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Herein, a three-dimensional metatungstate-based polyoxometalate photocatalyst [Ni(dmbpy)3]2H2[H2W12O40] (Ni\u2013W12) was synthesized via a solvothermal method using the Keggin-type polyoxoanion [H2W12O40]6\u2013 with \u201celectron sponge\u201d characteristics as the building block, Ni2+ as the metal center, and 4,4\u2032-dimethyl-2,2\u2032-bipyridine (dmbpy) as the organic ligand. Under mild conditions of visible light (\u03bb &amp;gt; 420 nm) irradiation in the absence of additional photosensitizers, Ni\u2013W12 catalyzed the selective oxidation of toluene to benzaldehyde, achieving toluene conversion of 58.3% and benzaldehyde selectivity of 95.5% within 5 h. Ni\u2013W12 exhibits excellent visible-light absorption and separation performance of photogenerated charge carrier, which endows it with high catalytic oxidation capability and outstanding cycling stability in toluene oxidation. The catalytic system is also applicable to the selective oxidation of various toluene derivatives, demonstrating good substrate generality. Mechanistic studies confirm that superoxide anion radicals (\u2022O2\u2013) and photogenerated holes (h+) are the key reactive species.<\/jats:p>","DOI":"10.1021\/acs.inorgchem.6c03356","type":"journal-article","created":{"date-parts":[[2026,9,2]],"date-time":"2026-09-02T02:55:29Z","timestamp":1788317729000},"page":"21179-21187","source":"Crossref","is-referenced-by-count":0,"title":["Heterogeneous\nPhotocatalytic Oxidation of Toluene\nto Benzaldehyde over Nickel Coordinated Metatungstate, [Ni(dmbpy)3]2H2[H2W12O40]"],"prefix":"10.1021","volume":"65","author":[{"ORCID":"https:\/\/orcid.org\/0009-0007-0020-5144","authenticated-orcid":true,"given":"Yiran","family":"Liu","sequence":"first","affiliation":[{"name":"Fudan University , , ,","place":["Shanghai, China, 200438"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Rui","family":"He","sequence":"additional","affiliation":[{"name":"Fudan University , , ,","place":["Shanghai, China, 200438"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jinwen","family":"Zhang","sequence":"additional","affiliation":[{"name":"Fudan University , , ,","place":["Shanghai, China, 200438"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0009-0003-6720-6134","authenticated-orcid":true,"given":"Wenhua","family":"Feng","sequence":"additional","affiliation":[{"name":"Fudan University , , ,","place":["Shanghai, China, 200438"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Hehua","family":"Hui","sequence":"additional","affiliation":[{"name":"Fudan University , , ,","place":["Shanghai, China, 200438"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Yuanhang","family":"Ren","sequence":"additional","affiliation":[{"name":"Fudan University , , ,","place":["Shanghai, China, 200438"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-3015-791X","authenticated-orcid":true,"given":"Xueying","family":"Chen","sequence":"additional","affiliation":[{"name":"Fudan University , , ,","place":["Shanghai, China, 200438"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Bin","family":"Yue","sequence":"additional","affiliation":[{"name":"Fudan University , , ,","place":["Shanghai, China, 200438"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Heyong","family":"He","sequence":"additional","affiliation":[{"name":"Fudan University , , ,","place":["Shanghai, China, 200438"]}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"316","published-online":{"date-parts":[[2026,8,28]]},"reference":[{"key":"2026091408080334700_cit1","doi-asserted-by":"publisher","first-page":"14114","DOI":"10.1021\/acssuschemeng.8b02686","article-title":"Innovative reactive distillation process for the sustainable synthesis\nof natural benzaldehyde","volume":"6","author":"Li","year":"2018","journal-title":"ACS Sustainable Chem.\nEng."},{"key":"2026091408080334700_cit2","doi-asserted-by":"publisher","first-page":"4791","DOI":"10.1021\/acscatal.4c00877","article-title":"Lewis acid sites in (110) facet-exposed BiOBr promote\nC\u2013H activation and selective photocatalytic toluene oxidation","volume":"14","author":"Zhou","year":"2024","journal-title":"ACS Catal."},{"key":"2026091408080334700_cit3","doi-asserted-by":"publisher","first-page":"10767","DOI":"10.1021\/acs.inorgchem.4c01401","article-title":"Preparation of a nanosheeted uranyl\u2013organic\nframework for enhanced photocatalytic oxidation of toluene","volume":"63","author":"Che","year":"2024","journal-title":"Inorg. 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