In situ XRD. In situ XRD was carried out on a Rigaku D/max-2600/PC apparatus equipped with a D/teX Ultra high-speed detector and scintillation counter. The x-ray generator consisted of a Cu rotating anode target with a maximum power of 9 kW. All the tests were operated at 40 mA and 40 kV. In situ XRD patterns were recorded in an Anton Paar XRK-900 cell equipped with a CO/H2/inert gas inlet system.

Temperature-programmed hydrogenation. TPH was conducted in a quartz tube reactor equipped with a mass spectrometer. Typically, 50 mg of the sample was in situ reduced and carburized before the TPH experiment. During the TPH, the temperature was increased from room temperature to 750°C at a rate of 5°C min−1 in a dilute H2 flow (20% H2 in He, 50 ml min−1 in total).

Environmental TEM. Environmental TEM images were recorded in an aberration-corrected FEI Titan ETEM G2 instrument at an acceleration voltage of 300 kV. A well-ground sample was in situ reduced in a H2 flow (10 mbar) at 430°C for 20 hours. After reduction, a syngas feed (H2/CO = 2, 3 mbar) was admitted to pass through the sample at 170°C and kept for 2 hours. The HRTEM was taken in situ during the process above.

Operando Mössbauer spectroscopy. Operando Mössbauer spectroscopy was carried out in a state-of-the-art high-pressure Mössbauer cell (35). Transmission 57Fe Mössbauer spectra were collected at 4.2 K (liquid helium) with a sinusoidal velocity spectrometer using a 57Co(Rh) source. The source and the absorbing samples were kept at the same temperature during the measurements. MossWinn 4.0 software was used for spectra fitting (36). Detailed fitting parameters (tables S2 to S4) and discussion (section S3) are provided in the supplementary materials.

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