An increasing activity with increasing temperature is observed. At lower reaction temperatures the catalytic performance of [Pd(2pymo)2]n in powder form is low, while at 70 °C however an acetylene conversion of 19.3 % with a low ethane make of 0.010 mol% and a total C4 selectivity of 8.4 % was achieved. An increase of the reaction temperature to 90 °C more than doubled the conversion to 43.8 % and decreased the C4 selectivity down to 4.2 % due to the higher hydrogenation activity. As expected, the ethane make increased to 0.055 mol% due to a decreasing selectivity and over-hydrogenation. Overall, performance data of MOFs for a direct comparison have not been reported yet. A direct comparison with an industrial catalyst shows a similar catalytic performance. A detailed analysis of the catalyst performance and properties (see XPS data in Figure ) shows that a quantity of the Pd 2+ was reduced to Pd 0 during the catalytic testing especially at elevated temperatures. N2 physisorption reveals a decreased specific surface area. XRD analysis shows an amorphous diffractogram and XRF confirms a loss in the ratio of organic building blocks by evaluation of the Compton radiation. In summary, the post-mortem analysis after catalytic testing of the MOF powder shows signs of decomposition in the MOF structure under the applied reaction conditions. Yet, based on the very good initial catalytic performance further research focused on the improvement of the stability. Due to the highly exothermic nature of the acetylene hydrogenation reaction and the known thermal vulnerability of MOFs, the next logical step was the preparation and testing of supported [Pd(2-pymo)2]n /Al2O3 catalysts.