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Herein, the frustrated packing of hairy nanoparticles (HNs) is applied for the fabrication of gas separation membranes. Poly (propylene glycol) (PPG) is covalently grafted on the surface of the 2.5\u00a0nm microporous coordination nanocages (CNCs) with predefined high grafting densities. By precisely tunning the\n                    <jats:italic>\n                      M\n                      <jats:sub>w<\/jats:sub>\n                    <\/jats:italic>\n                    , the grafted PPG demonstrates enhanced rigidity due to the spatial nanoconfinement from the grafted neighbors, and this imposes the frustrated packing of the polymer fragments\u00a0in the interstitial area among the HNs. The generated extra free volume and extrinsic microporosity can be confirmed from positron annihilation life spectroscopic studies, and it contributes to the interconnection of the intrinsic micropores of CNCs for a gas permeation framework. Meanwhile, the HN unit inherits the mechanical property from the grafted polymers and can be processed into flexible membranes that finally achieve H\n                    <jats:sub>2<\/jats:sub>\n                    \/CO\n                    <jats:sub>2<\/jats:sub>\n                    separation performance above the Robeson upper bound. The work reveals the microscopic mechanism for the control of frustrated packing and moreover, opens new avenues to the feasible fabrication of high\u2010performance gas separation membranes.\n                  <\/jats:p>","DOI":"10.1002\/smll.202509174","type":"journal-article","created":{"date-parts":[[2025,11,26]],"date-time":"2025-11-26T11:43:07Z","timestamp":1764157387000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":1,"title":["Precise Surface Engineering of Hairy Nanoparticles Promoted Packing Frustration for Gas Perm\u2010Selectivity Beyond Empirical Upper Bound"],"prefix":"10.1002","volume":"22","author":[{"given":"Yuyan","family":"Lai","sequence":"first","affiliation":[{"name":"State Key Laboratory of Luminescent Materials and Devices &amp; South China Advanced Institute for Soft Matter Science and Technology Guangdong Basic Research Center of Excellence for Energy and Information Polymer Materials South China University of Technology  Guangzhou 510640 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Yuan","family":"Liu","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Luminescent Materials and Devices &amp; South China Advanced Institute for Soft Matter Science and Technology Guangdong Basic Research Center of Excellence for Energy and Information Polymer Materials South China University of Technology  Guangzhou 510640 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Junsheng","family":"Yang","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Luminescent Materials and Devices &amp; South China Advanced Institute for Soft Matter Science and Technology Guangdong Basic Research Center of Excellence for Energy and Information Polymer Materials South China University of Technology  Guangzhou 510640 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Linkun","family":"Cai","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Luminescent Materials and Devices &amp; South China Advanced Institute for Soft Matter Science and Technology Guangdong Basic Research Center of Excellence for Energy and Information Polymer Materials South China University of Technology  Guangzhou 510640 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Wei","family":"Xu","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Particle Detection and Electronics University of Science and Technology of China  Hefei 230026 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Hongjun","family":"Zhang","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Particle Detection and Electronics University of Science and Technology of China  Hefei 230026 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-2902-8376","authenticated-orcid":false,"given":"Panchao","family":"Yin","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Luminescent Materials and Devices &amp; South China Advanced Institute for Soft Matter Science and Technology Guangdong Basic Research Center of Excellence for Energy and Information Polymer Materials South China University of Technology  Guangzhou 510640 China"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"311","published-online":{"date-parts":[[2025,11,26]]},"reference":[{"key":"e_1_2_8_1_1","doi-asserted-by":"publisher","DOI":"10.1038\/nmat4805"},{"key":"e_1_2_8_2_1","doi-asserted-by":"publisher","DOI":"10.1126\/science.aab0530"},{"key":"e_1_2_8_3_1","doi-asserted-by":"publisher","DOI":"10.1021\/ma501488s"},{"key":"e_1_2_8_4_1","doi-asserted-by":"publisher","DOI":"10.1016\/j.jiec.2021.03.030"},{"key":"e_1_2_8_5_1","doi-asserted-by":"publisher","DOI":"10.1016\/S0079-6700(01)00009-0"},{"key":"e_1_2_8_6_1","doi-asserted-by":"publisher","DOI":"10.1016\/0376-7388(93)80013-N"},{"key":"e_1_2_8_7_1","doi-asserted-by":"publisher","DOI":"10.1016\/j.memsci.2008.04.030"},{"key":"e_1_2_8_8_1","doi-asserted-by":"publisher","DOI":"10.1039\/C9EE01384A"},{"key":"e_1_2_8_9_1","doi-asserted-by":"publisher","DOI":"10.1002\/chem.200400860"},{"key":"e_1_2_8_10_1","doi-asserted-by":"publisher","DOI":"10.1021\/acs.macromol.2c00934"},{"key":"e_1_2_8_11_1","doi-asserted-by":"publisher","DOI":"10.1126\/science.1069580"},{"key":"e_1_2_8_12_1","doi-asserted-by":"publisher","DOI":"10.1021\/acs.nanolett.1c02379"},{"key":"e_1_2_8_13_1","doi-asserted-by":"publisher","DOI":"10.1002\/anie.202424238"},{"key":"e_1_2_8_14_1","doi-asserted-by":"publisher","DOI":"10.1016\/j.molstruc.2004.05.043"},{"key":"e_1_2_8_15_1","doi-asserted-by":"publisher","DOI":"10.1016\/j.ccst.2024.100347"},{"key":"e_1_2_8_16_1","doi-asserted-by":"publisher","DOI":"10.1021\/cr3003888"},{"key":"e_1_2_8_17_1","doi-asserted-by":"crossref","DOI":"10.1126\/sciadv.ads0583","volume":"11","author":"Guan J.","journal-title":"Sci. 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