Synthesis and characterization of tetraalkylammonium tetrathiotungstate complexes: X-ray crystal structure of tetrapropylammonium tetrathiotungstate, [{(C3 H7)4N}2WS4]

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Abstract

The metathesis reaction of aqueous solutions of tetraethylammonium chloride [(C2H5)4 NCl], tetrapropylammonium bromide [(C3H7)4 NBr] and tetrabutylammonium iodide [(C4H9)4NI] with ammonium tetrathiotungstate in the absence of oxidizing agent afforded the mononuclear tetraethylammonium tetrathiotungstate [{(C2H5)4N}2WS4] (1), tetrapropylammonium tetrathiotungstate [{(C3 H7)4N}2WS4] (2) and tetrabutylammonium tetrathiotungstate [{(C4 H9)4N}2WS4] (3). Yields obtained for the complexes were 17%, 21% and 14% respectively. The characteristic of W-S stretching mode was detected at 451, 448, 453 cm-1 for 1, 2 and 3. UV-Vis spectra showed three peaks for each complex. The complex 2 has been crystallographically and spectroscopically characterized. The crystal adopted a monoclinic system with a = 15.4246(2) Å, b = 29.7390(1) Å, c = 16.5056(2) Å and β = 114.11° and belong to the P2(1)/n space group. The crystal structure showed a highly disordered tetrapropylammonium molecule involving the position of the C and Natoms. Complexes 1 and 3 were not characterized crystallographically due to its difficulty to form a single crystal.

Original languageEnglish
Pages (from-to)195-199
Number of pages5
JournalSains Malaysiana
Volume37
Issue number2
Publication statusPublished - Jun 2008

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Tetraethylammonium
Crystal structure
X rays
Bromides
Oxidants
Stretching
Single crystals
Crystals
Molecules
tetrapropylammonium
tetrabutylammonium
ammonium tetrathiotungstate

Keywords

  • Hydrogen
  • Photocatalyst
  • Photolysis
  • Tris(dithiolene)
  • Tungsten

ASJC Scopus subject areas

  • General

Cite this

@article{521899593f6b4bfd8559f4abc58f677b,
title = "Synthesis and characterization of tetraalkylammonium tetrathiotungstate complexes: X-ray crystal structure of tetrapropylammonium tetrathiotungstate, [{(C3 H7)4N}2WS4]",
abstract = "The metathesis reaction of aqueous solutions of tetraethylammonium chloride [(C2H5)4 NCl], tetrapropylammonium bromide [(C3H7)4 NBr] and tetrabutylammonium iodide [(C4H9)4NI] with ammonium tetrathiotungstate in the absence of oxidizing agent afforded the mononuclear tetraethylammonium tetrathiotungstate [{(C2H5)4N}2WS4] (1), tetrapropylammonium tetrathiotungstate [{(C3 H7)4N}2WS4] (2) and tetrabutylammonium tetrathiotungstate [{(C4 H9)4N}2WS4] (3). Yields obtained for the complexes were 17{\%}, 21{\%} and 14{\%} respectively. The characteristic of W-S stretching mode was detected at 451, 448, 453 cm-1 for 1, 2 and 3. UV-Vis spectra showed three peaks for each complex. The complex 2 has been crystallographically and spectroscopically characterized. The crystal adopted a monoclinic system with a = 15.4246(2) {\AA}, b = 29.7390(1) {\AA}, c = 16.5056(2) {\AA} and β = 114.11° and belong to the P2(1)/n space group. The crystal structure showed a highly disordered tetrapropylammonium molecule involving the position of the C and Natoms. Complexes 1 and 3 were not characterized crystallographically due to its difficulty to form a single crystal.",
keywords = "Hydrogen, Photocatalyst, Photolysis, Tris(dithiolene), Tungsten",
author = "Rahman, {Fadhli Hadana} and Arifin Khuzaimah and {Wan Daud}, {Wan Ramli} and Rusli Daik and Mohammad Kassim",
year = "2008",
month = "6",
language = "English",
volume = "37",
pages = "195--199",
journal = "Sains Malaysiana",
issn = "0126-6039",
publisher = "Penerbit Universiti Kebangsaan Malaysia",
number = "2",

}

TY - JOUR

T1 - Synthesis and characterization of tetraalkylammonium tetrathiotungstate complexes

T2 - X-ray crystal structure of tetrapropylammonium tetrathiotungstate, [{(C3 H7)4N}2WS4]

AU - Rahman, Fadhli Hadana

AU - Khuzaimah, Arifin

AU - Wan Daud, Wan Ramli

AU - Daik, Rusli

AU - Kassim, Mohammad

PY - 2008/6

Y1 - 2008/6

N2 - The metathesis reaction of aqueous solutions of tetraethylammonium chloride [(C2H5)4 NCl], tetrapropylammonium bromide [(C3H7)4 NBr] and tetrabutylammonium iodide [(C4H9)4NI] with ammonium tetrathiotungstate in the absence of oxidizing agent afforded the mononuclear tetraethylammonium tetrathiotungstate [{(C2H5)4N}2WS4] (1), tetrapropylammonium tetrathiotungstate [{(C3 H7)4N}2WS4] (2) and tetrabutylammonium tetrathiotungstate [{(C4 H9)4N}2WS4] (3). Yields obtained for the complexes were 17%, 21% and 14% respectively. The characteristic of W-S stretching mode was detected at 451, 448, 453 cm-1 for 1, 2 and 3. UV-Vis spectra showed three peaks for each complex. The complex 2 has been crystallographically and spectroscopically characterized. The crystal adopted a monoclinic system with a = 15.4246(2) Å, b = 29.7390(1) Å, c = 16.5056(2) Å and β = 114.11° and belong to the P2(1)/n space group. The crystal structure showed a highly disordered tetrapropylammonium molecule involving the position of the C and Natoms. Complexes 1 and 3 were not characterized crystallographically due to its difficulty to form a single crystal.

AB - The metathesis reaction of aqueous solutions of tetraethylammonium chloride [(C2H5)4 NCl], tetrapropylammonium bromide [(C3H7)4 NBr] and tetrabutylammonium iodide [(C4H9)4NI] with ammonium tetrathiotungstate in the absence of oxidizing agent afforded the mononuclear tetraethylammonium tetrathiotungstate [{(C2H5)4N}2WS4] (1), tetrapropylammonium tetrathiotungstate [{(C3 H7)4N}2WS4] (2) and tetrabutylammonium tetrathiotungstate [{(C4 H9)4N}2WS4] (3). Yields obtained for the complexes were 17%, 21% and 14% respectively. The characteristic of W-S stretching mode was detected at 451, 448, 453 cm-1 for 1, 2 and 3. UV-Vis spectra showed three peaks for each complex. The complex 2 has been crystallographically and spectroscopically characterized. The crystal adopted a monoclinic system with a = 15.4246(2) Å, b = 29.7390(1) Å, c = 16.5056(2) Å and β = 114.11° and belong to the P2(1)/n space group. The crystal structure showed a highly disordered tetrapropylammonium molecule involving the position of the C and Natoms. Complexes 1 and 3 were not characterized crystallographically due to its difficulty to form a single crystal.

KW - Hydrogen

KW - Photocatalyst

KW - Photolysis

KW - Tris(dithiolene)

KW - Tungsten

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M3 - Article

AN - SCOPUS:51049116863

VL - 37

SP - 195

EP - 199

JO - Sains Malaysiana

JF - Sains Malaysiana

SN - 0126-6039

IS - 2

ER -