The local electronic structure and coordination environment of L-CoS were analyzed using ex situ XAS characterization (Figure ). As evident from ex situ Co Kedge X-ray absorption near-edge structure (XANES) spectra, the line shape and the rising absorption edge position of L-CoS are close to those of reference CoS2, suggesting a similar local geometry of Co centers coordinated by S atoms. Fourier-transform (FT) extended X-ray absorption fine structure (FT-EXAFS) spectra characterizations were conducted to identify the local coordination environment of Co centers. As shown in Figure , the FT-EXAFS spectrum of L-CoS resembles that of CoS2, namely, only one intense backscattering signal is present within the interval R + ΔR =1 to 3 Å, strongly validating the coordination environment of the first shell Co-S. Reference CoS2 features a second backscattering signal at R + ΔR of 3.55 Å, with the backscattering of the second coordination shell of Co-Co pairs (Figure ), correspondingly. However, this signal vanishes in the FT-EXAFS spectrum of L-CoS, suggesting the lack of long-range ordering in L-CoS. Fitting of FT-EXAFS spectra provides direct evidence of the presence of structural deficiencies in L-CoS. The results (Table ) indicate coordination numbers (CNCo-S) of L-CoS and the CoS2 reference of 5.18 and 6.00, respectively. The slightly lower CNCo-S of L-CoS compared with that of reference CoS2 suggests the absence of S atoms in L-CoS, in agreement with the aforementioned EDX discussion. The results are also evident from the wavelet transform (WT) of EXAFS spectra (Figure ). As expected, L-CoS and reference CoS2 only feature one intensity maximum at the k value of ca. 6.5 Å -1 with a strong negative shift compared with Co foil (ca. 8.0 Å -1 ). This indicates that the observed scattering features in the WT contour plots mainly arise from the Co-S coordination contributions. At the same time, as one can see from Figure , the Co-S scattering of L-CoS displays a weaker signal intensity compared to that of reference CoS2, further supporting the presence of structural deficiencies in L-CoS.