A new co-crystal complex [Ni-7(emmp)(6)(OH)(6)][Ni(emmp)(2)]center dot(CH3CN)(2)center dot(ClO4)(2) (1, Hemmp is 2-ethoxy-6-methyliminom-ethyl-phenol) has been synthesized by microwave-assist solvothermal method. Complex 1 was characterized by IR spectroscopy, elemental analysis, and X-ray single-crystal diffraction. The 1 was consist of a nano-bowl-like heptanuclear cation cluster [Ni-7(emmp)(6)(OH)(6)](2+), two counterion ClO4-, one neutral mononuclear complex [Ni(emmp)(2)] and two acetonitrile molecules. The five part of 1 constructed a whole through M center dot center dot center dot H interaction, O-H center dot center dot center dot N hydrogen bonds and C-H center dot center dot center dot O hydrogen bonds.