Non-hydrothermal synthesis and structure determination of two new β-octamolybdate (VI) stabilized with dialkylammonium counterions

Sarr, Bougar; Diop, Cheikh A.K.; Melin, Frédéric; Sidibe, Mamadou; Hellwig, Petra; Michaud, François; Maury, F.; Senocq, François; Mbaye, Abdou; Rousselin, Yoann

doi:10.1016/j.molstruc.2018.05.055

Cited by 10 publications

(5 citation statements)

References 35 publications

(39 reference statements)

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“…Above 500 °C, the octamolybdate cluster [Mo 8 O 26 ] 4– starts to collapse. These changes are related to the loss of either the MoO 3 units or the release of O 2 molecules . Hence, due to these disintegration steps, the total weight loss % observed from rt to 700 °C is nearly 55%.…”

Section: Resultsmentioning

confidence: 99%

“…These changes are related to the loss of either the MoO 3 units or the release of O 2 molecules. 47 Hence, due to these disintegration steps, the total weight loss % observed from rt to 700 °C is nearly 55%. C-BMO and U-BMO samples showed comparatively higher stability in the given temperature range, and only 3% weight loss was observed for these samples in the 400−700 °C temperature range.…”

Section: Synthesis Andmentioning

confidence: 98%

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Transformation of a Polyoxometalate Precursor into Carbon Doped Bismuth Molybdate Nanosheets for the Visible Light Photocatalytic Degradation of Aqueous Pollutants

Singh,

Gupta,

Bedi

et al. 2024

ACS Appl. Nano Mater.

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Heterogeneous photocatalysis is a convenient and effective tool for eliminating toxic organic effluents from the textile and pharmaceutical industries. The analogous photocatalytic properties of polyoxometalates (POMs) with metal oxide-based semiconductors make them applicable for photocatalytic wastewater treatment applications. However, the high aqueous solubility and low coverage of the visible solar spectrum limit the wider applicability of traditional POMs as heterogeneous photocatalysts. Herein, we report, for the first time, the hydrothermal transformation of a UV-active polyoxometalate precursor, (C 16 H 36 N) 4 [Mo 8 O 26 ] abbreviated as TBA-Mo8, into a visible light active photocatalytic carbon-doped Bi 2 MoO 6 nanosheets (C-BMO) in the presence of a Bi 3+ salt and studied its catalytic activities toward the degradation of a dye pollutant, malachite green (MG), and a pharmaceutical pollutant, ciprofloxacin (CF). For comparison purposes, an undoped Bi 2 MoO 6 (U-BMO) nanosheet was also prepared under identical conditions starting from an in situ generated POM precursor H 4 [Mo 8 O 26 ]. The successful transformation of TBA-Mo8 and H 4 [Mo 8 O 26 ] into Bi 2 MoO 6 photocatalysts under hydrothermal conditions was confirmed through a series of analytical and spectroscopic techniques, including Fourier transform infrared, Raman, X-ray photoelectron spectroscopy, X-ray diffraction, scanning electron spectroscopy, highresolution transmission electron spectroscopy, and other analyses. The results of the photocatalytic experiments revealed superior catalytic activities of C-BMO compared to U-BMO and the parent cluster TBA-Mo8 under visible light irradiation. C-BMO achieved 70 and 87% degradation of MG and CF under visible light irradiation against the 29 and 35% degradation, respectively, shown by U-BMO. A plausible reason for the higher photocatalytic activity of C-BMO is its better charge separation due to the band gap modification resulting from carbon doping. The detailed pathways of MG and CF degradation have also been proposed based on scavenger studies and ESI-MS analyses of the photocatalytic degradation products. This work, therefore, summarizes how simple polyoxometalate can serve as precursors for developing better and more efficient visible light active photocatalysts under milder experimental procedures.

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Section: Resultsmentioning

confidence: 99%

Section: Synthesis Andmentioning

confidence: 98%

Transformation of a Polyoxometalate Precursor into Carbon Doped Bismuth Molybdate Nanosheets for the Visible Light Photocatalytic Degradation of Aqueous Pollutants

Singh,

Gupta,

Bedi

et al. 2024

ACS Appl. Nano Mater.

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“…Continuing our research on polyoxometalates as organic-inorganic hybrid materials, and more specifically on oxomolybdate complexes [16], we have isolated in the present paper three molybdenum oxalate anionic species with three different ammonium counter cations, dipropylamine, diisopropylamine and Dabco (1,4- O (3) were both obtained from the same reagents (ammonium heptamolybdate tetrahydrate and oxalic acid) and using a similar simple procedure (one pot-synthesis in aqueous phase). All three compounds contain the same binuclear [Mo 2 O 6 (C 2 O 4 ) 2 ] 4− anion.…”

Section: Nowadays Molybdenum Chemistry Remains One Of the Most Excitimentioning

confidence: 99%

One pot-synthesis of the fourth category of dinuclear molybdenum(VI) oxalate series: Structure and study of thermal and redox properties

Sarr

Mbaye

Diop

et al. 2019

Inorganica Chimica Acta

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Three new dinuclear molybdenum(VI) oxalate (Pr 2 NH 2) 4 •[M�0 6 (¼0 4 hl (1), (�r 2 NH;J 4 •[M�0 6 (¼0 4 h] (2) and (HDabco) 4 [Mo 2 0 6 (C 2 0 4 hJ-2H 2 0 (3) compounds, have been prepared by one pot-synthesis at room temperature and characterized by single crystal X-ray diffraction and vibrational spectroscopies. F.ach compound contains the binuclear [Mo 2 0 6 (¼0 4 h] 4-anion where each molybdenum is in an octahedral Mo0 6 environment. ln compound (3), the interconnection between [M0206(C204)2J 4-anions, [HDabco] + cations and water molecules (H20) leads to an infinite inorganic-organic chain structure. Similarly, in compounds (1) and (2) the interactions between [Mo206(C2Ü 4hJ4-anions and respectively [Pr 2NH2l + and [ i Pr�2l + cations leads to an infinite inorganic-organic chain structure. A remarkable difference between the compounds is that in compounds (1) and (2) interactions between the chains involve only Van der Waals forces giving rise to layer-like structures, which also interact between them only by Van der Waals forces, whereas in compound (3) the chains interact also through hydrogen bonds giving a 30 supramolecular structure. The thermal properties of the compounds were investigated through thermogravimetric and differential thermal analyzes. The differences in the thermal decomposition of the compounds in the solid state are discussed in relation with their crystal structure. Cyclic voltammetry shows that the [Mo 2 0 6 (¼0 4 h] 4-anion can be reduced in both aprotic solvent and water.

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“…In this context, the [Mo 7 O 24 ] 6À heptamolybdate anion has been isolated with numerous different counter-cations such as 4-aminopyridinium, Npentylammonium,diethylenetriammonium,N,N,N 0 ,N 0 -tetramethylethylenediammonium, tetramethylammonium, guanidinium, hexanediammonium, butan-1-aminium, ammonium, potassium and sodium (Romá n et al, 1985(Romá n et al, , 1988(Romá n et al, , 1990(Romá n et al, , 1992Don & Weakly, 1981;Gatehouse & Leverett, 1968;Sjö bom & Hedman, 1973;Niu et al, 1996;Himeno et al, 1997;Reinoso et al, 2008;Ftini, 2015;Khandolkar et al, 2016). As a continuation of our work in this area (Sarr et al, 2018), we now describe the synthesis and structure of the title compound (I), which is notable for the incorporation of both protonated [C 4 H 7 N 2 ] + 2-methylimidazolium cations and neutral C 4 H 6 N 2 2-methylimidazole molecules in the crystal.…”

Section: Chemical Contextmentioning

confidence: 99%

Synthesis and crystal structure of a new hybrid organic–inorganic material containing neutral molecules, cations and heptamolybdate anions

et al. 2019

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The title compound, hexakis(2-methyl-1H-imidazol-3-ium) heptamolybdate 2-methyl-1H-imidazole disolvate dihydrate, (C4H7N2)6[Mo7O24]·2C4H6N2·2H2O, was prepared from 2-methylimidazole and ammonium heptamolybdate tetrahydrate in acid solution. The [Mo7O24]6− heptamolybdate cluster anion is accompanied by six protonated (C4H7N2)+ 2-methylimidazolium cations, two neutral C4H6N2 2-methylimidazole molecules and two water molecules of crystallization. The cluster consists of seven distorted MoO6 octahedra sharing edges or vertices. In the crystal, the components are linked by N—H...N, N—H...O, O—H...O, N—H...(O,O) and O—H...(O,O) hydrogen bonds, generating a three-dimensional network. Weak C—H...O interactions consolidate the packing.

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Non-hydrothermal synthesis and structure determination of two new β-octamolybdate (VI) stabilized with dialkylammonium counterions

Abstract: OATAO is an open access repository that collects the work of Toulouse researchers and makes it freely available over the web where possible.

Cited by 10 publications

References 35 publications

Transformation of a Polyoxometalate Precursor into Carbon Doped Bismuth Molybdate Nanosheets for the Visible Light Photocatalytic Degradation of Aqueous Pollutants

Transformation of a Polyoxometalate Precursor into Carbon Doped Bismuth Molybdate Nanosheets for the Visible Light Photocatalytic Degradation of Aqueous Pollutants

One pot-synthesis of the fourth category of dinuclear molybdenum(VI) oxalate series: Structure and study of thermal and redox properties

Synthesis and crystal structure of a new hybrid organic–inorganic material containing neutral molecules, cations and heptamolybdate anions

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