Two complexes, {[Co(L)(H2O)(3)]Cl-2 center dot 2H(2)O}(n)(1) and [Cu-2(L)(2)Cl-4]center dot 3C(2)H(5)OH (2) were synthesized from the reaction of phenanthroline substituted glycoluril (L) with CoC12.6H(2)O and CuCl2 center dot 2H(2)O, and characterized by elemental analysis, IR and single crystal X-ray diffraction. Complex 1 crystallized in the orthorhombic system, space group P2(1)2(1)2(1), the coordination environment of Co(II) adopted a distorted octahedron geometry, being bound to three oxygen donor from one H2O molecule as well as to two nitrogen atoms and oxygen atoms from two adjacent molecules of L. Each ligand L acted as a tridentate ligand coordinating two metal atoms to generate a one-dimensional (1D) chain structure. Complex 2 crystallized in the monoclinic system, space group P2(1)/n, the coordination environment of Cu(II) adopted a distorted square taper geometry, being bound to three chlorine atom as well as to two nitrogen atoms from ligand L. There are two chlorine atoms coordinating two metal atoms to generate binuclear complex 2. CCDC:1030117, 1; 1030116, 2.