A new hybrid compound formulated as [Fe3F8(H2O)(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 P (1) over bar with unit cell parameters a = 7.100(2) angstrom, 6 = 7.658(2) angstrom, c = 8.321(2) angstrom, alpha = 107.330(20)degrees, beta = 111.842(18)degrees, gamma = 93.049(17), Z = 1 and V = 394.01(17) angstrom(3). The studied X-ray crystal structure shows the two oxidation states for iron atoms (Fe2+, Fe3+) 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 (Fe3+(3)F-6) octahedral. OW-H center dot center dot center dot F and N-H center dot center dot center dot 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.