Two multiligand coordination compounds, [Mn(AZT) 4 (2), were synthesized with 3-azido-1,2,4-triazole (AZT) as a ligand and picrate (PA) as a counteranion and characterized by elemental analysis and FTIR spectroscopy. The crystal structures were determined by single-crystal X-ray diffraction. The results show that the crystals of 1 and 2 have a triclinic space group (P1) and orthorhombic space group (Pbca), respectively. Moreover, 1 and 2 have distorted octahedral structures. Their thermal decomposition mechanisms were investigated by