Treatment of bis（2-dimethylaminoethyl） ether（BDMAE） with nickel acetate afforded a novel 3D nickel（Ⅱ） complex [Ni（BDMAE）（H2O）3·（CH3COO）2·（H2O）2] under solvothermal conditions. Its crystal structure was characterized by elemental analysis, IR spectrum, PXRD and single-crystal X-ray diffraction analysis. The complex belongs to the orthorhombic system, space group C2221 with a=8.823（2）, b=13.932（3）, c=17.563（4） , V=2158.9（8） 3, Z=4, C（12）H（36）N2NiO（10）, Mr=427.14, Dc=1.314 g/cm3, F（000）=920 and μ=0.944 mm（-1）. Single-crystal X-ray diffraction reveals that the mononuclear nickel（Ⅱ） ion is six-coordinated to one oxygen, two nitrogen atoms of the BDMAE ligand and three oxygen atoms of coordinated water molecules. The complex exhibits a 3D supramolecular structure through a variety of intermolecular and intramolecular hydrogen bonding interactions. In addition, the complex has been investigated for catalytic properties towards the Henry reaction of nitromethane with p-nitrobenzaldehyde, and the results indicated that the 1-p-nitrophenyl-2-nitroethanol product was obtained in excellent yield under optimum conditions with the complex as the catalyst.
