We report the formation of á-cyclodextrin (áCD) inclusion compounds with octanethiol (OT), decanethiol (DT) and dodecanethiol (DDT). Elemental Microanalysis, ¹H-NMR solution, Scanning Electronic Microscopy (SEM) and Powder X-ray Diffraction analysis (PXRD) confirm the inclusion process of the alkylthiols in to the á-cyclodextrin molecules. The basic host structure of the products is similar to that of typical channel type structure cyclodextrin inclusion compounds. The guest presents extended linear (zig-zag) conformation. The presence of the -SH groups located in the (001) plane of the á-cyclodextrins-alkylthiol crystal, is evidenced by Energy dispersive X-ray (EDX) analysis. 13C CP-MAS NMR spectra of new á-cyclodextrin host-guest inclusion compounds are described.