). Fourier transforms-extended X-ray absorption fine structure (FT-EXAFS) spectra at the Cu K-edge reveal a distinct geometric arrangement in the Cu58-I and Cu58-II NCs, indicating a modified ligand environment compared to the standard sample, a characteristic maintained even after loading onto CB (Figure and Figure ). Notably, the peak observed at approximately ~1.8 Å in the FT-EXAFS is attributed to Cu-P or Cu-S bonding which is present in both NCs. Further analysis through R-space extended X-ray absorption fine structure (EXAFS) corroborates these observations, highlighting differences from the standard sample spectra while retaining their features upon loading (Figure ). Meanwhile we also confirm the size of these NCs are retaining upon loading on the CB surface through the TEM images (Figure ). Electrochemical Performance. The electrochemical performance of all these NCs was thoroughly evaluated across a range of constant voltages (-0.6 to -0.9 V vs. RHE) using CO2saturated 0.1 M KHCO3 aq. as an electrolyte in a gas-flow H-type cell setup. Subsequently, a comprehensive analysis employing gas chromatography (GC) and 1 H NMR was conducted to characterize the gas and liquid products, respectively. Our findings revealed that all these NCs given different products although they have almost similar overall geometrical architecture.