Tungsten Oxyhalides

Tillack, J.; Brown, T. M.; Schäfer, Harald

doi:10.1002/9780470132456.ch22

Cited by 15 publications

(1 citation statement)

References 11 publications

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“…Before use, WOCl 4 was sublimated twice 9,10. WOBr 4 was prepared by heating a mixture of W (Merck), WO 3 (Fluka) and Br 2 (Merck) in an ampoule at 670 K and sublimating the product twice 11. Bismuth, obtained by reduction of bismuth(III) oxide with potassium cyanide in a porcelain crucible,12 was liquated twice in vacuo to get bare metallic bismuth.…”

Section: Methodsmentioning

confidence: 99%

Mixed Valence Tungsten (IV, V) Compounds with Layered Structures (Part IV): Syntheses, Crystal Structures, and Conductivity of BiX₂[W₂O₂X₆] (X = Cl, Br)

Schieweling

Daniels

Beck

2012

Zeitschrift anorg allge chemie

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The reaction of metallic bismuth with either tungsten tetrachlorideoxide WOCl 4 at 650 K or tungsten tetrabromideoxide WOBr 4 at 670 K, respectively, leads to BiX 2 [W 2 O 2 X 6 ] (X = Cl, Br) as black, lustrous crystal needles. The crystal structure determinations (triclinic, P1) show the two isotypic structures to be closely related to Hg 0.55 [W 2 O 2 Cl 6 ] with the presence of 1D-polymeric W 2 O 2 X 6 double strands. Dinuclear [Bi 2 X 4 ] 2+ cations are embedded in the host structure via secondary W-X···Bi bonds. Unlike the other members of the M y [W 2 O 2 X 6 ] structure family, which crystallize monoclinic and show crystallographic equivalent tungsten atoms, BiX 2 [W 2 O 2 X 6 ] has indeAll steps of preparation were performed in an argon filled glove box. Ampoules were made of borosilicate glass or silica glass, if required, and flame-dried in vacuo prior to use. WOCl 4 was prepared by heating freshly precipitated WO 3 , obtained by spiking a saturated NaWO 4 solution with concentrated hydrochloric acid, with SOCl 2 under reflux.

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