Five new coordination polymers, namely, [Zn(2)(H(2)O)(2)(BBC)](NO(3))(DEF)(6) (DUT-40), [Zn(3)(H(2)O)(3)(BBC)(2)] (DUT-41), [(C(2)H(5))(2)NH(2)][Zn(2)(BBC)(TDC)](DEF)(6)(H(2)O)(7) (DUT-42), [Zn(10)(BBC)(5)(BPDC)(2)(H(2)O)(10)](NO(3))(DEF)(28)(H(2)O)(8) (DUT-43), and [Co(2)(BBC)(NO(3))(DEF)(2)(H(2)O)](DEF)(6)(H(2)O) (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-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.