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This new family of microporous Si\u2010POPs manifests as uniform, microporous, spherical particles with a high specific surface area. Notably, Si\u2010POPs were engineered to possess varying numbers of hydroxyl (\u2212OH) groups by altering the monomer in the synthetic process. Among these materials, the variant with the highest number of hydroxyl groups exhibited ultra\u2010high CO<jats:sub>2<\/jats:sub> adsorption capacity, reaching up to 4.3\u2005mmol\u2009g<jats:sup>\u22121<\/jats:sup> at 273\u2005K and 1.0\u2005bar, which surpasses the performance of most porous polymers. Furthermore, Si\u2010POPs also demonstrated remarkable selectivity adsorption for carbon dioxide over nitrogen (17\u201350, IAST at 273\u2005K and 1.0\u2005bar). 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