Two complexes,Co(LPy)2(1) and Ni(LPy)2(2) were synthesized from the reaction of Benzylidene Acetone Salicylhydrazone (HL) with Co(NO3)2, Ni(NO3)2,and characterized by FTIR,thermal analysis,single crystal X-ray diffrac-tion and XRD.The results of structuralanalysis indicate that both complexes aredistorted octahedral.Complex 1 belongs to triclinic system,space group P-1 witha=1.0347(3)nm,b=1.0052(4)nm,c=1.4541(4)nm;α=92.830(4)?β=109.054(3)?γ= 96.091(4)?V=1.9792(10)nm3,Z=2,F(000) =814,R1=0.0506.Complex 2 belongs to triclinic system,space group P-1 with a=1.0435(5)nm,b=1.3940(7)nm,c=1.4542(7)nm;α=92.41(2)?β=109.73(2)?γ=95.80(2)?V=1.9745(17)nm3,Z=2,F(000) =816,R1=0.0438.The result of TG analysis shows that the title complexswere stable under 200 ℃.