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Keywords = octamolybdate

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19 pages, 3765 KiB  
Article
Versatile Polyoxometalates of Different Structural Dimensionalities for Liquid Phase Catalytic Oxidation
by Patrícia Neves, Guilherme Simões, Bogna D. Napruszewska, Katarzyna Pamin, Paweł Serda, Wieslaw Łasocha and Anabela A. Valente
Catalysts 2024, 14(4), 251; https://doi.org/10.3390/catal14040251 - 10 Apr 2024
Cited by 1 | Viewed by 1592
Abstract
Ionic polymolybdate compounds (IPOM) possessing the anions [Mo8O26]4− and [Mo3O10]2−, and cyclohexylammonium (Cy6N) or anilinium (Anil) as organic cations, namely cyclohexylammonium β-octamolybdate dihydrate (1), cyclohexylammonium trimolybdate hydrate (2 [...] Read more.
Ionic polymolybdate compounds (IPOM) possessing the anions [Mo8O26]4− and [Mo3O10]2−, and cyclohexylammonium (Cy6N) or anilinium (Anil) as organic cations, namely cyclohexylammonium β-octamolybdate dihydrate (1), cyclohexylammonium trimolybdate hydrate (2), anilinium β-octamolybdate dihydrate (3), anilinium trimolybdate tetrahydrate (4) and anilinium trimolybdate dihydrate (5), were synthesized via simple, eco-friendly one-pot routes. New crystal structures of 1, 2 and 5 were discovered. IPOM compounds with different structural dimensionality, density and ratio of the number of terminal oxo groups/molybdenum atoms (n(oxo)/Mo) were developed. The IPOM compounds promoted the epoxidation of biobased olefins such as the fatty acid methyl esters methyl oleate and methyl linoleate with tert-butylhydroperoxide as oxidant, leading to conversions of at least 81% at 4 h, 70 °C and the corresponding epoxides. The reaction scope of applications for the IPOM catalysts covered cyclooctane oxidation. Full article
(This article belongs to the Special Issue Exclusive Papers of the Editorial Board Members and Topical Advisory Panel Members of Catalysts in Section "Catalytic Materials")
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15 pages, 4414 KiB  
Article
Proton Affinity in the Chemistry of Beta-Octamolybdate: HPLC-ICP-AES, NMR and Structural Studies
by Victoria V. Volchek, Nikolay B. Kompankov, Maxim N. Sokolov and Pavel A. Abramov
Molecules 2022, 27(23), 8368; https://doi.org/10.3390/molecules27238368 - 30 Nov 2022
Cited by 4 | Viewed by 2007
Abstract
The affinity of [β-Mo8O26]4− toward different proton sources has been studied in various conditions. The proposed sites for proton coordination were highlighted with single crystal X-ray diffraction (SCXRD) analysis of (Bu4N)3[β-{Ag(py-NH2)Mo8 [...] Read more.
The affinity of [β-Mo8O26]4− toward different proton sources has been studied in various conditions. The proposed sites for proton coordination were highlighted with single crystal X-ray diffraction (SCXRD) analysis of (Bu4N)3[β-{Ag(py-NH2)Mo8O26]}] (1) and from analysis of reported structures. Structural rearrangement of [β-Mo8O26]4− as a direct response to protonation was studied in solution with 95Mo NMR and HPLC-ICP-AES techniques. A new type of proton transfer reaction between (Bu4N)4[β-Mo8O26] and (Bu4N)4H2[V10O28] in DMSO results in both polyoxometalates transformation into [V2Mo4O19]4−, which was confirmed by the 95Mo, 51V NMR and HPLC-ICP-AES techniques. The same type of reaction with [H4SiW12O40] in DMSO leads to metal redistribution with formation of [W2Mo4O19]2−. Full article
(This article belongs to the Special Issue Research on Polyoxometalate Materials)
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12 pages, 31960 KiB  
Article
Polyoxomolybdate Layered Crystals Constructed from a Heterocyclic Surfactant: Syntheses, Pseudopolymorphism and Introduction of Metal Cations
by Jun Kobayashi, Keisuke Shimura, Keisuke Mikurube, Saki Otobe, Takashi Matsumoto, Eri Ishikawa, Haruo Naruke and Takeru Ito
Materials 2022, 15(7), 2429; https://doi.org/10.3390/ma15072429 - 25 Mar 2022
Cited by 2 | Viewed by 2184
Abstract
Crystals with layered structures are crucial for the construction of functional materials exhibiting intercalation, ionic conductivity, or emission properties. Polyoxometalate crystals hybridized with surfactant cations have distinct layered packings due to the surfactants which can form lamellar structures. Introducing metal cations into such [...] Read more.
Crystals with layered structures are crucial for the construction of functional materials exhibiting intercalation, ionic conductivity, or emission properties. Polyoxometalate crystals hybridized with surfactant cations have distinct layered packings due to the surfactants which can form lamellar structures. Introducing metal cations into such polyoxometalate-surfactant hybrid crystals is significant for the addition of specific functions. Here, polyoxomolybdate–surfactant hybrid crystals were synthesized as single crystals, and unambiguously characterized by X-ray structure analyses. Octamolybdate ([Mo8O26]4–, Mo8) and heterocyclic surfactant of 1-dodecylpyridinium (C12py) were employed. The hybrid crystals were composed of α-type and β-type Mo8 isomers. Two crystalline phases containing α-type Mo8 were obtained as pseudopolymorphs depending on the crystallization conditions. Crystallization with the presence of rubidium and cesium cations caused the formation of metal cation-introduced hybrid crystals comprising β-Mo8 (C12py-Rb-Mo8 and C12py-Cs-Mo8). The yield of the C12py-Rb-Mo8 hybrid crystal was almost constant within crystallization temperatures of 279–303 K, while that of C12py-Cs-Mo8 decreased over 288 K. This means that the C12py-Mo8 hybrid crystal can capture Rb+ and Cs+ from the solution phase into the solids as the C12py-Rb-Mo8 and C12py-Cs-Mo8 hybrid crystals. The C12py-Mo8 hybrid crystals could be applied to ion-capturing materials for heavy metal cation removal. Full article
(This article belongs to the Special Issue Inorganic Metal-to-Ligand Clusters)
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14 pages, 2849 KiB  
Article
Dimensional Control in Polyoxometalate Crystals Hybridized with Amphiphilic Polymerizable Ionic Liquids
by Toshiyuki Misawa, Jun Kobayashi, Yoshiki Kiyota, Masayuki Watanabe, Seiji Ono, Yosuke Okamura, Shinichi Koguchi, Masashi Higuchi, Yu Nagase and Takeru Ito
Materials 2019, 12(14), 2283; https://doi.org/10.3390/ma12142283 - 16 Jul 2019
Cited by 6 | Viewed by 2895
Abstract
Ionic liquids are an important component for constructing functional materials, and polyxometalate cluster anion is a promising partner for building inorganic–organic hybrid materials comprising ionic liquids. In such hybrid materials, the precise control of the molecular arrangement in the bulk structures is crucial [...] Read more.
Ionic liquids are an important component for constructing functional materials, and polyxometalate cluster anion is a promising partner for building inorganic–organic hybrid materials comprising ionic liquids. In such hybrid materials, the precise control of the molecular arrangement in the bulk structures is crucial for the emergence of characteristic functions, which can be realized by introducing an amphiphilic moiety into the ionic liquids. Here, an amphiphilic polymerizable imidazolium ionic liquid with a methacryloyl group was firstly hybridized with polyoxometalate anions of octamolybdate ([Mo8O26]4−, Mo8) and silicotungstate ([SiW12O40]4−, SiW12) to obtain inorganic–organic hybrid crystals. The polymerizable ionic liquid with a octyl chain (denoted as MAImC8) resulted in the formation of anisotropic molecular arrangements in the bulk crystal structure, which was compared with the hybrid crystals composed from the polymerizable ionic liquid without a long alkyl chain (denoted as MAIm). Rather densely packed isotropic molecular arrangements were observed in the hybrid crystals of MAIm–Mo8 and MAIm–SiW12 due to the lack of the amphiphilic moiety. On the other hand, using the amphiphilic MAImC8 cation gave rise to a honeycomb-like structure with the Mo8 anion and a layered structure with the SiW12 anion, respectively. Full article
(This article belongs to the Special Issue Growth and Design of Inorganic Crystal)
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14 pages, 1622 KiB  
Article
A Comprehensive Study on the Dye Adsorption Behavior of Polyoxometalate-Complex Nano-Hybrids Containing Classic β-Octamolybdate and Biimidazole Units
by Shuang Liang, Yan-Mei Nie, Sang-Hao Li, Jian-Liang Zhou and Jun Yan
Molecules 2019, 24(4), 806; https://doi.org/10.3390/molecules24040806 - 22 Feb 2019
Cited by 11 | Viewed by 4130
Abstract
Six new hybrids based on β-[Mo8O26]4− polyoxometalates, [Ni(H2biim)3]2[β-Mo8O26]•8DMF(1); (DMA)2[M(H2biim)2(H2O)2][β-Mo8O26]•4DMF (M = Ni [...] Read more.
Six new hybrids based on β-[Mo8O26]4− polyoxometalates, [Ni(H2biim)3]2[β-Mo8O26]•8DMF(1); (DMA)2[M(H2biim)2(H2O)2][β-Mo8O26]•4DMF (M = Ni (2), Co (3)), DMA = dimethyl-ammonium, H2biim=2,2′-biimidazole); [M(H2biim)(DMF)3]2[β-Mo8O26]•2DMF (M = Zn (4), Cu (5)); [(DMA)2[Cu(DMF)4][β-Mo8O26]•2DMF]n (6), have been successfully synthesized and characterized. Compounds 2–5 show favorable capacity to adsorb methylene blue (MB) at room temperature, and they can selectively capture MB molecules from binary-mixture solutions of MB/MO (MO = Methyl Orange), or MB/RhB (RhB = Rhodamine B). Compound 3 can uptake up to 521.7 mg g−1 MB cationic dyes rapidly, which perform the maximum adsorption in an hour among the reported materials as far as we know. The compounds are stable and still work very efficiently after three cycles. For compound 3, the preliminary adsorption mechanism studies indicated that the adsorption is an ion exchange process and the adsorption behavior of polyoxometalate-complex can be benefited from additional exchangeable protons in the complex cations. Full article
(This article belongs to the Special Issue Polyoxometalates and Polyoxometalate-Based Systems)
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15 pages, 3293 KiB  
Article
A Robust Framework Based on Polymeric Octamolybdate Anions and Copper(II) Complexes of Tetradentate N-donor Ligands
by Nour Dissem, Beñat Artetxe, Leire San Felices, Luis Lezama, Amor Haddad and Juan M. Gutiérrez-Zorrilla
Crystals 2018, 8(1), 20; https://doi.org/10.3390/cryst8010020 - 6 Jan 2018
Cited by 10 | Viewed by 5261
Abstract
A new organic-inorganic compound based on octamolybdate building blocks and copper(II) complexes of tetradentate N-donor ligands has been hydrothermally synthesized, namely [Cu(cyclam)]2[Mo8O26]·1.5H2O (1), (cyclam: 1,4,8,11–tetraazacyclotetradecane). Compound 1 has been chemically (elemental and thermal [...] Read more.
A new organic-inorganic compound based on octamolybdate building blocks and copper(II) complexes of tetradentate N-donor ligands has been hydrothermally synthesized, namely [Cu(cyclam)]2[Mo8O26]·1.5H2O (1), (cyclam: 1,4,8,11–tetraazacyclotetradecane). Compound 1 has been chemically (elemental and thermal analyses), spectroscopically (infrared spectroscopy), and structurally (single crystal and powder X-ray diffraction) characterized. The crystal packing of 1 shows a covalent framework structure formed by [Mo8O26]n4n− chains running along the 100 direction which are linked to each other through the coordination spheres of {Cu(cyclam)}2+ complexes leading to a three-dimensional open network. This structural assembly generates voids that can be described as a succession of cavities communicated through narrow bottlenecks with approximate cross section of 4 × 7 Å2 where the hydration water molecules are hosted. The robust open structure of 1 remains virtually unaltered upon thermal evacuation of guest solvent molecules at 130 °C, resulting in the anhydrous phase [Cu(cyclam)]2[Mo8O26] (1a) with potentially accessible micropores as demonstrated by single-crystal X-ray diffraction measurements. Electron paramagnetic resonance spectroscopy analysis of 1 has also been assessed. Full article
(This article belongs to the Special Issue Crystal Structure Analysis of Supramolecular and Porous Solids)
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12 pages, 6041 KiB  
Article
An Investigation of Polyoxometalate Hybrid Materials as Patternable Dielectrics and Lithographic Resists
by Brandon Hardie and Mark Roll
Materials 2017, 10(11), 1309; https://doi.org/10.3390/ma10111309 - 15 Nov 2017
Viewed by 4378
Abstract
Polyoxometalate (POM) hybrid materials have shown potential as spin-coatable, patternable dielectric thin-films and components for lithographic resists. In particular, the octamolybdate cluster has been shown to possess good spin-coating properties and the patterning capabilities of hybrid octamolybdate thin-films were explored using a combination [...] Read more.
Polyoxometalate (POM) hybrid materials have shown potential as spin-coatable, patternable dielectric thin-films and components for lithographic resists. In particular, the octamolybdate cluster has been shown to possess good spin-coating properties and the patterning capabilities of hybrid octamolybdate thin-films were explored using a combination of broadband UV and electron beam lithography (EBL) techiniques. Dielectric properties of these films were determined by ellipsometry, and octamolybdate clusters were subsequently investigated as negative resists in various blends for potential uses in next-generation photolithography, where contrast, sensitivity, and line edge roughness characteristics were determined. Preliminary evidence for the suppression of the diffusion of photo-generated acids is presented. Full article
(This article belongs to the Special Issue Polyoxometalate and Nanohybrid Materials)
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11 pages, 2852 KiB  
Article
Conductive Hybrid Crystal Composed from Polyoxomolybdate and Deprotonatable Ionic-Liquid Surfactant
by Jun Kobayashi, Ryosuke Kawahara, Sayaka Uchida, Shinichi Koguchi and Takeru Ito
Int. J. Mol. Sci. 2016, 17(7), 994; https://doi.org/10.3390/ijms17070994 - 23 Jun 2016
Cited by 14 | Viewed by 6867
Abstract
A polyoxomolybdate inorganic-organic hybrid crystal was synthesized with deprotonatable ionic-liquid surfactant. 1-dodecylimidazolium cation was employed for its synthesis. The hybrid crystal contained δ-type octamolybdate (Mo8) isomer, and possessed alternate stacking of Mo8 monolayers and interdigitated surfactant bilayers. The crystal structure [...] Read more.
A polyoxomolybdate inorganic-organic hybrid crystal was synthesized with deprotonatable ionic-liquid surfactant. 1-dodecylimidazolium cation was employed for its synthesis. The hybrid crystal contained δ-type octamolybdate (Mo8) isomer, and possessed alternate stacking of Mo8 monolayers and interdigitated surfactant bilayers. The crystal structure was compared with polyoxomolybdate hybrid crystals comprising 1-dodecyl-3-methylimidazolium surfactant, which preferred β-type Mo8 isomer. The less bulky hydrophilic moiety of the 1-dodecylimidazolium interacted with the δ-Mo8 anion by N–H···O hydrogen bonds, which presumably induced the formation of the δ-Mo8 anion. Anhydrous conductivity of the hybrid crystal was estimated to be 5.5 × 10−6 S·cm−1 at 443 K by alternating current (AC) impedance spectroscopy. Full article
(This article belongs to the Special Issue Ionic Liquids 2016 and Selected Papers from ILMAT III)
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11 pages, 683 KiB  
Article
Structural Variation in Polyoxomolybdate Hybrid Crystals Comprising Ionic-Liquid Surfactants
by Takeru Ito, Keisuke Mikurube, Kimiko Hasegawa, Takashi Matsumoto, Kurato Kosaka, Haruo Naruke and Shinichi Koguchi
Crystals 2014, 4(1), 42-52; https://doi.org/10.3390/cryst4010042 - 4 Mar 2014
Cited by 12 | Viewed by 6861
Abstract
Polyoxomolybdate inorganic-organic hybrid crystals were synthesized with 1-decyl-3-methylimidazolium and 1-dodecyl-3-methylimidazolium as ionic-liquid surfactants. Both hybrid crystals possessed alternate stacking of surfactant layers and octamolybdate (Mo8) monolayers, while the molecular structures of Mo8 were different depending on the surfactants and solvents [...] Read more.
Polyoxomolybdate inorganic-organic hybrid crystals were synthesized with 1-decyl-3-methylimidazolium and 1-dodecyl-3-methylimidazolium as ionic-liquid surfactants. Both hybrid crystals possessed alternate stacking of surfactant layers and octamolybdate (Mo8) monolayers, while the molecular structures of Mo8 were different depending on the surfactants and solvents employed for crystallization. Each Mo8 anion was connected by two sodium cations to form infinite one-dimensional chain. The surfactant chains in these crystals were arranged in a complicatedly bent manner, which will be induced by the weak C–H···O hydrogen bonds between the Mo8 anions and ionic-liquid surfactants. Full article
(This article belongs to the Special Issue Crystal Engineering Involving Weak Bonds)
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7 pages, 480 KiB  
Article
Controllable Layered Structures in Polyoxomolybdate-Surfactant Hybrid Crystals
by Takeru Ito and Toshihiro Yamase
Materials 2010, 3(1), 158-164; https://doi.org/10.3390/ma3010158 - 6 Jan 2010
Cited by 15 | Viewed by 14205
Abstract
Inorganic-organic hybrid crystals containing α-octamolybdate (Mo8) or hexamolybdate (Mo6) were isolated by using hexadecyltrimethylammonium (C16) surfactant. The packing mode of the inorganic layers depended on a difference in the polyoxomolybdate molecular structure. The structure for both crystals [...] Read more.
Inorganic-organic hybrid crystals containing α-octamolybdate (Mo8) or hexamolybdate (Mo6) were isolated by using hexadecyltrimethylammonium (C16) surfactant. The packing mode of the inorganic layers depended on a difference in the polyoxomolybdate molecular structure. The structure for both crystals consisted of alternate stacking of C16 organic bilayers and polyoxomolybdate inorganic layers with a periodicity of 24.4–24.6 Å. However, the C16-Mo8 crystals contained Mo8 monolayers, while the C16-Mo6 crystals contained Mo6 bilayers. These lattice structures for the polyoxometalate/organic hybrid will be designed by the molecular structures of polyoxometalate. Full article
(This article belongs to the Special Issue Inorganic-Organic Hybrid Materials)
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7 pages, 328 KiB  
Article
Efficient Syntheses of [(n-C4H9)4N]4[α-Mo8O26] and [(n-C4H9)4N]2[Mo2O7]
by Shusaku Ikegami and Atsushi Yagasaki
Materials 2009, 2(3), 869-875; https://doi.org/10.3390/ma2030869 - 28 Jul 2009
Cited by 8 | Viewed by 17288
Abstract
Efficient and simple syntheses of [(n-C4H9)4N]4[a-Mo8O26] (I) and [(n-C4H9)4N]2[Mo2O7] (II) from MoO3 and aqueous [(n-C4H9)4N]OH are described. The yield is 72% for I and 73% for II. Full article
(This article belongs to the Special Issue Polyoxometalate Compounds)
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