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Typically, the uptake of a single gas by a sorbent decreases with temperature, but the relative affinity for two similar gases does not change. However, in this study, we report a rare example of \u201ccrossover sorption,\u201d in which the uptake capacity and apparent affinity for two similar gases reverse at different temperatures. We synthesized two soft porous coordination polymers (PCPs), [Zn\n                    <jats:sub>2<\/jats:sub>\n                    (L1)(L2)\n                    <jats:sub>2<\/jats:sub>\n                    ]\n                    <jats:sub>\n                      <jats:italic>n<\/jats:italic>\n                    <\/jats:sub>\n                    (PCP\u20101) and [Zn\n                    <jats:sub>2<\/jats:sub>\n                    (L1)(L3)\n                    <jats:sub>2<\/jats:sub>\n                    ]\n                    <jats:sub>\n                      <jats:italic>n<\/jats:italic>\n                    <\/jats:sub>\n                    (PCP\u20102) (L1= 1,4\u2010bis(4\u2010pyridyl)benzene, L2=5\u2010methyl\u20101,3\u2010di(4\u2010carboxyphenyl)benzene, and L3=5\u2010methoxy\u20101,3\u2010di(4\u2010carboxyphenyl)benzene). These PCPs exhibits structural changes upon gas sorption and show the crossover sorption for both C\n                    <jats:sub>2<\/jats:sub>\n                    H\n                    <jats:sub>2<\/jats:sub>\n                    \/CO\n                    <jats:sub>2<\/jats:sub>\n                    and C\n                    <jats:sub>2<\/jats:sub>\n                    H\n                    <jats:sub>6<\/jats:sub>\n                    \/C\n                    <jats:sub>2<\/jats:sub>\n                    H\n                    <jats:sub>4<\/jats:sub>\n                    , in which the apparent affinity reverse with temperature. We used in situ gas\u2010loading single\u2010crystal X\u2010ray diffraction (SCXRD) analysis to reveal the guest inclusion structures of PCP\u20101 for C\n                    <jats:sub>2<\/jats:sub>\n                    H\n                    <jats:sub>2<\/jats:sub>\n                    , CO\n                    <jats:sub>2<\/jats:sub>\n                    , C\n                    <jats:sub>2<\/jats:sub>\n                    H\n                    <jats:sub>6<\/jats:sub>\n                    , and C\n                    <jats:sub>2<\/jats:sub>\n                    H\n                    <jats:sub>4<\/jats:sub>\n                    gases at various temperatures. Interestingly, we observed three\u2010step single\u2010crystal to single\u2010crystal (sc\u2010sc) transformations with the different loading phases under these gases, providing insight into guest binding positions, nature of host\u2013guest or guest\u2010guest interactions, and their phase transformations upon exposure to these gases. Combining with theoretical investigation, we have fully elucidated the crossover sorption in the flexible coordination networks, which involves a reversal of apparent affinity and uptake of similar gases at different temperatures. We discovered that this behaviour can be explained by the delicate balance between guest binding and host\u2013guest and guest\u2010guest interactions.\n                  <\/jats:p>","DOI":"10.1002\/anie.202308438","type":"journal-article","created":{"date-parts":[[2023,8,3]],"date-time":"2023-08-03T05:40:25Z","timestamp":1691041225000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":33,"title":["Crossover Sorption of C\n                    <sub>2<\/sub>\n                    H\n                    <sub>2<\/sub>\n                    \/CO\n                    <sub>2<\/sub>\n                    and C\n                    <sub>2<\/sub>\n                    H\n                    <sub>6<\/sub>\n                    \/C\n                    <sub>2<\/sub>\n                    H\n                    <sub>4<\/sub>\n                    in Soft Porous Coordination Networks"],"prefix":"10.1002","volume":"62","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-8933-305X","authenticated-orcid":false,"given":"Mohana","family":"Shivanna","sequence":"first","affiliation":[{"name":"Institute for Integrated Cell-Material Sciences Kyoto University Institute for Advanced Study Kyoto University Yoshida Ushinomiya-cho, Sakyo-ku  Kyoto 606-8501 Japan"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-7904-5003","authenticated-orcid":false,"given":"Ken\u2010ichi","family":"Otake","sequence":"additional","affiliation":[{"name":"Institute for Integrated Cell-Material Sciences Kyoto University Institute for Advanced Study Kyoto University Yoshida Ushinomiya-cho, Sakyo-ku  Kyoto 606-8501 Japan"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-7853-1619","authenticated-orcid":false,"given":"Shotaro","family":"Hiraide","sequence":"additional","affiliation":[{"name":"Department of Chemical Engineering Kyoto University Nishikyo  Kyoto 615-8510 Japan"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Takao","family":"Fujikawa","sequence":"additional","affiliation":[{"name":"Institute for Integrated Cell-Material Sciences Kyoto University Institute for Advanced Study Kyoto University Yoshida Ushinomiya-cho, Sakyo-ku  Kyoto 606-8501 Japan"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-8464-7092","authenticated-orcid":false,"given":"Ping","family":"Wang","sequence":"additional","affiliation":[{"name":"Institute for Integrated Cell-Material Sciences Kyoto University Institute for Advanced Study Kyoto University Yoshida Ushinomiya-cho, Sakyo-ku  Kyoto 606-8501 Japan"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-7648-306X","authenticated-orcid":false,"given":"Yifan","family":"Gu","sequence":"additional","affiliation":[{"name":"Institute for Integrated Cell-Material Sciences Kyoto University Institute for Advanced Study Kyoto University Yoshida Ushinomiya-cho, Sakyo-ku  Kyoto 606-8501 Japan"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Hirotaka","family":"Ashitani","sequence":"additional","affiliation":[{"name":"Department of Physical Science Graduate School of Science Osaka Prefecture, University  Sakai Osaka 599-8531 Japan"},{"name":"Japan Synchrotron Radiation Research Institute (JASRI)  SPring-8, 1\u20131-1 Kouto Sayo-cho, Sayo-gun Hyogo 679-5198 Japan"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-8498-0936","authenticated-orcid":false,"given":"Shogo","family":"Kawaguchi","sequence":"additional","affiliation":[{"name":"Japan Synchrotron Radiation Research Institute (JASRI)  SPring-8, 1\u20131-1 Kouto Sayo-cho, Sayo-gun Hyogo 679-5198 Japan"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-1365-1577","authenticated-orcid":false,"given":"Yoshiki","family":"Kubota","sequence":"additional","affiliation":[{"name":"Department of Physical Science Graduate School of Science Osaka Prefecture, University  Sakai Osaka 599-8531 Japan"},{"name":"Department of Physics Graduate School of Science Osaka Metropolitan University  Sakai Osaka 599-8531 Japan"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-8883-5851","authenticated-orcid":false,"given":"Minoru T.","family":"Miyahara","sequence":"additional","affiliation":[{"name":"Department of Chemical Engineering Kyoto University Nishikyo  Kyoto 615-8510 Japan"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-6956-9543","authenticated-orcid":false,"given":"Susumu","family":"Kitagawa","sequence":"additional","affiliation":[{"name":"Institute for 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