxylate bridged Mn3 cluster. 1 has no significant adsorption for H2 and N2 gas upon desolvation by long-time thermal activation, indicating that access to the void space is blocked by the immovable anions and interpenetrated feature. In addition, the 3D luminescence for 1 and magnetism for 2 were also explored.