Quick and selective synthesis of Li6[α-P2W18O62]·28H2O soluble in various organic solvents

Kato, Chisato; Nishihara, Sadafumi; Tsunashima, Ryo; Tatewaki, Yoko; Okada, Shuji; Ren, Xiao‐Ming; Inoue, Katsuya; Long, De‐Liang; Cronin, Leroy

doi:10.1039/c3dt51120k

Cited by 25 publications

(18 citation statements)

References 20 publications

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“…In the course of our research on the Preyssler anion, we have reported that the ammonium salt of the Keggin anion (NH 4 ) 3 [PW 12 O 40 ] was formed when ammonium metatungstate (NH 4 ) 6 [H 2 W 12 O 40 ] was used as the tungsten source, in spite of a large P/W ratio of 3.0 6. Recently, Nishihara's group reported that the lithium salt of the Dawson anion Li 6 [P 2 W 18 O 62 ] was formed when lithium tungstate (Li 2 WO 4 ) was used as the tungsten source, in spite of a P/W ratio of 4.8 7. These results inspired us to investigate the cation effect in the synthesis of the 30‐tungsto‐5‐phosphate systematically.…”

Section: Introductionsupporting

confidence: 81%

“…–12.54 ppm corresponding to the two equivalent P atoms in the alpha isomer of the Dawson anion was observed, and two small singlets with 1:1 integration ratio at –11.06 and –11.80 ppm corresponding to the two P atoms in the beta isomer of the Dawson anion were observed 7. This result is similar to Nishihara 's result where Li 2 WO 4 was used as tungsten source 7. We also confirmed that the Dawson anion is detected as the only product when Li 2 WO 4 was used as W‐source under our conditions (Figure 4a, no.…”

Section: Resultsmentioning

confidence: 99%

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Cation Effect on Formation of Preyssler‐type 30‐Tungsto‐5‐phosphate: Enhanced Yield of Na‐encapsulated Derivative and Direct Synthesis of Ca‐ and Bi‐Encapsulated Derivatives

Hayashi

Haioka

Takahashi

et al. 2015

Zeitschrift anorg allge chemie

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The effect of cations in a reaction mixture for the preparation of the Preyssler‐Jeannin‐Pope type 30‐tungsto‐5‐phosphate [P5W30O110Na]14– is investigated. Reaction of phosphate and tungstate with a P/W ratio of ca. 3.9 in an acidic aqueous solution without cations selectively leads to the Dawson‐type 18‐tungsto‐2‐phosphate, [P2W18O62]6–. Amongst all the alkali cations, only Na+ allows formation of the Preyssler‐type polyanion [P5W30O110Na]14–, with an encapsulated Na+ ion, and the product yield can be improved by increasing Na+ amount. The presence of Li+ ions instead results in the Dawson‐type polyanion [P2W18O62]6–, whereas K+, Rb+, and Cs+ selectively result in the Keggin‐type polyanion [PW12O40]3–. An improved synthetic procedure for the Na+‐encapsulated Preyssler‐ion leading to a higher isolated yield is presented. Furthermore, addition of Ca2+ and Bi3+ compounds allows formation of the Ca2+‐ and Bi3+‐encapsulated Preyssler‐type polyanions, [P5W30O110Ca]13– and [P5W30O110Bi]12–, respectively. Furthermore, single‐crystal XRD structure of the Bi3+‐encapsulated Preyssler‐type polyanions, [P5W30O110Bi]12–, is presented for the first time.

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Section: Introductionsupporting

confidence: 81%

Section: Resultsmentioning

confidence: 99%

Cation Effect on Formation of Preyssler‐type 30‐Tungsto‐5‐phosphate: Enhanced Yield of Na‐encapsulated Derivative and Direct Synthesis of Ca‐ and Bi‐Encapsulated Derivatives

Hayashi

Haioka

Takahashi

et al. 2015

Zeitschrift anorg allge chemie

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“…[28] This allowso ne to scrutinize the influence of the size effecto ft he PMs on the self-assembly of peptides. We herein chose several PM clusters (PM-n, n = 1-7, Figure1a), such as Na 6 [V 10 O 28 ]( PM-1), [29] Na 9 [PW 9 O 34 ]( PM-2), [30] H 4 [SiW 12 O 40 ]( PM-3), K 6 [P 2 W 18 O 62 ]( PM-4), [31] K 12.5 Na 1.5 [NaP 5 W 30 O 110 ]( PM-5), [32] [33] and (NH 4 ) 42 [Mo 132 O 372 (CH 3 COO) 30 (H 2 O) 72 ]( PM-7). [34] The estimated sizes of these PMs are summarizedi nT able 1 based on their crystal structures (CIF data).…”

Section: Resultsmentioning

confidence: 99%

“…Materials H 4 [SiW 12 O 40 ]( PM-3) was acquired from Aladdin GmbH, Na 6 [V 10 O 28 ] (PM-1), [29] Na 9 [PW 9 O 34 ]( PM-2), [30] K 6 [P 2 W 18 O 62 ]( PM-4), [31] K 12.5 Na 1.5 [NaP 5 W 30 O 110 ]( PM-5), [32] K 28 L i5 [H 7 (P 8 W 48 O 184 )]·92 H 2 O( PM-6), [33] and (NH 4 ) 42 [Mo 132 O 372 (CH 3 COO) 30 (H 2 O) 72 ]( PM-7) [34] were prepared according to reported procedures. Fmoc-Rink amide MBHA (4-methylbenzhydrylamine hydrochloride) resin (0.65 mmol g À1 ) was obtained from Advanced Chem Te ch.…”

Section: Methodsmentioning

confidence: 99%

Engineering the Ionic Self‐Assembly of Polyoxometalates and Facial‐Like Peptides

et al. 2016

Chemistry A European J

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The self-assembly behavior of polyoxometalates (PMs) and facial-like cationic peptides carrying lysine residues were systematically investigated. Circular dichroism and UV/Vis spectra demonstrated that the multivalent electrostatic attractions between polyanionic PMs and short peptides with protonated lysine residues initiated the conformational transition of peptide molecules from random-coil to β-sheet state, and subsequently the co-assembly. TEM and atomic force microscopy (AFM) measurements showed that uniform nanofibers formed with decreasing size of the PMs or increasing the intermolecular forces of the peptides, such as through hydrogen-bonding, hydrophobic, and/or π-π interactions. Additionally, the stability of the nanostructures can be improved by rational suppression of the electrostatic repulsion of the shell peptides covering the surface of the nanostructures. These results provide new insight into understanding the ionic self-assembly of peptides and PMs and controlling their final morphology.

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“…Darker and lighter polyhedra in (B) represent the cap and belt types of tungsten sites, respectively. The Wells-Dawson structure by Kato et al (2013) with refcode RIBFUF is the structure with the lowest R 1 value reported (Kato et al, 2013) and is used in this work as a reference Wells-Dawson structure.…”

Section: Introductionmentioning

confidence: 99%

Exploring Wells-Dawson Clusters Associated With the Small Ribosomal Subunit

2019

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The polyoxometalate P 2 W 18 , the Wells-Dawson cluster, stabilized the ribosome sufficiently for the crystallographers to solve the phase problem and improve the structural resolution. In the following we characterize the interaction of the Wells-Dawson cluster with the ribosome small subunit. There are 14 different P 2 W 18 clusters interacting with the ribosome, and the types of interactions range from one simple residue interaction to complex association of multiple sites including backbone interactions with a Wells-Dawson cluster. Although well-documented that bridging oxygen atoms are the main basic sites on other polyoxometalate interaction with most proteins reported, the W=O groups are the main sites of the Wells-Dawson cluster interacting with the ribosome. Furthermore, the peptide chain backbone on the ribosome host constitutes the main sites that associate with the Wells-Dawson cluster. In this work we investigate the potential of one representative pair of closely-located Wells-Dawson clusters being a genuine Double Wells-Dawson cluster. We found that the Double Wells-Dawson structure on the ribosome is geometrically sound and in line with other Double Wells-Dawson clusters previously observed in the solid state and solution. This information suggests that the Double Wells-Dawson structure on the ribosome is real and contribute to characterization of this particular structure of the ribosome.

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Quick and selective synthesis of Li6[α-P2W18O62]·28H2O soluble in various organic solvents

Abstract: Herein we report the synthesis of α-Dawson type POM, Li6[α-P2W18O62]·28H2O, directly from the use of Li2WO4 as the tungstate source. The salt obtained was soluble not only in water but also in a range of polar and non-polar organic solvents, such as benzene.

Cited by 25 publications

References 20 publications

Cation Effect on Formation of Preyssler‐type 30‐Tungsto‐5‐phosphate: Enhanced Yield of Na‐encapsulated Derivative and Direct Synthesis of Ca‐ and Bi‐Encapsulated Derivatives

Cation Effect on Formation of Preyssler‐type 30‐Tungsto‐5‐phosphate: Enhanced Yield of Na‐encapsulated Derivative and Direct Synthesis of Ca‐ and Bi‐Encapsulated Derivatives

Engineering the Ionic Self‐Assembly of Polyoxometalates and Facial‐Like Peptides

Exploring Wells-Dawson Clusters Associated With the Small Ribosomal Subunit

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