| Summary: | A three-component reaction between the 1,4-benzenedicarboxylic (terephthalic) acid (H<sub>2</sub>bdc), bis(1,2,4-triazol-1-yl)methane (btrm) and zinc nitrate was studied, and three new coordination polymers were isolated by a careful selection of the reaction conditions. Coordination polymers {[Zn<sub>3</sub>(DMF)(btrm)(bdc)<sub>3</sub>]·nDMF}<sub>∞</sub> and {[Zn<sub>3</sub>(btrm)(bdc)<sub>3</sub>]·nDMF}<sub>∞</sub> containing trinuclear {Zn<sub>3</sub>(bdc)<sub>3</sub>} secondary building units are joined by btrm auxiliary linkers into three-dimensional metal–organic frameworks. The coordination polymer {[Zn(bdc)(btrm)]∙nDMF}<sub>∞</sub> consists of Zn<sup>2+</sup> cations joined by bdc<sup>2−</sup> and btrm linkers into a two-fold interpenetrated network. Upon activation, MOF [Zn<sub>3</sub>(btrm)(bdc)<sub>3</sub>]<sub>∞</sub> demonstrated CO<sub>2</sub>/N<sub>2</sub> adsorption selectivity with an ideal adsorbed solution theory (IAST) factor of 21. All three MOF demonstrated photoluminescence with a maximum near 435–440 nm upon excitation at 330 nm.
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