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Starting with a simple mixing of Li\/Nb ethoxides, water addition is used to promote condensation after ligand exchange with different co\u2010solvents including alcohols and glycols of variable carbon\u2010chain length. A nonclassical nucleation scheme is first demonstrated after the identification of new octanuclear complexes with a {Li<jats:sub>4<\/jats:sub>Nb<jats:sub>4<\/jats:sub>O<jats:sub>10<\/jats:sub>} core whose solvophobic interactions mediate their aggregation, thus, resulting in a colloidal gel at room\u2010temperature. Upon heating, a more or less frustrated aggregation\u2010mediated crystallization process is then evidenced leading to LiNbO<jats:sub>3<\/jats:sub> nanocrystals of adjustable mean size between 20 and 100\u00a0nm. Such a fine control can be attributed to the variable Nb\u2212OR (R = alkoxy\/glycoxy ligand) binding interactions at the surface of crystalline intermediates. Demonstration of such a nonclassical nucleation process and crystallization mechanism for LiNbO<jats:sub>3<\/jats:sub> not only sheds light on the entire growth process of multifunctional nanomaterials with non\u2010perovskite crystalline structures, but also opens new avenues for the identification of novel bimetallic oxoclusters involved in the formation of several mixed oxides from the aqueous alkoxide route.<\/jats:p>","DOI":"10.1002\/smll.202306417","type":"journal-article","created":{"date-parts":[[2023,11,16]],"date-time":"2023-11-16T04:00:51Z","timestamp":1700107251000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":9,"title":["Nonclassical Nucleation and Crystallization of LiNbO<sub>3<\/sub> Nanoparticles from the Aqueous Solvothermal Alkoxide 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