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Metal–organic structures have great potential for practical applications in many areas. However, their widespread use is often hindered by time-consuming and expensive synthesis procedures that often involve hazardous solvents and, therefore, generate wastes that need to be remediated and/or recycled. The development of cleaner, safer, and more sustainable synthesis methods is extremely important and is needed in the context of green chemistry. In this work, a facile mechanochemical method involving water-assisted ball milling was used for the synthesis of MOF-303. The obtained MOF-303 exhibited a high specific surface area of 1180 m²/g and showed an excellent CO₂ adsorption capacity of 9.5 mmol/g at 0 °C and under 1 bar.