| 1. |
- Blahut, Jan, et al.
(författare)
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Proton-detected fast-magic-angle spinning NMR of paramagnetic inorganic solids
- 2021
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Ingår i: RSC Advances. - : Royal Society of Chemistry (RSC). - 2046-2069. ; 11:47, s. 29870-29876
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Tidskriftsartikel (refereegranskat)abstract
- Fast (60 kHz) magic angle spinning solid-state NMR allows very sensitive proton detection in highly paramagnetic organometallic powders. We showcase this technique with the complete assignment of H-1 and C-13 resonances in a high-spin Fe(ii) polymerisation catalyst with less than 2 mg of sample at natural abundance.
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| 2. |
- Gahlot, Sweta, et al.
(författare)
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Molecules versus Nanoparticles : Identifying a Reactive Molecular Intermediate in the Synthesis of Ternary Coinage Metal Chalcogenides
- 2020
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Ingår i: Inorganic Chemistry. - : American Chemical Society (ACS). - 0020-1669 .- 1520-510X. ; 59:11, s. 7727-7738
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Tidskriftsartikel (refereegranskat)abstract
- The identification of reactive intermediates during molecule-to-nanoparticle (NP) transformation has great significance in comprehending the mechanism of NP formation and, therefore, optimizing the synthetic conditions and properties of the formed products. We report here the room temperature (RT) synthesis of AgCuSe NPs from the reaction of di-tert-butyl selenide with trifluoroacetates (TFA) of silver(I) and copper(II). The isolation and characterization of a molecular species during the course of this reaction, [Ag2Cu(TFA)(4)((Bu2Se)-Bu-t)(4)] (1), which shows extraordinary reactivity and interesting thermochromic behavior (blue at 0 degrees C and green at RT), confirmed that ternary metal selenide NPs are formed via this intermediate species. Similar reactions with related dialkyl chalcogenide R2E resulted in the isolation of molecular species of similar composition, [Ag2Cu(TFA)(4)(R2E)(4)] [R = Bu-t, E = S (2); R = Me, E = Se (3); R = Me, E = S (4)], which are stable at RT but can be converted to ternary metal chalcogenides at elevated temperature. Density functional theory calculations confirm the kinetic instability of 1 and throw light on its thermochromic properties.
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| 3. |
- Mishra, Shashank, et al.
(författare)
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Asymmetry-Induced Redistribution in Sn(IV)-Ti(IV) Hetero-Bimetallic Alkoxide Precursors and Its Impact on Thin-Film Deposition by Metal-Organic Chemical Vapor Deposition
- 2022
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Ingår i: Crystal Growth & Design. - : American Chemical Society (ACS). - 1528-7483 .- 1528-7505. ; 22:1, s. 54-59
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Tidskriftsartikel (refereegranskat)abstract
- With an aim to enhance the stability and volatility of the heterometallic derivative [SnCl4(mu-OEt)(2)Ti(OEt)(2)(HOEt)(2)] (A), obtained conveniently and quantitatively as a simple adduct formula from the equivalent reaction of commercially available SnCl4 and Ti(OEt)(4) in toluene/ethanol, its modification with 2,2,6,6-tetramethyl-3,5-heptanedione (thdH) is reported. The modified precursor [SnCl4(mu-OEt)(2)Ti(thd)(OEt)(HOEt)] (1), obtained from an equimolar reaction of A and thdH, is stable at room temperature but rearranges on heating into A and [SnCl4(mu-OEt)(2)Ti(thd)(2)] (2), as confirmed by vapor pressure measurements and density functional theory calculations. The heterometallic 2 can be obtained in excellent yield from the reaction of A and thdH in a 1:2 molar ratio and is stable in the solid and solution phase up to 200 degrees C. However, the asymmetric nature of its structure consisting of fragments of titanium beta-diketonate and tin chloride connected by bridging ethoxo groups leads to its breakdown into two homometallic components in the gas phase, leading to the deposition of tin-rich metal oxide films on the substrate.
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