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Inspired by natural nacre and bone, inorganic ionic oligomers and organic molecular chains are employed to achieve multiscale crosslinking assembly, advancing from the ionic\u2010molecular level to nanolines, nanorods, nanofibers, microfibers, and ultimately to nanocomposite films and bulk nanocomposite materials. This process results in a highly integrated organic\u2012inorganic hierarchical ordered structure, imparting exceptional record\u2010breaking ultrahigh toughness (558.90\u00a0\u00b1\u00a034.84\u00a0MJ\u00a0m<jats:sup>\u22123<\/jats:sup>), excellent tensile strength (353.84\u00a0\u00b1\u00a018.77\u00a0MPa), and fracture energy (2.93\u00a0MJ\u00a0m<jats:sup>\u22122<\/jats:sup>) to the nanocomposite films. The resulting bulk nanocomposite exhibits outstanding bending mechanical properties (a maximum bending stress of 207.17\u00a0\u00b1\u00a012.37\u00a0MPa, and a bending energy of 37.62\u00a0\u00b1\u00a07.33\u00a0MJ\u00a0m<jats:sup>\u22123<\/jats:sup> without fracture), exceptional fatigue resistance, and remarkable toughness in extreme environments (e.g., \u2212196 and 200\u00a0\u00b0C). Furthermore, the nanocomposites can undergo hydrothermal\u2010induced recycling and regeneration owing to their noncovalent crosslinking nature. Consequently, these nanocomposites exhibit significant potential for applications in high\u2010performance structural engineering materials. The proposed organic\u2012inorganic multiscale crosslinking assembly tactic based on inorganic ionic oligomers presents a promising approach for the fabrication of ultrahigh\u2010toughness nanocomposites.<\/jats:p>","DOI":"10.1002\/adma.202508572","type":"journal-article","created":{"date-parts":[[2025,7,23]],"date-time":"2025-07-23T08:17:07Z","timestamp":1753258627000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":20,"title":["Organic\u2012Inorganic Multiscale Crosslinking Assembly for Ultrahigh\u2010Toughness Nanocomposites"],"prefix":"10.1002","volume":"37","author":[{"ORCID":"https:\/\/orcid.org\/0009-0003-2576-3389","authenticated-orcid":false,"given":"Yadong","family":"Yu","sequence":"first","affiliation":[{"name":"School of Chemical Engineering and Technology Tianjin University  Tianjin 300072 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