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Herein, we report highly efficient electrostatically driven CO<jats:sub>2<\/jats:sub>\/C<jats:sub>2<\/jats:sub>H<jats:sub>2<\/jats:sub> separation in an ultramicroporous cadmium nitroprusside (<jats:bold>Cd\u2010NP<\/jats:bold>) with compact pore space and complementary electrostatic potential well fitting for CO<jats:sub>2<\/jats:sub>, thus enabling molecular quadrupole moment recognition of CO<jats:sub>2<\/jats:sub> over C<jats:sub>2<\/jats:sub>H<jats:sub>2<\/jats:sub>. This material shows a high CO<jats:sub>2<\/jats:sub>\/C<jats:sub>2<\/jats:sub>H<jats:sub>2<\/jats:sub> uptake ratio of 6.0 as well as remarkable CO<jats:sub>2<\/jats:sub>\/C<jats:sub>2<\/jats:sub>H<jats:sub>2<\/jats:sub> selectivity of 85 under ambient conditions with modest CO<jats:sub>2<\/jats:sub> heat of adsorption. Neutron powder diffraction experiments and molecular simulations revealed that the electrostatic potential compatibility between pore structure and CO<jats:sub>2<\/jats:sub> allows it to be trapped in a head\u2010on orientation towards the Cd center, whereas the diffusion of C<jats:sub>2<\/jats:sub>H<jats:sub>2<\/jats:sub> is electrostatically forbidden. Dynamic breakthrough experiments have validated the separation performance of this compound for CO<jats:sub>2<\/jats:sub>\/C<jats:sub>2<\/jats:sub>H<jats:sub>2<\/jats:sub> separation.<\/jats:p>","DOI":"10.1002\/anie.202100584","type":"journal-article","created":{"date-parts":[[2021,2,3]],"date-time":"2021-02-03T02:53:19Z","timestamp":1612320799000},"page":"9604-9609","update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":133,"title":["Electrostatically Driven Selective Adsorption of Carbon Dioxide over Acetylene in an Ultramicroporous Material"],"prefix":"10.1002","volume":"60","author":[{"given":"Yi","family":"Xie","sequence":"first","affiliation":[{"name":"Department of Chemistry University of Texas at San Antonio  One UTSA Circle San Antonio TX 78249-0698 USA"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Hui","family":"Cui","sequence":"additional","affiliation":[{"name":"Department of Chemistry University of 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