A facile approach, named phase transfer catalyst supported, room temperature biphasic synthesis, has been developed to synthesize a new type of coordination polymers. Compared to the traditional biphasic solvothermal synthesis that was run at high temperature (100-200 °C), the new approach introduced here can be operated under a mild condition (room temperature) with the support of phase transfer catalyst. With the application of this new approach, two copper coordination complexes with 1D metal-organic nanotube and 1D coordination polymer containing large water clusters have been successfully synthesized and characterized. Furthermore, the synthetic approach presented here can be extended to synthesize other coordination polymers, including porous lanthanide-organic frameworks.