The Preparation and Reactions of Some Tungsten(II) and Tungsten (IV) Halides

McCarley, Robert E.; Brown, Theodore M.

doi:10.1021/ic50019a007

Cited by 89 publications

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“…[8] The synthesis of metal-rich tungsten chlorides is usually performed following the reduction of WCl 6 with electropositive metals; the reduction with aluminium is well-established. [9] Recently, the reduction of WCl 6 with the metal bis- [11] At present, we are exploring the reduction of WCl 6 by using soft reducing agents and moderate heating temperatures (this temperature region is not often used) in order to explore the potentially largest field of missing compoundsthe thermally labile cluster compounds. [12] Over the course of systematic investigations with the employment of phosphorus as a reducing agent, we here present the novel cluster compounds W 6 PCl 17 and W 4 (PCl)Cl 10 , which represent the first examples of phosphorus-containing tungsten halide clusters.…”

Section: Introductionmentioning

confidence: 99%

Phosphorus‐Centered and Phosphinidene‐Capped Tungsten Chloride Clusters

2011

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Keywords: Tungsten / Cluster compounds / Solid-state structures / X-ray diffraction Black crystalline powders of W 6 PCl 17 and W 4 (PCl)Cl 10 were obtained after reducing WCl 6 with red phosphorus at 370 and 500°C. The crystal structures were determined by single-crystal and powder X-ray diffraction analyses. The structure of W 6 PCl 17 is represented by a phosphorus-centered hexanuclear tungsten cluster, whose (W 6 PCl 11 )Cl 4 a Cl 4/2 a-a chains form a hexagonal stick packing structure. The struc-

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Section: Introductionmentioning

confidence: 99%

Phosphorus‐Centered and Phosphinidene‐Capped Tungsten Chloride Clusters

2011

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“…However, WCI, prepared by the method of McCarley and Brown (18) failed to react with our donors. Like NbCl, and TaCl,, WCl, appears to contain a much stronger metal-metal bond (5).…”

Section: Mc14(g) + 2l(g) = Mc142l(g)mentioning

confidence: 80%

Enthalpies of reaction of zirconium and molybdenum tetrachlorides with pyridine, tetrahydrofuran, and tetrahydrothiophene

Westland¹,

Uzelac²

1970

Can. J. Chem.

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“…A more recent report indicates that heating of this mixed product under vacuum can yield pure WBr 5 [14]. A low-yield (*10 %) synthesis of WBr 4 has been reported from the high-temperature reduction of WBr 5 using W [15] or Al [2] in a uniform temperature gradient. McCarley and Brown [15] have reported the synthesis of WBr 3 using WBr 2 and Br 2 heated in a sealed tube at 50°C for 2 weeks.…”

Section: Introductionmentioning

confidence: 95%

“…Further reduction of WCl 4 to tungsten(II), in the form of the cluster compound (W 6 Cl 8 )Cl 4 , is possible via solidstate disproportionation of WCl 4 [2] or via direct reduction of WCl 6 using Al [3,4]. The majority of these reductions involve tube furnace reactions where high pressures and temperatures are used.…”

Section: Introductionmentioning

confidence: 99%

Improved synthetic routes to tungsten(IV) bromide complexes

Bhuiyan

Hargrove

Metz

et al. 2015

Transition Met Chem

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Convenient synthetic routes to the compounds WBr 4 (1), WBr 4 (MeCN) 2 (2), WBr 4 (THF) 2 (3), WBr 4 (PPh 3 ) 2 (4), WBr 4 (bpy) (6), and WBr 4 (dppe) (7) are described via the solution-phase oxidation of W(CO) 6 using two equivalents of bromine. These one-pot syntheses use inexpensive and readily available starting materials and produce analytically pure compounds with high yields under mild conditions. Attempts to grow crystals of 1 by heating in a sealed tube at *200°C resulted in formation of the previously reported compound WOBr 4 . Attempts to recrystallize 4 from dichloromethane solution produced [HPPh 3 ] 2 [WBr 6 ] (5). X-ray crystallographic studies showed that 5 consists of an array of [WBr 6 ] 2-anions and [HPPh 3 ] ? cations and that 7ÁCH 2 Cl 2 has the expected sixcoordinate tungsten center. The synthesis of tungsten(IV) bromide compounds via oxidation of W(CO) 6 is simple and provides better yields than previously reported methods. This synthetic route also has many advantages over the syntheses of similar tungsten(IV) chloride compounds which involve reduction of WCl 6 .

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The Preparation and Reactions of Some Tungsten(II) and Tungsten (IV) Halides

Cited by 89 publications

References 0 publications

Phosphorus‐Centered and Phosphinidene‐Capped Tungsten Chloride Clusters

Phosphorus‐Centered and Phosphinidene‐Capped Tungsten Chloride Clusters

Enthalpies of reaction of zirconium and molybdenum tetrachlorides with pyridine, tetrahydrofuran, and tetrahydrothiophene

Improved synthetic routes to tungsten(IV) bromide complexes

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