| Summary: | The title compound, [dicyclohexyl(sulfanylidene)-λ<sup>5</sup>-phosphanyl]methanol, Cy<sub>2</sub>P(=S)CH<sub>2</sub>OH (<b>1</b>), was obtained from the reaction between [Cy<sub>2</sub>P(CH<sub>2</sub>OH)<sub>2</sub>]Cl with one molar equivalent of NaOH and an excess of elemental sulfur (powdered). Characterization was by a single-crystal X-ray structure determination as well as IR, and 1D-NMR (<sup>1</sup>H, <sup>13</sup>C{<sup>1</sup>H}, <sup>31</sup>P{<sup>1</sup>H}), and 2D-NMR (DEPT-135 and HSQC) spectroscopy, ESI mass spectrometry, and elemental analysis. X-ray crystallography on Compound <b>1</b> shows the phosphorus atom to be tetrahedrally coordinated within a non-symmetric C<sub>3</sub>S donor set but with relatively minor distortions from the ideal geometry. In the molecular packing, hydroxyl-O−H⋯S(thione) hydrogen bonds led to supramolecular helical chains along the <i>b</i>-axis direction.
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