Metal organic frameworks (MOFs) contain inorganic and organic networks that can be easily functionalized to get tuneable properties. MOFs as highly porous crystalline materials constructed by coordination bonds between metal ions/clusters and organic ligands, have developed very fast due to not only their intriguing structures but also the potential applications, such as gas separation, storage, and sensing. They have great potential as adsorbents/catalysts due to their extremely large surface area, well-ordered porous structures, and diverse means available for functionalization. MOF-5 consists of four [Zn₄O]⁶⁺ clusters in octahedral subunits that are connected to each other by terephthalate or benzene-1,4-dicarboxylate (BDC) groups, to form a porous cubic framework [3]. In this work, we have synthesized Ni-doped, MOF-5 by solvothermal method according to the literature. The Ni-MOF was formed with cubic structure but changing the reaction conditions resulted to the novel hexagonnal structure. The characterization was performed by FTIR, XRD and SEM methods.