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Thecontrol of the metallic nanocrystal shape is of prime importancefor a wide variety of applications. We report a detailed researchwork on metal–organic chemical routes for the synthesis ofa highly symmetrical crystal structure. In particular, this studyshows the key parameters ensuring the anisotropic growth of nickelnanostructures (fcc crystal). Numerous reaction conditions are investigated(precursors, solvents, temperature, reducing agents, reaction time,and types and ratios of surfactants, such as alkyl amines, carboxylicacids, and phosphine oxides), and their effects on the size and shapeof the final product are reported. The role of the growth modifiersand the structuring of the reaction media on the anisotropic growthare demonstrated. This metal–organic approach generates severalnovel anisotropic nanostructures in a wide size range depending onthe reaction conditions. In this way, nanomaterials with reproduciblesize, shape, and composition are obtained with good yield. Transmissionelectron microscopy techniques (TEM and HRTEM) are the principal methodsfor monitoring the morphology. [ABSTRACT FROM AUTHOR]