| Crynodeb: | The order of OH groups in the crystal structure of SbC<sub>2</sub>O<sub>4</sub>OH, a potential precursor in the synthesis of ternary oxides, was debated. Neutron diffraction on the deuteride SbC<sub>2</sub>O<sub>4</sub>OD revealed disordered OD groups with half occupation for deuterium atoms on either side of a mirror plane (SbC<sub>2</sub>O<sub>4</sub>OD at <i>T</i> = 298(1) K: <i>Pnma</i>, <i>a</i> = 582.07(3) pm, <i>b</i> = 1128.73(5) pm, <i>c</i> = 631.26(4) pm). O−H stretching frequencies are shifted by a factor of 1.35 from 3390 cm<sup>−1</sup> in the hydride to 2513 cm<sup>−1</sup> in the deuteride as seen in infrared spectra. SbC<sub>2</sub>O<sub>4</sub>OH suffers radiation damage in a synchrotron beam, which leaves a dark amorphous residue. Thermal decomposition at 564 K yields antimony oxide, carbon dioxide, carbon oxide, and water in an endothermic reaction. When using SbC<sub>2</sub>O<sub>4</sub>OH as a precursor in reactions, however, ternary oxides are only formed at much higher temperatures.
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