The development of materials for CO₂ capture with high selectivity and high tolerance to H₂S is of prime importance for various industrially relevant gas streams (e.g. natural gas and biogas upgrading as well as pre-combustion capture). Here, we report the successful fabrication of a MOF with combined exceptional CO₂ capture properties and H₂S tolerance, namely the NiSIFSIX-based MOF using both solvothermal and solvent-free methodologies.