Herein, we synthesized  membered pyridine based transition metal macrocyclic complexes [MIILCl2] (M = Fe(II) and Ni(II), L = 6,12,5,11-tetraphenyl di(2-pyridyl)[b,h][1,4,7,10]-N4annulene). The synthesized macrocycles were characterized by using microanalysis (C, H, and N), DTA/TGA and other spectroscopic techniques. A nonplanar saddle-shaped octahedral geometry was assigned to the macrocycles. The TGA results indicated the higher stability of these macrocycles over 250°C temperature. Cyclic volumetric studies showed the abnormal quasi-reversible behavior for these complexes, which further indicates the unusual oxidation state on metal ions. In addition, these macrocyclic complexes possess good antimicrobial activities against E. coli, P. aeruginosa, B. cereus, S. aureus and antifungal against C. albicans when compared with Gentamycin.