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Various room-temperature-stable monoorganylpolysulfanides of the form [X][RS  n  ] (X = [PPh 4 ] + , [PNP] + , [NE 4 ] + ; R = Ph,  -Bu, n ≥ 2) were synthesized in a simple and versatile one-step process starting from sodium thiolates and elemental sulfur. The compounds were characterized by X-ray crystal structure analysis, NMR spectroscopy, microelemental analysis, and electrospray mass ionization spectrometry including collision-induced dissociation experiments. While these salts are well-defined species as crystals, they undergo complex equilibria in solution. In one case, compounds ranging from n = 1-8 have been observed in solution. Structural features, dynamics in solution, as well as thermochromic properties of one of the compounds, [PPh 4 ][PhS 2 ], are investigated in detail by temperature- and pressure-dependent X-ray crystal structure analysis. The experimental data are complemented by periodic boundary density functional theory calculations on the crystal structures, as well as energy decomposition analyses.

Synthesis, Spectroscopic, and Structural Characterization of Organyl Disulfanides and a Tetrasulfanide