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              <p>Synthesized powders and grown single crystals of nominal compositions Li&lt;sub&gt;6&lt;/sub&gt; Ln(BO&lt;sub&gt;3&lt;/sub&gt;)&lt;sub&gt;3&lt;/sub&gt;:Yb&lt;sup&gt;3+&lt;/sup&gt; (Ln=Y, Gd) were investigated by means of powder and single-crystal X-ray diffraction (XRD), as well as optical near-IR spectroscopy in conjunction with electron paramagnetic resonance (EPR) spectroscopy. The appearance of two distinct zero-phonon lines suggests the existence of two kinds of Yb&lt;sup&gt;3+&lt;/sup&gt; ions in the single crystals. The XRD results exclude the possibility of a phase transition occurring between room and low temperatures. EPR spectra of single crystals show the presence of both isolated ions and pairs of ytterbium ions substituted for Y&lt;sup&gt;3+&lt;/sup&gt;. A strong temperature dependence of the intensity of Yb-Yb pairs resonance lines coincides with temperature dependence of emission peak at 978 nm, confirming a common origin of the defect giving rise to these spectra. Calculated from EPR spectra, the distance between pairs of Yb(3+) is in good agreement with crystallographic ones: R=3.856 Å, R(cryst) =3.849 Å.</p>
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