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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 C 2 H 2 uptake capacity and preferential adsorption behaviour for C 2 H 2 over CO 2 , 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.