Two complexes, [Cu(2)(Htdb)(4)(H(2)O)(2)] (1) and [Cd(bipy)(2)(Hmcmbc)(2)] (2) (H(2)tdb = 2,2-thiodibenzoic acid, H(2)mcmbc = m-(carboxyl-methyloxy)-benzenecarboxylic acid, bipy = 4,4'-bipyridine), have been prepared, and were characterized by elemental analysis, FT-IR and single-crystal X-ray diffraction. Structures indicate that complex 1 is a single molecule, and 2 is a one-dimensional chain. Their two-and three-dimensional frameworks are constructed through hydrogen bonding, pi center dot center dot center dot pi or C-H center dot center dot center dot pi stacking, and such other weak interactions. The cyclic voltametric behavior of complex 1 and luminescence property of complex 2 were investigated. 1 belongs to the triclinic system, space group P (1) over bar with a = 7.8607(6), b = 11.7619(9), c = 15.3481(12) angstrom, alpha = 109.3670(10), beta = 92.4420(10), gamma = 92.0450(10), V = 1335.65(18) angstrom(3), M(r) = 1256.26, D(c) = 1.5619(2) g/cm(3), F(000) = 642, mu = 1.029 mm(-1), Z = 1, the final R = 0.0289 and wR = 0.0763 for 5199 observed reflections with I > 2 sigma(I). Complex 2 crystallizes in triclinic, space group P (1) over bar with a = 9.6378(10), b = 9.7508(10), c = 19.055(2) angstrom, alpha = 88.7020(10), beta = 80.5260(10), gamma = 69.2000(10)degrees, V = 1649.9(3) angstrom(3), M(r) = 815.07, D(c) = 1.641 g/cm(3), mu = 0.732 mm(-1), F(000) = 828, Z = 2, the final R = 0.0511 and wR = 0.1149 for 4729 observed reflections (I > 2 sigma(I)).