Preparation, characterization, and X-ray structure analysis of diethylenetriammonium tetrathiomolybdate
01 Nov 2003-Journal of Chemical Crystallography (Kluwer Academic Publishers-Plenum Publishers)-Vol. 33, Iss: 11, pp 903-908
TL;DR: In this article, a tetrahedral tetrathiomolybdate anions formed an extended three-dimensional network in the solid state with MoS4−2−Moiety with the organic cation.
Abstract: The interaction of H2S gas with aqueous ammonium heptamolybdate solution in the presence of diethylenetriamine (dien) led to the formation of diethylenetriammonium tetrathiomolybdate crystals. The elemental analyses, UV-Visible, IR, and 1H NMR spectra suggested the presence of organic cation and (MoS4)2− moiety. The 1H NMR revealed the presence of two sets of symmetrical A2X2 multiple patterns. The compound crystallizes in the monoclinic system with space group Pn, a = 7.196(6), b = 7.532(3), c = 11.525(10) A, α = 90°, β = 90.17(3)°, γ = 90°, V = 624.78(8) A3, and Z = 2, wR
1 = 0.0261 and wR
2 = 0.0698. The structure consists of tetrahedral tetrathiomolybdate anions, which form an extended three-dimensional network in the solid state with Mo–S⋅⋅⋅H–N hydrogen bonding with the organic cation.
Citations
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TL;DR: Interestingly, the soft X-ray, low energy M(4,5)-edges had greatest potential chemical sensitivity and using the high-resolution superconducting tunnel junction (STJ) fluorescence detector they appear to be straightforward to measure.
37 citations
TL;DR: In this paper, a single-crystal structure analysis indicates a DETA-carbamate is formed with equimolar CO2 absorption, and the absorption-desorption cycles using microwave heating shows that the system has a relatively stable cycling performance.
Abstract: Conventional amine scrubbing systems for carbon dioxide capture require a large amount of energy to regenerate the absorbent. Theoretically, if CO2-captured product can be separated from the liquid counterpart, and only this product need to be heated for desorption, the energy efficiency for CO2 capture can be improved greatly. In the present work, diethylenetriamine (DETA) dissolved in ethanol, diethylene glycol dimethyl ether, N-methyl-pyrrolidone, or dimethyl carbonate can absorb CO2 to result in liquid–solid phase-change in addition to making the reaction to achieve its stoichiometric maximum. The results show that the different organic solvents have no influence on the formation of precipitate. Single-crystal structure analysis indicates a DETA–carbamate is formed with equimolar CO2 absorption. The absorption–desorption cycles using microwave heating shows that the system has a relatively stable cycling performance.
26 citations
TL;DR: The organic ammonium tetrathiomolybdates N-methylethylenediammonium (N-Me-enH2) (1), N-(3-aminopropyl)propane-1,3-diaminium-tetrathio-bdate (dipnH2)[MoS4] (2), 4-(2-ammonioethyl)piperazin-1-polyamide (PPA)-1-EtNH3) (3), 2,2′-imin
18 citations
TL;DR: In this article, it was shown that the all-sulphur analogue of heptamolybdate [M07S24]6− does not exist in alkaline medium and also cannot be isolated from aqueous acidic medium.
Abstract: The complexes [MoX4]2− (M = Mo; X = O or S) exist as the monomeric tetrahedral species in aqueous alkaline solutions. Acidification of tetraoxomolybdate results in the condensation of the tetrahedral units via a series of polyoxomolybdates leading to the ultimate formation of the trioxide MoO3. Heptamolybdate [Mo7O24]6− is the first major polyanion of the acidification reaction. In contrast, acidification of tetrathiomolybdates leads to the formation of amorphous molybdenum trisulphide via a dinuclear Mo(V) complex. The formation of the dinuclear Mo(V) complex precludes the formation of any higher nuclearity Mo(VI)-S complexes in aqueous solution. Thus it is shown that the all-sulphur analogue of heptamolybdate [M07S24]6− does not exist in alkaline medium and also cannot be isolated from aqueous acidic medium
15 citations
TL;DR: In this paper, the homologous series of organic-inorganic hybrid single crystals (diethylenetriamine-H 2 -MoS 4 -I, triethylenetetramineH 2 −MoS4 -II and 1,4-diazobicyclo-2,2-2-octaneH-NH 4 -NH 4 −III ) were prepared by passing hydrogen sulfide gas in the aqueous solution of ammonium heptamolybdate and their respective amines.
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Book•
01 Jan 1948
TL;DR: Textbook of quantitative inorganic analysis as discussed by the authors, Textbook of qualitative and quantitative analysis of inorganic properties, textbook of quantitatively analytically-inorganic analysis, as discussed by the authors.
Abstract: Textbook of quantitative inorganic analysis , Textbook of quantitative inorganic analysis , مرکز فناوری اطلاعات و اطلاع رسانی کشاورزی
2,103 citations
523 citations
TL;DR: In this article, an investigation has been carried out into the possibility of in situ formation of molybdenum trisulphide (MoS2) within porous anodic films on aluminium, to improve subsequent tribological behavior, by re-anodizing in thiomolybdate electrolyte.
Abstract: An investigation has been carried out into the possibility of in situ formation of MoS2 within porous anodic films on aluminium, to improve subsequent tribological behaviour, by re-anodizing in thiomolybdate electrolyte. Acidification of thiomolybdate was employed to simulate the conditions for formation of the sulphide at the anodic film/electrolyte interface, followed by appropriate vacuum heat treatments to study possible temperature effects on the sulphide due to either friction or Joule heating during anodizing. The products of both acidification and heat treatment, characterized by X-ray powder diffraction and scanning electron microscopy, were compared with those formed by direct thermal decomposition of ammonium tetrathiomolybdate crystals. The precipitate formed by acidification was mainly amorphous molybdenum trisulphide (MoS3), which on heat treatment at 450 and 850°C yielded 3R-MoS2. 3R-MoS2 also formed by the thermal decomposition of thiomolybdate crystals. Thermogravimetric and differential thermal analyses showed that the decomposition of MoS3 to MoS2 occurred in the range 220–370°C and revealed the sequence of reaction steps. The findings suggest that mainly amorphous MoS3 is formed as a consequence of changes in the pH of the film/electrolyte interface during re-anodizing but the product is relatively easily transformed to crystalline MoS2 on moderate heating which may occur during wear processes.
78 citations
TL;DR: The tetrathiomolybdates of ammonium, potassium, cobalt, nickel, copper, and zinc have been studied by X-ray powder diffraction, infrared and diffuse reflectance spectroscopy as discussed by the authors.
25 citations