Two novel metal-organic coordination compounds, [Co-2(OH)(chdc)(1.5)(bibp)](n) (1) and [Ni(chdc)(bib)](n)center dot 2nH(2)O (2, H(2)chdc = 1,4-cyclohexanedicarboxylic acid, bibp = 4,4'-bis(1imidazolyl)biphenyl, bib = 1,4-bis(1-imidazolyl)benzene), were synthesized and characterized. Compound 1 crystallizes in monoclinic system, space group P (1) over bar with a = 10.591(3), b = 11.146(3), c = 12.264(3) angstrom(3), alpha = 89.009(6), beta = 88.397(4), gamma = 87.823(3)degrees, V = 1446.0(6) angstrom(3), D-c = 1.554 g/cm(3), C30H30Co2N4O7, M-r = 676.44, F(000) = 696, mu(MoK alpha) = 1.202 mm(-1), Z = 2, R = 0.0278 and wR = 0.0718. In 1, it contains an interesting tetranuclear Co(II) cluster. The neighboring {Co-4} clusters are linked by chdc(2-) ligands to generate a 2D network. The bibp ligands connect adjacent layers to form an open 3D metal-organic framework. Compound 2 crystallizes in monoclinic system, space group P2(1)/n with a = 8.8110(1), b = 19.369(1), c = 12.7379(4) angstrom, beta = 102.952(5)degrees, V = 2118.5(2) angstrom(3), D-c = 1.490 g/cm(3), C20H24N4NiO6, M-r = 475.14, F(000) = 992, mu(MoK alpha) = 0.961 mm(-1), Z = 4, R = 0.0306 and wR = 0.0738. In 2, each deprotonated chdc 2- ligand links two Ni(II) atoms to generate a 1D chain along the a axis. The adjacent chains are further connected by bib ligands to build up an interesting two-dimensional network. Compound 1 shows antiferromagnetic property.