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Fe₄(OAc)₁₀[EMIM]₂: Novel Iron-Based Acetate EMIM Ionic Compound.

ABSTRACT: We synthesized and characterized a novel iron(II) aceto EMIM coordination compound, which has a simplified empirical formula Fe₄(OAc)₁₀[EMIM]₂, in two different hydration forms: as anhydrous monoclinic compound and triclinic dihydrate Fe₄(OAc)₁₀[EMIM]₂·2H₂O. The dihydrate compound is isostructural with recently reported Mn₄(OAc)₁₀[EMIM]₂·2H₂O, while the anhydrate is a superstructure of the Mn counterpart, suggesting the existence of solid solutions. Both new Fe compounds contain chains of Fe²⁺ octahedrally coordinated exclusively by acetate groups. The EMIM moieties do not interact directly with the Fe²⁺ and contribute to the structural framework of the compound through van der Waals forces and C-H···O hydrogen bonds with the acetate anions. The compounds have a melting temperature of ∼94 °C; therefore, they can be considered metal-containing ionic liquids. Differential thermal analysis indicates three endothermic transitions associated with melting, structural rearrangement in the molten state at about 157 °C, and finally, thermal decomposition of the Fe₄(OAc)₁₀[EMIM]₂. Thermogravimetric analyses indicate an ∼72 wt % mass loss during the decomposition at 280-325 °C. The Fe₄(OAc)₁₀[EMIM]₂ compounds have higher thermal stability than their Mn counterparts and [EMIM][OAc] but lower compared to iron(II) acetate. Temperature-programmed desorption coupled with mass spectrometry shows that the decomposition pathway of the Fe₄(OAc)₁₀[EMIM]₂ involves four distinct regimes with peak temperatures at 88, 200, 267, and 345 °C. The main species observed in the decomposition of the compound are CH₃, H₂O, N₂, CO, OC-CH₃, OH-CO, H₃C-CO-CH₃, and H₃C-O-CO-CH₃. Variable-temperature infrared vibrational spectroscopy indicates that the phase transition at 160-180 °C is associated with a reorientation of the acetate ions, which may lead to a lower interaction with the [EMIM]⁺ before the decomposition of the Fe₄(OAc)₁₀[EMIM]₂ upon further heating. The Fe₄(OAc)₁₀[EMIM]₂ compounds are porous, plausibly capable of accommodating other types of molecules.

SUBMITTER: Severa G

PROVIDER: S-EPMC8637965 | biostudies-literature |

REPOSITORIES: biostudies-literature

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Project description:Understanding the nature of interactions between nanomaterials, such as commercially ubiquitous hematite (α-Fe2O3) Nanorhombohedra (N-Rhomb) and biological systems is of critical importance for gaining insight into the practical applicability of nanomaterials. Microglia represent the first line of defense in the central nervous system (CNS) during severe injury or disease such as Parkinson's and Alzheimer's disease as illustrative examples. Hence, to analyze the potential cytotoxic effect of nanorhombohedra exposure in the presence of microglia, we have synthesized Rhodamine B (RhB) labeled-α-Fe2O3 N-Rhomb, with lengths of 47 ± 10 nm and widths of 35 ± 8 nm. Internalization of RhB labeled-α-Fe2O3 N-Rhomb by microglia in the mouse brain was observed, and a dose-dependent increase in the cellular iron content as probed by cellular fluorescence was detected in cultured microglia after nanoparticle exposure. The cells maintained clear functional viability, exhibiting little to no cytotoxic effects after 24 and 48 hours at acceptable, physiological concentrations. Importantly, the nanoparticle exposure did not induce microglial cells to produce either tumor necrosis factor alpha (TNFα) or interleukin 1-beta (IL1β), two pro-inflammatory cytokines, nor did exposure induce the production of nitrites and reactive oxygen species (ROS), which are common indicators for the onset of inflammation. Finally, we propose that under the conditions of our experiments, i.e. in the presence of RhB labeled-α-Fe2O3 N-Rhomb maintaining concentrations of up to 100 µg/mL after 48 hours of incubation, the in vitro and in vivo internalization of RhB labeled-α-Fe2O3 N-Rhomb are likely to be clathrin-dependent, which represents a conventional mechanistic uptake route for most cells. Given the crucial role that microglia play in many neurological disorders, understanding the potential cytotoxic effects of these nanostructures is of fundamental importance if they are to be used in a therapeutic setting.

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Fe₄(OAc)₁₀[EMIM]₂: Novel Iron-Based Acetate EMIM Ionic Compound.

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Fe₄(OAc)₁₀[EMIM]₂: Novel Iron-Based Acetate EMIM Ionic Compound.