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The development of porous adsorbents integrating ultrahigh structural stability, excellent separation capability, and moisture resistance represents a desirable yet challenging objective for upgrading natural gas. Unlike conventional synthesis strategies for hydrogen\u2011bonded organic frameworks (HOFs) that utilize strong hydrogen\u2010bonding groups such as carboxylic acid groups and 2,4\u2010diaminotriazine, this study employs aldehyde functionalities to construct a novel HOF (HFPTP\u2010HOF) with exceptional moisture resistance and ultrahigh stability. At 298 K and 1 atm, the material exhibits an IAST selectivity of 18.61 for equimolar CO\n                    <jats:sub>2<\/jats:sub>\n                    \/CH\n                    <jats:sub>4<\/jats:sub>\n                    mixtures, representing the highest values among reported HOF materials. Dynamic breakthrough experiments confirm its ability to produce 99.99% pure CH\n                    <jats:sub>4<\/jats:sub>\n                    . More notably, the HOF adopts a distinctive interlayer stacking structure formed by synergistic interligand multiple C\u2013H\u22efO hydrogen bonding and interdigitation. This interlayer stacking architecture imparts remarkable stability to HFPTP\u2010HOF by encapsulating the hydrogen bonds responsible for framework formation within a hydrophobic barrier, which allows it to retain structural integrity even when immersed in 12\u00a0M hydrochloric acid at 50\u00b0C, 20\u00a0M sodium hydroxide at 100\u00b0C or boiling water for 7 days. To our knowledge, this stability exceeds those of all reported HOFs. In addition, within the HOF's pore channels, aldehyde groups and hydrophobic benzene rings are distributed on opposite sides of the pores. This spatial arrangement effectively prevents water molecule clustering within the pores, enabling HFPTP\u2010HOF to maintain outstanding CO\n                    <jats:sub>2<\/jats:sub>\n                    \/CH\n                    <jats:sub>4<\/jats:sub>\n                    separation performance even under 90% RH. Overall, this work provides new insights into the design and synthesis of HOFs that combine ultrahigh stability with exceptional humidity\u2011resistant separation efficiency.\n                  <\/jats:p>","DOI":"10.1002\/anie.2076718","type":"journal-article","created":{"date-parts":[[2026,9,27]],"date-time":"2026-09-27T16:40:58Z","timestamp":1790527258000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Ultrastable Hydrogen\u2010Bonded Organic Framework for Efficient CO\n                    <sub>2<\/sub>\n                    \/CH\n                    <sub>4<\/sub>\n                    Separation in Humid Environments"],"prefix":"10.1002","author":[{"ORCID":"https:\/\/orcid.org\/0000-0003-4056-1964","authenticated-orcid":false,"given":"Shuai","family":"Zhang","sequence":"first","affiliation":[{"name":"Zhejiang Engineering Laboratory For Green Syntheses and Applications of Fluorine\u2010Containing Specialty 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