Iron-tungsten compound, preparation

Bis[iV,iV -di(2-pyridyl)-imidazol-2-ylidene]aurate(I) tetrafluoroborates, preparation, 2, 292-293 Bis[iV,iV -di(2-pyridyl-methyl)-imidazol-2-ylidene]aurate(I) tetrafluoroborates, preparation, 2, 292-293 Bis(diselenolate) complexes, dinuclear iron compounds, 6, 242 Bis(dithiolene) compounds, in tungsten carbonyl and isocyanide complexes, 5, 644 Bis(enolato) complexes, with bis-Cp Ti(IV), 4, 589 Bis(enones), in reductive cyclizations, 10, 502 Bis(ethanethiolato) complexes, with bis-Cp Ti(IV), 4, 601 Bis(ethene)iridium complexes, preparation, 7, 328-329 -Bis(fluorenyl)zirconocene dichlorides, preparation,... 

Iron-chromium alloys, free from carbon, may be prepared from chromite by the alumino-thermic method. From a study of the cooling-and freezing-point curves it has been suggested that a compound, Cr Fe, exists, but this is questioned by Janecke, who studied the iron-chromium system by means of fusion curves and by the microscopic study of polished sections of various alloys between the limits 10 Fe 90 Cr and 90 Fe 10 Cr, and came to the conclusion that the system consists of a single eutectic which can form mixed crystals with either component. The eutectic contains 75 per cent, of chromium and melts at 1320° C. The addition of chromium to iron increases the readiness of attack by hydrochloric and sulphuric acids, but towards concentrated nitric acid the alloys are rendered passive. They remain bright in air and in water. The presence of carbon increases the resistance to acids and renders them very hard if carbon-free, they are softer than cast iron. All the alloys up to 80 per cent, chromium are magnetic. Molybdenum, titanium, vanadium, and tungsten improve the mechanical properties and increase the resistance to acids. 

Preparation of Pure Tungsten Trioxlde.—The oxide prepared by any of the above processes is alwaj s impure, the nature of the imj urities depending on the composition of the ore and on the materials employed in the process. If alkali has been used, the presence of sodium, potassium, or calcium tends to give the product a greenish appearance. Iron, manganese, silica, phosphorus, tin, molybdenum, vanadium, and columbium may all be present, and since tungsten is prone to form complex compounds with many of these, the purification of the oxide is not easily accomplished. 

Bis-3,4-(trifluoromethyl)-l,2-diselenete 651 is prepared by refluxing selenium with hexafluoro-2-butyne. It reacts with triphenylphosphine and triphenyl-arsine. Triphenylphosphine selenide was isolated, but no other compounds were identified.Ring-opened complexes with nickel, copper, vanadium, molybdenum (652), tungsten, iron, and cobalt are analogous to complexes of the 1,2-dithiete (527) (Section XXXV.2.C.). 

Vanhoye and coworkers [402] synthesized aldehydes by using the electrogenerated radical anion of iron pentacarbonyl to reduce iodoethane and benzyl bromide in the presence of carbon monoxide. Esters can be prepared catalytically from alkyl halides and alcohols in the presence of iron pentacarbonyl [403]. Yoshida and coworkers reduced mixtures of organic halides and iron pentacarbonyl and then introduced an electrophile to obtain carbonyl compounds [404] and converted alkyl halides into aldehydes by using iron pentacarbonyl as a catalyst [405,406]. Finally, a review by Torii [407] provides references to additional papers that deal with catalytic processes involving complexes of nickel, cobalt, iron, palladium, rhodium, platinum, chromium, molybdenum, tungsten, manganese, rhenium, tin, lead, zinc, mercury, and titanium. 

Various metal-metal single o-bonded complexes have been obtained by the reaction of metal carbonyls with metal-carbon o-bonded porphyrins or by the reaction of metal carbonyl anions and chlorometalloporphyrins (Scheme 14). For example, the reaction of dimanganese carbonyl and methyl indium(III) porphyrin gives manganese pen-tacarbonyl indium porphyrin In(Por)Mn(CO)5. The same compound is isolated when chloroindium porphyrin is allowed to react with the manganese pentacarbonyl monoanion. Various iron, cobalt, tungsten, and molybdenum complexes have been prepared by these two methods. 

Bersch (1901) describes Tessie du Motay s blue as prepared from 10 parts sodium tungstate, 8 parts tin crystals , 5 parts yellow prussiate and 1 part of iron(lll) chloride these are dissolved separately and mixed. The precipitate is washed and exposed to light in thin layers, with the blue colour developing over a period of a few days. According to the discoverer, the pigment consists of a compound of tungsten oxide with a double cyanide of iron and tin . 

As an initial exploratory experiment dodecafluoro n-pentane was chosen as a model compound for P.T.F.E. to simulate part of the perfluorinated molecular chain and allowed to adsorb at 0.13 pPa pressure and ambient temperature on a freshly prepared iron film produced by an evaporation process in situ from an iron wire wrapped around a tungsten filament. The events inside the vacuum chamber were followed with an MS 10 mass spectrometer and (where appropriate) a Pi rani gauge. These experiments suggest that the clean iron acts as a catalyst for the breakdown of the perf1uorinated alkane producing a variety of transiently reactive fragments, such as CF2, that in turn may react with the borosilicate (Pyrex) glass walls of the reaction chamber. 

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