Herein, we report the synthesis of a 3D hierarchical heterostructure microsphere through a facile solvothermal and hydrothermal method followed by an annealing treatment. The obtained ternary core-shell nanostructured was comprehensively characterized by means of variety techniques including FT-IR, XRD, BET, TEM, FE-SEM, EDX, EDX-mapping, VSM and ICPOES. It was found that this hierarchical nanostructured could promote the C???? P cross coupling reaction of a large library of functional substrates. Benefiting from the unique hierarchical architecture and the synergistic effect among multiple components resulted from the coexistence of micro-, meso- and macropores as well as its small nano-crystallite size (20-71 nm), this novel catalyst revealed superior catalytic performance in the C???? P cross coupling reaction. More importantly, the ferromagnetic behavior of 3D hierarchical core-shell Fe3O4@NiO/Co3O4 microspheres is responsible for easy separation from the reaction mixture using an external magnetic field and its long term-durability under reaction conditions even after nine consecutive recycle runs.

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