Implementing the dual-ligand strategy, a microporous Zn-based MOF 1 with nitro and amino groups was effectively produced. The activated interconnected pores of 1 exhibited high C₂H₂ uptake capacity and preferential adsorption behaviour for C₂H₂ over CO₂, as identified by the experiments and simulations. This work provides a new approach for designing and synthesizing the MOFs with desired structures and properties by optimizing their pore environment via the dual-ligand strategy.