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Herein, we report two isostructural metal\u2212organic frameworks, LIFM-712 and LIFM-713, constructed from fluorido-bridged heptanuclear [Co7F12]2+ clusters and tritopic pyridyl ligands, which feature a pyr topology. Confined BF4\u2212 counteranions synergize with bridging fluorido ligands to generate fluorine-rich pore environments, thus providing abundant C\u2212H\u00b7\u00b7\u00b7F recognition sites for C2H2. LIFM-712 exhibits stronger C2H2 binding (Qst = 35.2 kJ mol\u22121), whereas LIFM-713 balances affinity and specific surface area, achieving a higher C2H2 uptake of 149.8 cm3 g\u22121 at 298 K and 1 bar. For LIFM-713, ideal adsorbed solution theory calculations afford a C2H2\/CO2 selectivity up to 4.5, and breakthrough experiments demonstrate a clear separation with a 35 min g\u22121 separation window at 298 K. For the two Co-MOFs, theoretical simulations and in situ infrared spectra reveal that cooperative interactions between cluster-bound fluorido sites and pore-confined counteranions govern the selective adsorption of C2H2. This work highlights a synergistic fluorine-functionalization strategy for designing efficient adsorbents for challenging gas separations.<\/jats:p>","DOI":"10.1021\/acsami.6c10075","type":"journal-article","created":{"date-parts":[[2026,7,9]],"date-time":"2026-07-09T14:29:26Z","timestamp":1783607366000},"page":"41075-41081","source":"Crossref","is-referenced-by-count":1,"title":["Heptanuclear Fluorido-Bridged Cobalt Metal\u2212Organic Frameworks Containing BF4\u2212 Counteranions for Highly Selective C2H2\/CO2 Separation"],"prefix":"10.1021","volume":"18","author":[{"given":"Zi-Qian","family":"Zhou","sequence":"first","affiliation":[{"name":"Sun Yat-Sen University , , ,","place":["Guangzhou, China, 510006"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Liang","family":"Song","sequence":"additional","affiliation":[{"name":"Sun Yat-Sen University , , ,","place":["Guangzhou, China, 510006"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Xiao-Yan","family":"Zhu","sequence":"additional","affiliation":[{"name":"Sun Yat-Sen University , , ,","place":["Guangzhou, China, 510006"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Ya-Nan","family":"Guo","sequence":"additional","affiliation":[{"name":"Sun Yat-Sen University , , ,","place":["Guangzhou, China, 510006"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Dieter","family":"Fenske","sequence":"additional","affiliation":[{"name":"Sun Yat-Sen University , , ,","place":["Guangzhou, China, 510006"]},{"name":"Karlsruhe Institute of Technology (KIT) , , ,","place":["Eggenstein-Leopoldshafen, Germany, 76344"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Ya-Nan","family":"Fan","sequence":"additional","affiliation":[{"name":"Sun Yat-Sen University , , ,","place":["Guangzhou, China, 510006"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-9483-6033","authenticated-orcid":true,"given":"Ji-Jun","family":"Jiang","sequence":"additional","affiliation":[{"name":"Sun Yat-Sen University , , ,","place":["Guangzhou, China, 510006"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-1845-8987","authenticated-orcid":true,"given":"Cheng-Xia","family":"Chen","sequence":"additional","affiliation":[{"name":"Sun Yat-Sen University , , ,","place":["Guangzhou, China, 510006"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-8378-2479","authenticated-orcid":true,"given":"Zhang-Wen","family":"Wei","sequence":"additional","affiliation":[{"name":"Sun Yat-Sen University , , ,","place":["Guangzhou, China, 510006"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-3604-7858","authenticated-orcid":true,"given":"Cheng-Yong","family":"Su","sequence":"additional","affiliation":[{"name":"Sun Yat-Sen University , , ,","place":["Guangzhou, China, 510006"]}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"316","published-online":{"date-parts":[[2026,7,9]]},"reference":[{"issue":"1","key":"2026080518091654100_cit1","doi-asserted-by":"publisher","first-page":"14085","DOI":"10.1038\/ncomms14085","article-title":"Unravelling exceptional acetylene and carbon dioxide adsorption within a tetra-amide functionalized metal-organic framework","volume":"8","author":"Moreau","year":"2017","journal-title":"Nat. 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