present the synthesis of four new chiral monomers and polymers based on menthol. Their chemical structures, phase behavior, and thermal stability are characterized by FT-IR, NMR, DSC, POM, XRD, and TGA. By inserting a flexible spacer between the mesogenic core and the terminal menthyl groups, the target monomers and polymers can form the SmC*, cholesteric, and SmA phases. By increasing the mesogenic core rigidity, the corresponding T m , T g , and T i increased. In addition, increasing the spacer length decreased the T m and T g , while T i increased. POLYMER NANOSPHERES Polyacetylenes are formed upon irradiation with gamma rays of ortho-substituted aryl alkynes 2-RC 6 H 4 CBCH (R = CF 3 , OMe, Me) in methanol solutions. An osmosis driven manipulation allows the soluble polymers to aggregate in the form of nanospheres, as well as hollow nanospheres, of different dimensions. The finding and development of this transition metal-free activation process of terminal alkynes come from the collaboration of three research groups with authors Mauro Bassetti, Ilaria Fratoddi, Laura Lilla, Chiara Pasquini, Maria Vittoria Russo, and Ornella Ursini, as presented on page 5097. The SEM image in the picture highlights the shape and size of the nanoparticles obtained via the osmosis-based methodology for one of these polymers (R = CF 3).