The multiferroic
RFe
3(BO
3)
4 family is characterized by diverse magnetic, magnetoelectric, and magnetoelastic properties, the fundamental aspects of which are essential for modern electronics. The present research, using single-crystal X-ray diffraction (XRD) and Mössbauer spectroscopy (MS) in the
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The multiferroic
RFe
3(BO
3)
4 family is characterized by diverse magnetic, magnetoelectric, and magnetoelastic properties, the fundamental aspects of which are essential for modern electronics. The present research, using single-crystal X-ray diffraction (XRD) and Mössbauer spectroscopy (MS) in the temperature range of 25–500 K, aimed to analyze the influence of local atomic coordination on magnetoelectric properties and exchange and super-exchange interactions in
RFe
3(BO
3)
4. Low-temperature, single-crystal XRD data of the magnetically ordered phase of
RFe
3(BO
3)
4 at 25 K, which were obtained for the first time, were supplemented with data obtained at higher temperatures, making it possible to draw conclusions about the mechanism of the structural dynamics. It was shown that, in structures with
R = Gd, Ho, and Y (low-temperature space group
P3
121), a shift in oxygen atoms (O2, second coordination sphere of
R atoms) was accompanied by rotation of the B2O
3 triangle toward
R atoms at low temperatures, and by different rearrangements in iron chains of two types, in contrast to Nd and Sm iron borates (space group
R32). These rearrangements in the structures of space group
P3
121 affected the exchange and super-exchange paths at low temperatures. The MS results confirm the influence of the distant environment of atoms on the magnetoelectric properties of rare-earth iron borates at low temperatures.
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