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Herein, we propose and demonstrate a hydrogen\u2010bond\u2010directed assembly strategy to regulate the packing density and orientation of\n                    <jats:italic>\u03c0<\/jats:italic>\n                    \u2010conjugated cations in urea derivatives, achieving a synergistic enhancement of optical properties. Four novel urea derivative crystals, CO(NH\n                    <jats:sub>2<\/jats:sub>\n                    )\n                    <jats:sub>2<\/jats:sub>\n                    H\n                    <jats:sub>2<\/jats:sub>\n                    C\n                    <jats:sub>2<\/jats:sub>\n                    O\n                    <jats:sub>2<\/jats:sub>\n                    (UCO), C(OH)(NH\n                    <jats:sub>2<\/jats:sub>\n                    )\n                    <jats:sub>2<\/jats:sub>\n                    NO\n                    <jats:sub>3<\/jats:sub>\n                    (UNO), [C(OH)(NH\n                    <jats:sub>2<\/jats:sub>\n                    )\n                    <jats:sub>2<\/jats:sub>\n                    ]\n                    <jats:sub>2<\/jats:sub>\n                    SiF\n                    <jats:sub>6<\/jats:sub>\n                    (USF\u20101), and [C(OH)(NH\n                    <jats:sub>2<\/jats:sub>\n                    )\n                    <jats:sub>2<\/jats:sub>\n                    ]\n                    <jats:sub>2<\/jats:sub>\n                    CO(NH\n                    <jats:sub>2<\/jats:sub>\n                    )\n                    <jats:sub>2<\/jats:sub>\n                    SiF\n                    <jats:sub>6<\/jats:sub>\n                    (USF\u20102), were synthesized. Among them, UNO exhibits a record\u2010high birefringence of 0.372 at 546\u00a0nm within the urea family, while USF\u20101 and USF\u20102 achieve DUV transparency with cutoff edges below 200\u00a0nm (193 and 195\u00a0nm, respectively). Structural and theoretical analyses reveal that the introduced groups ([H\n                    <jats:sub>2<\/jats:sub>\n                    C\n                    <jats:sub>2<\/jats:sub>\n                    O\n                    <jats:sub>2<\/jats:sub>\n                    ], [NO\n                    <jats:sub>3<\/jats:sub>\n                    ]\n                    <jats:sup>\u2212<\/jats:sup>\n                    , [SiF\n                    <jats:sub>6<\/jats:sub>\n                    ]\n                    <jats:sup>2<\/jats:sup>\n                    <jats:sup>\u2212<\/jats:sup>\n                    ) reconstruct the hydrogen\u2010bonding network, steering the planar [CO(NH\n                    <jats:sub>2<\/jats:sub>\n                    )\n                    <jats:sub>2<\/jats:sub>\n                    ] from the vertical and antiparallel arrangement found in pristine urea into a highly parallel alignment within layered structures. This significantly enhances macroscopic optical anisotropy. This work establishes a hydrogen\u2010bond engineering paradigm for the rational design of high\u2010performance UV\/DUV optical crystals by controlling\n                    <jats:italic>\u03c0<\/jats:italic>\n                    \u2010conjugated unit assembly.\n                  <\/jats:p>","DOI":"10.1002\/smll.73374","type":"journal-article","created":{"date-parts":[[2026,4,14]],"date-time":"2026-04-14T10:50:26Z","timestamp":1776163826000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":3,"title":["Hydrogen\u2010Bond\u2010Directed Assembly of Urea Derivatives: Exceptional Birefringence Achieved by\n                    <i>\u03c0<\/i>\n                    \u2010Conjugated Unit Alignment"],"prefix":"10.1002","volume":"22","author":[{"given":"Peng","family":"Jiang","sequence":"first","affiliation":[{"name":"Research Center for Crystal Materials CAS Key Laboratory of Functional Materials and Devices for Special Environmental Conditions Xinjiang Key Laboratory of Functional Crystal Materials Xinjiang Technical Institute of Physics and Chemistry Chinese Academy of Sciences  Urumqi P. R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Yuqi","family":"Qin","sequence":"additional","affiliation":[{"name":"Research Center for Crystal Materials CAS Key Laboratory of Functional Materials and Devices for Special Environmental Conditions Xinjiang Key Laboratory of Functional Crystal Materials Xinjiang Technical Institute of Physics and Chemistry Chinese Academy of Sciences  Urumqi P. R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Junwei","family":"Feng","sequence":"additional","affiliation":[{"name":"Research Center for Crystal Materials CAS Key Laboratory of Functional Materials and Devices for Special Environmental Conditions Xinjiang Key Laboratory of Functional Crystal Materials Xinjiang Technical Institute of Physics and Chemistry Chinese Academy of Sciences  Urumqi P. R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0009-0009-3418-4913","authenticated-orcid":false,"given":"Minqiang","family":"Gai","sequence":"additional","affiliation":[{"name":"Research Center for Crystal Materials CAS Key Laboratory of Functional Materials and Devices for Special Environmental Conditions Xinjiang Key Laboratory of Functional Crystal Materials Xinjiang Technical Institute of Physics and Chemistry Chinese Academy of Sciences  Urumqi P. R. China"},{"name":"Center of Materials Science and Optoelectronics Engineering University of Chinese Academy of Sciences  Beijing P. R. 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