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Herein, four In-based OIMHs, (C7H12N2)InCl5(H2O)\u00b7H2O (1), (C7H10N2)InCl3(C3H7NO) (2) and (C7H10N2)2In2Cl6 (3), and [(C7H10N2)InBr4][(C7H10N2)2InBr2] (4), were synthesized via solvent-controlled crystallization using 2-[(methylamino)methyl]pyridine as the organic component. Changing the crystallization solvent modulates ligand protonation, In\u2013N\/O coordination, and In-halide connectivity, giving rise to distinct coordination motifs and intermolecular confinement. Specifically, HCl favors ligand protonation and In\u2013Cl coordination, whereas N,N-dimethylformamide and acetonitrile promote In-ligand coordination. Such solvent-induced structural modulation enables the excited-state relaxation pathways to be tuned without heterometal incorporation. Three chlorides (1-3) exhibit blue prompt emission accompanied by green room-temperature phosphorescence. The bromide (4) displays excitation-independent yellow emission centered at 555 nm under dual excitation channels, together with a second-harmonic generation response. Spectroscopic analyses and theoretical calculations reveal that the emissions are associated with halide-to-organic charge-transfer-related excited states, whose relaxation is governed by local coordination geometry and intermolecular interactions. This work provides an effective solvent-mediated strategy for tuning both prompt and long-lived emissions in OIMHs.<\/jats:p>","DOI":"10.1021\/acs.inorgchem.6c02671","type":"journal-article","created":{"date-parts":[[2026,7,21]],"date-time":"2026-07-21T16:03:42Z","timestamp":1784649822000},"page":"17756-17765","source":"Crossref","is-referenced-by-count":0,"title":["Solvent-Mediated\nStructural Modulation for Excited-State\nRelaxation in In-Based Hybrid Halides"],"prefix":"10.1021","volume":"65","author":[{"given":"Haonan","family":"Wu","sequence":"first","affiliation":[{"name":"University of Science and Technology Beijing , , ,","place":["Beijing, P. R. 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