Five new 2D coordination polymers, [Co(nip)(CuL)(H2O)]·CH3OH (1), [Mn(ip)(NiL)]·0.63H2O (2), [Cu(ip)(CuL)] (3), [Mn6(CuL)6(btc)4(H2O)4]·7H2O (4), and [Cu(CuL)(Hbtc)(H2O)] (5)(ML, H2L = 2,3-dioxo-5,6,14,15-dibenzo-1,4,8,12-tetraazacyclo-pentadeca-7,13-diene; H2nip = 5-nitroisophthalic acid; H2ip = m-isophthalic acid; H3btc = 1,3,5-benzenetricarboxylic acid) have been synthesized by a solvothermal method and characterized by single-crystal X-ray diffraction. Complexes 1–5 exhibit different 2D layered structures formed by Co2Cu2 (1), Mn2Ni2 (2), Cu4 (3), Mn3Ni3 (4), Cu4 (5) units, respectively, via the oxamide and diverse carboxylic acid bridges. Compounds 1, 2, 3 and 5 are uninodal 4-connected (4, 4)-grids topology, while complex 4 possesses a 2D network with (3, 4)-connected (42.8)4(43.62.8)3 topology. The results of magnetic determination show pronounced antiferromagnetic interactions in 1–4.