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Here, we report liquid\u2013air interfacial assembly of polymer\u2010grafted chiral gold nanoparticles into macroscopic two\u2010dimensional superlattice films with long\u2010range positional order and orientational coherence. The orientational coherence, interparticle spacing, and stacking dimensionality can be finely modulated, enabling systematic control over their collective chiroptical response. Combined experimental and simulation studies reveal that orientationally coherent superlattices support a long\u2010wavelength collective chiroptical mode with sign inversion relative to the intrinsic particle circular dichroism. This emergent mode, which is absent in isolated nanoparticles and orientationally disordered assemblies, is attributed to order\u2010dependent collective near\u2010field plasmonic coupling among aligned chiral building blocks and is structurally tunable: increasing orientational coherence enhances its intensity, decreasing interparticle spacing red\u2010shifts its spectral position, and multilayer stacking further amplifies the optical dissymmetry. As a proof\u2011of\u2011concept demonstration, these superlattice films enable reproducible, highly enantioselective surface\u2010enhanced Raman scattering detection of penicillamine enantiomers. This work establishes orientational coherence as a decisive structural parameter for engineering emergent chiroptical activity in chiral plasmonic superlattices, providing a versatile assembly strategy for designing collective optical functionality from chiral building blocks.<\/jats:p>","DOI":"10.1002\/anie.7913188","type":"journal-article","created":{"date-parts":[[2026,9,16]],"date-time":"2026-09-16T03:27:32Z","timestamp":1789529252000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Orientationally Coherent Chiral Nanoparticle Superlattices With Emergent and Tunable Collective Chiroptical Activity"],"prefix":"10.1002","author":[{"given":"Ting","family":"Wang","sequence":"first","affiliation":[{"name":"State Key Laboratory of Porous Materials For Separation and Conversion Department of Chemistry and Shanghai Key Laboratory of Molecular Catalysis and Innovative Materials Fudan University  Shanghai 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