Facile Reduction of Tungsten Halides with Nonconventional, Mild Reductants. I. Tungsten Tetrachloride: Several Convenient Solid-State Syntheses, a Solution Synthesis of Highly Reactive (WCl4)x, and the Molecular Structure of Polymeric Tungsten Tetrachloride
Publication type: Journal Article
Publication date: 1998-05-30
scimago Q1
wos Q1
SJR: 0.958
CiteScore: 7.4
Impact factor: 4.7
ISSN: 00201669, 1520510X
Inorganic Chemistry
Physical and Theoretical Chemistry
Abstract
Polymeric (WCl4)x has been prepared in crystalline form from WCl6 by three new, safer solid-state approaches via mercury (in 83% yield), bismuth (82% yield), or antimony (97% yield) reduction. A modification of a published procedure for reduction of WCl6 with red phosphorus, which improves (WCl4)x purity, is also described. Highly reactive (WCl4)x powder can be prepared in 99% yield via tin reduction of WCl6 in 1,2-dichloroethane. (WCl4)x powder was readily converted in high yields to the known WCl4(MeCN)2 and W2Cl4(OMe)4(HOMe)2. The molecular structure of (WCl4)x, as determined by single-crystal X-ray diffractometry, consists of a polymer of opposite-edge-sharing bioctahedra with alternating short (W(1)−W(1A), 2.688(2) A) and long (W(1)···W(1B), 3.787(3) A) tungsten−tungsten distances. The acute W(1)−Cl(2)−W(1A) angle (69.4(2)°), obtuse Cl(1)−W(1)−W(1A) angle (94.99(12)°), short axial Cl(1)···Cl(1A) nonbonded distance (3.085(10) A, substantially less than twice the Cl van der Waals radius), and short W(1...
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Kolesnichenko V., Swenson D. C., Messerle L. Facile Reduction of Tungsten Halides with Nonconventional, Mild Reductants. I. Tungsten Tetrachloride: Several Convenient Solid-State Syntheses, a Solution Synthesis of Highly Reactive (WCl4)x, and the Molecular Structure of Polymeric Tungsten Tetrachloride // Inorganic Chemistry. 1998. Vol. 37. No. 13. pp. 3257-3262.
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Kolesnichenko V., Swenson D. C., Messerle L. Facile Reduction of Tungsten Halides with Nonconventional, Mild Reductants. I. Tungsten Tetrachloride: Several Convenient Solid-State Syntheses, a Solution Synthesis of Highly Reactive (WCl4)x, and the Molecular Structure of Polymeric Tungsten Tetrachloride // Inorganic Chemistry. 1998. Vol. 37. No. 13. pp. 3257-3262.
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TY - JOUR
DO - 10.1021/ic9801286
UR - https://doi.org/10.1021/ic9801286
TI - Facile Reduction of Tungsten Halides with Nonconventional, Mild Reductants. I. Tungsten Tetrachloride: Several Convenient Solid-State Syntheses, a Solution Synthesis of Highly Reactive (WCl4)x, and the Molecular Structure of Polymeric Tungsten Tetrachloride
T2 - Inorganic Chemistry
AU - Kolesnichenko, Vladimir
AU - Swenson, Dale C.
AU - Messerle, Louis
PY - 1998
DA - 1998/05/30
PB - American Chemical Society (ACS)
SP - 3257-3262
IS - 13
VL - 37
SN - 0020-1669
SN - 1520-510X
ER -
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@article{1998_Kolesnichenko,
author = {Vladimir Kolesnichenko and Dale C. Swenson and Louis Messerle},
title = {Facile Reduction of Tungsten Halides with Nonconventional, Mild Reductants. I. Tungsten Tetrachloride: Several Convenient Solid-State Syntheses, a Solution Synthesis of Highly Reactive (WCl4)x, and the Molecular Structure of Polymeric Tungsten Tetrachloride},
journal = {Inorganic Chemistry},
year = {1998},
volume = {37},
publisher = {American Chemical Society (ACS)},
month = {may},
url = {https://doi.org/10.1021/ic9801286},
number = {13},
pages = {3257--3262},
doi = {10.1021/ic9801286}
}
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MLA
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Kolesnichenko, Vladimir, et al. “Facile Reduction of Tungsten Halides with Nonconventional, Mild Reductants. I. Tungsten Tetrachloride: Several Convenient Solid-State Syntheses, a Solution Synthesis of Highly Reactive (WCl4)x, and the Molecular Structure of Polymeric Tungsten Tetrachloride.” Inorganic Chemistry, vol. 37, no. 13, May. 1998, pp. 3257-3262. https://doi.org/10.1021/ic9801286.