Cu(NO3)2•3H2O was reacted with a tetrahedral ligand (AdDB) at 105 °C in a 0.5:1 molar ratio in a chloroform/dimethylformamide (DMF) solution (1:3 v/v) for two days. This solvothermal reaction resulted in the formation of a green solid at the bottom of the glass pressure tube. The solid can be collected in high yield (>90%) by decanting the colorless reaction solution and washing with common organic solvents.