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Structural determination of inorganic clusters relies heavily on mass spectrometry because of, in most cases, their poor responsivities toward nuclear magnetic resonance, ultraviolet/visible, and infrared analyses. Nevertheless, mass spectrometry analysis of oligosulfurs (S  n  ), which are unique clusters with copious allotropic forms, usually displays their fragment peaks. Here we report that a polyaromatic capsule acts as a supramolecular matrix for the mass determination of the neutral sulfur clusters. Upon encapsulation, molecular ion peaks derived from the host–guest complexes including cyclic S 6  and S 8  clusters are exclusively detected by common electrospray ionization time-of-flight mass spectrometry analysis. Furthermore, mass spectrometry analysis of a cyclic S 12  cluster, which is in situ prepared from two S 6  clusters within the matrix upon light irradiation, is achieved by the same way. The present matrix can remarkably stabilize the otherwise labile S 6  and S 12  clusters in the polyaromatic shell not only under mass spectrometry conditions but also in an ambient solution state.

Exact mass analysis of sulfur clusters upon encapsulation by a polyaromatic capsular matrix