A new hybrid compound formulated as [Fe 3 F 8 (H 2 O) 2 ](Am 2 TAZ) 2 (Am 2 TAZ= 3,5-diamino-1,2,4-triazole) was prepared under hydrothermal conditions. The crystal structure was solved by single-crystal X-ray diffraction and the bulk was characterized by thermal analyses (TG-MS), vibrational spectroscopy (FTIR, Raman), Ultraviolet-visible spectroscopy (UV-Vis), and scanning electron microscopy (SEM-EDX). It crystallizes in the triclinic system space group P1 ̅ with unit cell parameters a= 7.100(2) Å, b= 7.658(2) Å, c= 8.321(2) Å, α= 107.330(20)°, β= 111.842(18)°, γ = 93.049(17)°, Z= 1 and V= 394.01(17) Å 3. The studied X-ray crystal structure shows the two oxidation states for iron atoms (Fe 2+ , Fe 3+) and generates a 2D inorganic network, built up of inorganic layers constructed from infinite inorganic chains running along a axis. In fact, these chains are connected via (Fe 3+ (3)F 6) octahedral. OW-H ... F and N-H ... F hydrogen bonds, making up the whole 3D network, are strongly linked in the layers. Magnetization measurements were performed, exhibiting the paramagnetic feature of the studied compound above 150 K.