2026-10-07T22:45:16Z https://api.figshare.com/v2/oai

oai:figshare.com:article/34018419 2026-10-01T14:54:59Z category_25099 category_25135 category_25144 category_25162 category_25231 portal_918 item_type_3 month_year_10_2026

From Molecule to Nanocrystal in Real Time: In-Situ Solid-State NMR Uncovers Divergent Decomposition Mechanisms of Cadmium Chalcogenide Precursors Ran Eitan Abutbul (12656618) Grigore Timco: (12893499) Yuhang Yang (6580181) George F. S. Whitehead (5732672) Richard E. P. Winpenny (5745390) David J. Lewis (1353324) Daniel Lee (18879769) Analytical chemistry not elsewhere classified Transition metal chemistry Inorganic materials (incl. nanomaterials) Structure and dynamics of materials Colloid and surface chemistry Cadmium Sulfide Nanostructures cadmium selenide nanostructures solid-state NMR spectroscopy electron microscopy <p dir="ltr">Nanocrystalline metal chalcogenides are an important class of materials for energy-related applications. A powerful synthetic route to these materials is the single-source precursor (SSP) approach, in which molecular precursors containing metal and chalcogenide sources are thermally decomposed to generate metal chalcogenide nanocrystals. The morphology, quality, and functional properties of the resulting nanomaterials are dictated by the underlying decomposition mechanism. In this study, we performed in situ solid-state NMR (ssNMR) spectroscopy as a method for tracking these transformations in real time. By acquiring time-resolved ¹H, ¹³C, and ¹¹³Cd spectra during controlled heating, ligand mobility, carbon bond evolution, and cadmium coordination are followed. This method provides both structural and kinetic information largely inaccessible through ex situ studies. Applied to two types of SSPs, dicadmium(II) tetrakis(N-benzoyl-N′,N′-diisobutylselenourea) and cadmium ethyl xanthate, the technique resolves fundamentally different decomposition routes: a direct single-step conversion versus a multistage pathway involving transient xanthate and disulfide intermediates followed by ligand rearrangement. These results demonstrate that in situ ssNMR spectroscopy can classify precursor reactivity into mechanistic archetypes, cor-relate ligand dynamics with nanocrystal nucleation, and identify surface-bound species as they emerge. </p> 2026-10-01T14:54:59Z Dataset Dataset 10.48420/34018419.v1 https://figshare.com/articles/dataset/From_Molecule_to_Nanocrystal_in_Real_Time_In-Situ_Solid-State_NMR_Uncovers_Divergent_Decomposition_Mechanisms_of_Cadmium_Chalcogenide_Precursors/34018419 CC BY 4.0