In this paper, MOF-177 was embedded with Rh for the improvement of NO adsorptive selectivity at room temperature. The results showed that the experimental NO saturated adsorption capacity of MOF-177 was very limited value of 1.35 mLÁg À1 with a negligible selectivity, but the embedded 3 wt % Rh/MOF-177 improved it to 16 mLÁg À1 with higher maximal selectivity of NO to CO 2 (352) and to O 2 (600) under low partial pressure. In the simulated mixture gas, the adsorption capacity of NO atmosphere was about 9-18 times higher than that of O 2 and CO 2 , and the adsorptive selectivity was up to near 18. The reductive Rh particles in MOF-177 were basically nanometer-sized higher dispersion state by great carrier function of MOF-177. The pulse adsorption experiments verified that one reduced Rh 0 adsorbed three NO molecules, indicating that the NO adsorption form in Rh/MOF-177 should be a trinitrogroup (Rh (NO) 3 ) adsorbed species in low pressure. This work firstly illustrated that the MOFs materials embedded with metal particle such as Rh can obviously improve NO adsorption selectivity and also provided a reference way for functionalized modification of MOFs materials to enhance the adsorptive separation performance of pollutant NO in flue gas.