The reactions of 5,5’-bis(2-acylphenyl)diazo-dipyrromethane(H2L) with CuSO4 and NiCl2 resulted in the formation of corresponding mononuclear coordination complexes 2(CuL)and 3(NiL).The crystal of complex 2 is of monoclinic system,space group P21 with α = 10.040(5),b = 11.900(5),c = 11.170(5) A,β = 93.057(8)°,V= 1332.8(2) A3,Z = 2,C29H28N6O2 Cu,Mr =556.11,Dc = 1.386 g/cm,F(000) = 578 and μ(MoKα) = 0.857 mm-1.The crystal of complex 3belongs to the monoclinic system,space group P21/n with α = 12.0445(6),b = 17.2101(8),c =16.3304(6) A,β = 128.407(2)°,V= 2654.6(2) A3,Z = 4,C29H28N6O2 Ni,Mr= 551.28,Dc = 1.380g/cm,F(000) = 1152 and μ(MoKα) = 0.770 mm-1.In both complexes,the metal ions are in square-planar geometry by coordinating to two azo N atoms and two deprotonated pyrrole N atoms.Intramolecular Cu…O=C in complex 2 and intermolecular Ni…O=C in complex 3 were found.The UV-Vis spectra and thermal stability of complexes 2 and 3 were also studied.