As-synthesized [Zn(Oxac) (Taz)]·(HO), referred to as ZOTW, was prepared from aqueous methanol solutions of Zn(CO)(OH) and two kinds of ligands of 1,2,4-triazole (Taz) and oxalic acid (Oxac) at 453 K for 12 h. The crystal structure was determined by the Rietveld method. As-synthesized ZOTW was pretreated at 383 K and 1 mPa for t h, ZOTW(th). ZOTW(≥3h) showed a type I adsorption isotherm for N at 77 K having a saturation amount (V) of 180 mg/g, but that pretreated shortly showed only 1/10 in V. CO was adsorbed at 303 K in sigmoid on nonporous ZOTW(≤2h) and in Langmuir-type on ZOTW(≥3h) to reach the adsorption amount of 120 mg/g at 700 Torr. N adsorption on ZOTW(≤2h)deCO, degassed after CO adsorption on ZOTW(≤2h), was promoted 5-fold from 180 mg/g on ZOTW(th) and ZOTW(≥3h)deCO up to ca. 1000 mg/g. The interaction of CO and HO molecules in micropores may lead to a new route for micropore formation.
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