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Here, we selectively passivate external rhodium (Rh) sites on a zeolite-encapsulated Rh@MEL catalyst using bulky 2,4-dimethylbenzenethiol (DMBT), producing Rh@MEL-DMBT that exposes only micropore-confined single Rh sites within 5.3\u00a0\u00c5 \u00d7\u00a05.4 \u00c5 MEL channels. This eliminates interference from unrestricted surface Rh, enabling unambiguous probing of true shape-selective hydroformylation. Rh@MEL-DMBT delivers exceptional performance for C5\u2013C12 \u00a0\u03b1-olefins, achieving linear-to-branched (l\/b) ratios up to 600, &amp;gt;95% aldehyde chemoselectivity, and significant suppression of isomerization (&amp;lt;5% internal olefins) observed for most substrates within this range. Strikingly, activity and aldehyde selectivity exhibit sinusoidal oscillation with increasing chain length which is directly linked to resonant diffusion of olefins in toluene-filled pores revealed by molecular dynamics simulations. In situ Fourier-transform infrared spectroscopy confirms encaged [HRh(CO)2] and [HRh(CO)] intermediates, while kinetic isotope effect (KIE\u00a0=\u00a01.2) and pressure-dependent kinetics rigorously identify CO insertion as the rate-determining step. These results establish the first experimentally validated molecular mechanism of zeolite-confined single-site Rh hydroformylation and unveil diffusion-controlled chain-length-dependent regioselectivity in confined catalysis.<\/jats:p>","DOI":"10.1093\/nsr\/nwag110","type":"journal-article","created":{"date-parts":[[2026,2,21]],"date-time":"2026-02-21T12:37:57Z","timestamp":1771677477000},"source":"Crossref","is-referenced-by-count":1,"title":["Unmasking true confinement effects: ultrahigh linear selectivity and chain-length oscillatory behavior in zeolite-encapsulated rhodium hydroformylation"],"prefix":"10.1093","volume":"13","author":[{"given":"Tao","family":"Yan","sequence":"first","affiliation":[{"name":"State Key Laboratory of Coal Conversion, Institute of Coal Chemistry, Chinese Academy of Sciences , Taiyuan 030001 ,","place":["China"]},{"name":"National Energy Center for Coal to Clean Fuels, Synfuels China Technology Co., Ltd. , Beijing 101407 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Chemical Sciences, University of Chinese Academy of Sciences , Beijing 100190 ,","place":["China"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Zhiqiang","family":"Liu","sequence":"additional","affiliation":[{"name":"Interdisciplinary Institute of NMR and Molecular Sciences, Key Laboratory of Hubei Province for Coal Conversion and New Carbon Materials, School of Chemistry and Chemical Engineering, Wuhan University of Science and Technology , Wuhan 430081 ,","place":["China"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-7115-6510","authenticated-orcid":false,"given":"Anmin","family":"Zheng","sequence":"additional","affiliation":[{"name":"Interdisciplinary Institute of NMR and Molecular Sciences, Key Laboratory of Hubei Province for Coal Conversion and New Carbon Materials, School of Chemistry and Chemical Engineering, Wuhan University of Science and Technology , Wuhan 430081 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