Five new coordination polymers, namely, [Zn ₂(H ₂O) ₂(BBC)](NO ₃)(DEF) ₆ (DUT-40), [Zn ₃(H ₂O) ₃(BBC) ₂] (DUT-41), [(C ₂H ₅) ₂NH ₂][Zn ₂(BBC)(TDC)] (DEF) ₆(H ₂O) ₇ (DUT-42), [Zn ₁₀(BBC) ₅(BPDC) ₂(H ₂O) ₁₀](NO ₃)(DEF) ₂₈(H ₂O) ₈ (DUT-43), and [Co ₂(BBC)(NO ₃)(DEF) ₂(H ₂O)](DEF) ₆(H ₂O) (DUT-44), where BBC - 4,4′,4′′- (benzene-1,3,5-triyl-tris(benzene-4,1-diyl))tribenzoate, TDC - 2,5-thiophenedicarboxylate, BPDC - 4,4′-biphenyldicarboxylate, DEF - N,N-diethylformamide, were obtained under solvothermal conditions and structurally characterized. It has been shown that compounds DUT-40, DUT-41 and DUT-44 exhibit 2D layered structures with large hexagonal channels. Utilization of additional angular dicarboxylic TDC linker led to the formation of the DUT-42 compound with the structure consisting of three interpenetrated 3D networks. Using the linear co-linker dicarboxylic BPDC, DUT-43 was obtained which forms a complicated 3D architecture arising from the polycatenation of triple-layered 2D building units and 2D single layer units. The pore accessibility of the synthesized compounds in the liquid phase was proved by the adsorption of dye molecules.