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Single‐crystalline MgFeBO 4,  Mg 0.5 Co 0.5 FeBO 4 , and CoFeBO 4  have been grown by the flux method. The samples have been characterized by X‐ray spectral analysis, X‐ray diffraction, and X‐ray absorption spectroscopy. The X‐ray absorption near‐edge structure (XANES) and extended X‐ray absorption fine structure (EXAFS) spectra have been measured at the Fe and Co  K ‐edges over a wide temperature range (6.5–300 K). The composition, the charge state, and local environment of both Fe and Co atoms have been determined. The effects of Co substitution for Mg on the local structural distortions have been revealed experimentally and the MO bond anisotropy has been found.

Crystal and local atomic structure of MgFeBO 4 , Mg 0.5 Co 0.5 FeBO 4 and CoFeBO 4 : Effects of Co substitution