Then, a pairs of chiral macrocyclic POP, denoted as PRBT and PSBT, were successfully obtained via Yamamoto polymerization of RBT-Br and SBT-Br. The Fourier Transform infrared (FT-IR) spectra of the chiral POP obtained had directly indicated the disappearance of the band at 1064 cm -1 (Figure and S14), which corresponded to the asymmetric stretching vibration of C-Br bond. 13 C CP-MAS NMR spectra spectra of PRBT and PSBT were also similar with that of RBT-H and SBT-H (Figure ), indicating their similar structure. Scanning electronic microscopy (SEM) results verified the sphere-like morphology for these chiral POPs (Figure ), whereas X-ray diffraction curves directly supported their amorphous nature (Figure ). Energy dispersive spectrometer (EDS) analysis of these POP samples suggested their compositions (Figure -S18, Table -S3), whereas no residual Ni had been recorded. Thermogravimetric analysis (TGA) further indicated their high thermal stability with decomposition temperature up to 420 o C (Figure ).