Dataset Information

Fe^III ₄₈ -Containing 96-Tungsto-16-Phosphate: Synthesis, Structure, Magnetism and Electrochemistry.

ABSTRACT: The 48-Fe^III -containing 96-tungsto-16-phosphate, [Fe^III ₄₈ (OH)₇₆ (H₂ O)₁₆ (HP₂ W₁₂ O₄₈ )₈ ]^36- (Fe₄₈ ), has been synthesized and structurally characterized. This polyanion comprises eight equivalent {Fe^III ₆ P₂ W₁₂ } units that are linked in an end-on fashion forming a macrocyclic assembly that contains more iron centers than any other polyoxometalate (POM) known to date. The novel Fe₄₈ was synthesized by a simple one-pot reaction of an {Fe₂₂ } coordination complex with the hexalacunary {P₂ W₁₂ } POM precursor in water. The title polyanion was characterized by single-crystal XRD, FTIR, TGA, magnetic and electrochemical studies.

SUBMITTER: Goura J

PROVIDER: S-EPMC7756653 | biostudies-literature | 2020 Dec

REPOSITORIES: biostudies-literature

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Publications

FeIII 48 -Containing 96-Tungsto-16-Phosphate: Synthesis, Structure, Magnetism and Electrochemistry.

Goura Joydeb J Bassil Bassem S BS Bindra Jasleen K JK Rutkowska Iwona A IA Kulesza Pawel J PJ Dalal Naresh S NS Kortz Ulrich U

Chemistry (Weinheim an der Bergstrasse, Germany) 20201103 68

The 48-FeIII -containing 96-tungsto-16-phosphate, [FeIII 48 (OH)76 (H2 O)16 (HP2 W12 O48 )8 ]36- (Fe48 ), has been synthesized and structurally characterized. This polyanion comprises eight equivalent {FeIII 6 P2 W12 } units that are linked in an end-on fashion forming a macrocyclic assembly that contains more iron centers ...[more]

PMID: 32744748

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Project description:The three complexes [Fe(opo)3], [Cu(opo)2], and [Zn(opo)2] containing the non-innocent anionic ligand opo- (opo- = 9-oxido-phenalenone, Hopo = 9-hydroxyphenalonone) were synthesised from the corresponding acetylacetonates. [Zn(opo)2] was characterised using 1H nuclear magnetic resonance (NMR) spectroscopy, the paramagnetic [Fe(opo)3] and [Cu(opo)2] by electron paramagnetic resonance (EPR) spectroscopy. While the EPR spectra of [Cu(opo)2] and [Cu(acac)2] in dimethylformamide (DMF) solution are very similar, a rather narrow spectrum was observed for [Fe(opo)3] in tetrahydrofuran (THF) solution in contrast to the very broad spectrum of [Fe(acac)3] in THF (Hacac = acetylacetone, 2,4-pentanedione; acac- = acetylacetonate). The narrow, completely isotropic signal of [Fe(opo)3] disagrees with a metal-centred S = 5/2 spin system that is observed in the solid state. We assume spin-delocalisation to the opo ligand in the sense of an opo- to FeIII electron transfer. All compounds show several electrochemical opo-centred reduction waves in the range of -1 to -3 V vs. the ferrocene/ferrocenium couple. However, for CuII and FeIII the very first one-electron reductions are metal-centred. Electronic absorption in the UV to vis range are due to π-π* transitions in the opo core, giving Hopo and [Zn(opo)2] a yellow to orange colour. The structured bands ranging from 400 to 500 for all compounds are assigned to the lowest energy π-π* transitions. They show markedly higher intensities and slight shifts for the CuII (brown) and FeIII (red) complexes and we assume admixing metal contributions (MLCT for CuII, LMCT for FeIII). For both complexes long-wavelength absorptions assignable to d-d transitions were detected. Detailed spectroelectrochemical experiments confirm both the electrochemical and the optical assignments. Hopo and the complexes [Cu(opo)2], [Zn(opo)2], and [Fe(opo)3] show antiproliferative activities against HT-29 (colon cancer) and MCF-7 (breast cancer) cell lines in the range of a few µM, comparable to cisplatin under the same conditions.

Dataset Information

Fe^III ₄₈ -Containing 96-Tungsto-16-Phosphate: Synthesis, Structure, Magnetism and Electrochemistry.

Publications

Fe<sup>III</sup> <sub>48</sub> -Containing 96-Tungsto-16-Phosphate: Synthesis, Structure, Magnetism and Electrochemistry.

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