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This advanced CS technology provides a versatile structural analysis technique applicable to a broad range of guest molecules,\u00a0regardless of polarity, with molecular weights ranging from 300 to 1500. However, the method often fails when analyzing rather low\u2010polarity small molecules (MW 200\u2013300) due to an \u201cunfavorable chemical space,\u201d where the host cavities are too large to facilitate sufficient host\u2013guest interactions. Here we overcome this limitation by establishing a size\u2010compensation strategy based on cage\u2010mediated pair\u2010selective bimolecular recognition. By co\u2010encapsulating a target analyte with a shape\u2010complementary \u201cmodulator\u201d (e.g., phenanthrene), we precisely tailor the cavity environment without the need for chemical modification of the host. This adaptive approach enabled the x\u2010ray structural determination of\u00a024 of 30 low\u2010polarity C15 analytes, predominantly sesquiterpenoids, including absolute configuration determination for selected chiral analytes. This work translates a decades\u2010old molecular recognition phenomenon into a practical approach to crystallographic structure determination of low\u2010polarity sesquiterpenoids.<\/jats:p>","DOI":"10.1002\/anie.4748505","type":"journal-article","created":{"date-parts":[[2026,10,20]],"date-time":"2026-10-20T15:34:48Z","timestamp":1792510488000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Expanding the Chemical Space of Analytes in the 2G Crystalline Sponge Method: Size\u2010Compensation Strategy for the Structural Analysis of Low\u2010Polarity Small Molecules"],"prefix":"10.1002","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-5287-6579","authenticated-orcid":false,"given":"Wei","family":"He","sequence":"first","affiliation":[{"name":"Division of Advanced Molecular Science Institute For Molecular Science (IMS)  Okazaki Aichi 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