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However, this same reactivity limits its use for soft hydrogels, as gelation often proceeds faster than precursor mixing, leading to spatially heterogeneous networks. Here, S\u2010nitrosothiols (RSNOs) are introduced as thiol\u2010protecting groups that suppress premature thiol\u2010maleimide coupling and enable homogeneous mixing of polymer precursors prior to on\u2010demand crosslinking. Despite common assumptions about RSNO instability, RSNO\u2010modified 4\u2010arm polyethylene glycol (PEGSNO) is stable in aqueous solution for months at 4\u00b0C protected from light. The nucleophiles sodium ascorbate or sodium thiosulfate (STS) trigger thiol regeneration and controlled crosslinking with maleimide\u2010modified PEG. The resulting hydrogels are homogeneous with Young's moduli tunable across a physiologically relevant range by independently varying nucleophile identity, concentration, or polymer content. In a cell\u2010adhesive system based on maleimide\u2010modified cold water fish skin gelatin, STS\u2010triggered gelation supports 3D cell encapsulation, with cytocompatibility depending on formulation and cell type, while matrix stiffness is tuned through polymer content and STS concentration. This work establishes RSNO chemistry as a previously unexplored strategy for controlled thiol\u2010maleimide crosslinking, enabling reproducible, homogeneous network formation, with potential for dual\u2010function materials coupling network formation with local reactive nitrogen species delivery.<\/jats:p>","DOI":"10.1002\/adma.74627","type":"journal-article","created":{"date-parts":[[2026,8,17]],"date-time":"2026-08-17T09:00:30Z","timestamp":1786957230000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["S\u2010Nitrosothiols as Thiol\u2010Protecting Groups for Controlled Thiol\u2010Maleimide Crosslinking of Homogeneous Soft Hydrogels"],"prefix":"10.1002","volume":"38","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-8298-9179","authenticated-orcid":false,"given":"Julian A.","family":"Serna","sequence":"first","affiliation":[{"name":"Institute of Biological and Chemical Systems\u2010Functional Molecular Systems 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