The crystallization and magnetic behavior of yttrium iron garnet (YIG) prepared by metalloorganic decomposition (MOD) method are discussed. The chemistry and physics related to synthesis of iron and yttrium carboxylates based on 2-ethylhexanoic acid (2EHA) are studied, since no literature was found which elucidates synthesis of metallo-organic precursor of YIG in spite of the literatures of doped YIG samples such as Bi-YIG. Typically, the metal carboxylates used in preparation of ceramic oxide materials are 2-ethylhexanoate (2EH) solvents. Herein, the synthesis, thermal behavior and solubility of yttrium and iron 2EH used in synthesis of YIG powder by MOD are reported. The crystallization and magnetic parameters, including saturation magnetization and coercivity of these samples, smoothly change as a function of the annealing temperature. It is observed that high sintering temperature of 1300 to 1400 °C promotes the diffraction peaks of YIG, therefore, we can conclude that the formation of YIG in MOD method increases the crystallization temperature. The maximum value of saturation magnetization and minimum value of coercivity and remanence are observed for the sample sintered at 1200°C which are 13.7 emu/g, 10.38 Oe and 1.5 emu/g, respectively. This study cites the drawbacks in chemical synthesis of metallo-organic based YIG production. 2