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• Membranes containing SNW-1 nanoparticles and Co(acac) 3 were successfully fabricated. • Combined use of SNW-1 and Co(acac) 3 enhanced O 2 permeability and O 2 /N 2 selectivity. • Both solubility and diffision selectivity can be enhanced by Co(acac) 3 and SNW-1. Mixed-matrix membranes containing a porous organic framework (SNW-1 nanoparticles) and a cobalt-based complex (Co(acac) 3) were fabricated using the solution-casting technique for potential applications in O 2 /N 2 separation. The mixed-matrix membranes did not show any appreciable defects. In the following mixture gas permeation testing conducted with a binary mixture composed of 21% O 2 and 79% N 2 at 1 bar feed pressure and 35 °C, the mixed-matrix membranes containing SNW-1 nanoparticles showed an enhanced O 2 permeability, whereas Co(acac) 3 improved the O 2 /N 2 selectivity. Hence, with a combination of both nanoparticles and a Cobalt complex in a polymer matrix, a clear synergistic enhancement in O 2 /N 2 separation properties was reported, in which O 2 permeability and O 2 /N 2 selectivity were escalated by 33% and 18%, respectively. Solubility-diffusivity analysis in the mixed-matrix membranes revealed that SNW-1 and Co(acac) 3 can improve O 2 diffusivity and O 2 solubility, respectively, resulting in an enhancement of both O 2 permeability and O 2 /N 2 selectivity for membranes containing both the nanoparticles and the cobalt complex. Future efforts will be focused on developing asymmetric hollow fiber membranes with thin skin layer comprising both SNW-1 and Co(acac) 3. [ABSTRACT FROM AUTHOR]