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In this study, binary (Fe\u2013M) and ternary (Fe\u2013M\u2013M\u2032) metal oxide nanoparticles were synthesized via a polyol method optimized to produce flower-like \u03b3-Fe2O3 (maghemite) structures, with M and M\u2032 representing Zn and\/or Mn. Comprehensive structural and magnetic characterization was conducted to explain the relationship between composition, defect structure, and hyperthermic performance. The analyses revealed that cation substitution induced an Fe-site vacancy, primarily at octahedral positions, leading to local structural distortions, as confirmed by powder X-ray diffraction and pair distribution function analysis. The optimized composition, with Zn\/Mn\/Fe = 0.040:0.182:1, exhibited the highest concentration of vacancies and structural disorder. These vacancies altered the bonding environment, enhancing magnetic interactions at tetrahedral sites while weakening those at the octahedral positions. The resulting multicore nanoflowers (20\u201363 nm; core size 13\u201318 nm) displayed strong heating performance, with intrinsic loss power ranging from 0.34 to 5.77 nHm2 kg\u20131. The optimized sample achieved a temperature increase of 30 \u00b0C within 2 min and a specific absorption rate of 369 W g\u20131. This composition was further coated with citrate (CA) and successfully radiolabeled with 177Lu, achieving a radiolabeling yield of 92.7% and excellent stability, thus forming a robust nanoplatform for combined magnetic hyperthermia and radionuclide therapy. Biological evaluation of the optimized S5 composition revealed selective cytotoxicity toward HeLa and LS174 cells, while toxicity was significantly lower to A549, A375, and normal MRC-5 cells. Citrate coating of S5 nanoparticles (S5@CA) drastically reduced their cytotoxicity across all tested cell lines (IC50 &amp;gt; 200 \u03bcg mL\u20131), confirming their enhanced biocompatibility for therapeutic applications. In HeLa cells subjected to magnetic hyperthermia, the viability decreased to approximately 84% after 30 min and 61% after 60 min of treatment, demonstrating the sustained hyperthermic effect at a controlled working temperature of 48 \u00b0C. These results underscore the effectiveness of cation substitution and vacancy engineering in tailoring the functional properties of maghemite-based nanomaterials for advanced multimodal cancer therapies.<\/jats:p>","DOI":"10.1021\/acsami.5c12439","type":"journal-article","created":{"date-parts":[[2025,8,10]],"date-time":"2025-08-10T13:49:32Z","timestamp":1754833772000},"page":"46836-46849","source":"Crossref","is-referenced-by-count":5,"title":["From Structure to\nFunction: Zn\/Mn-Modified Maghemite\nas an Advanced Nanoplatform for Magnetic Hyperthermia and Radionuclide\nTherapy"],"prefix":"10.1021","volume":"17","author":[{"ORCID":"https:\/\/orcid.org\/0000-0003-2889-4416","authenticated-orcid":true,"given":"Milos\u030c","family":"Ognjanovic\u0301","sequence":"first","affiliation":[{"name":"University of Belgrade , , Mike Petrovic\u0301a Alasa 12-14 , ,","place":["Belgrade, Serbia, 11000"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Marko","family":"Bos\u030ckovic\u0301","sequence":"additional","affiliation":[{"name":"University of Belgrade , , Mike Petrovic\u0301a Alasa 12-14 , ,","place":["Belgrade, Serbia, 11000"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Tatjana","family":"Stanojkovic\u0301","sequence":"additional","affiliation":[{"name":"Institute for Oncology and Radiology of Serbia , Pasterova 14 , ,","place":["Belgrade, Serbia, 11000"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Biljana P.","family":"Dojc\u030cinovic\u0301","sequence":"additional","affiliation":[{"name":"University of Belgrade , , Njegos\u030ceva 12 , ,","place":["Belgrade, Serbia, 11000"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"A. M. Milinda","family":"Abeykoon","sequence":"additional","affiliation":[{"name":"Brookhaven National Laboratory , , , ,","place":["Upton, New York, United States of America, 11973"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Aleksandra","family":"Tomic\u0301","sequence":"additional","affiliation":[{"name":"Institute of Physics, Belgrade , , 118 Pregrevica , ,","place":["Belgrade, Serbia, 11080"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Drina","family":"Jankovic\u0301","sequence":"additional","affiliation":[{"name":"University of Belgrade , , Mike Petrovic\u0301a Alasa 12-14 , ,","place":["Belgrade, Serbia, 11000"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Sanja","family":"Vranjes\u030c-D\u0335uric\u0301","sequence":"additional","affiliation":[{"name":"University of Belgrade , , Mike Petrovic\u0301a Alasa 12-14 , ,","place":["Belgrade, Serbia, 11000"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Emil S.","family":"Bozin","sequence":"additional","affiliation":[{"name":"Institute of Physics, Belgrade , , 118 Pregrevica , ,","place":["Belgrade, Serbia, 11080"]},{"name":"Brookhaven National Laboratory , , , ,","place":["Upton, New York, United States of America, 11973"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-5693-6401","authenticated-orcid":true,"given":"Bratislav V.","family":"Antic\u0301","sequence":"additional","affiliation":[{"name":"University of Belgrade , , Mike Petrovic\u0301a Alasa 12-14 , ,","place":["Belgrade, Serbia, 11000"]}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"316","published-online":{"date-parts":[[2025,8,10]]},"reference":[{"issue":"20","key":"2026093015083405700_cit1","doi-asserted-by":"publisher","first-page":"11614","DOI":"10.1039\/D1CS00427A","article-title":"Magnetic Nanoparticles and Clusters for Magnetic Hyperthermia:\nOptimizing Their Heat Performance and Developing Combinatorial Therapies\nto Tackle Cancer","volume":"50","author":"Gavila\u0301n","year":"2021","journal-title":"Chem. 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