Tritungsten(IV) cluster compounds with hydroxo ligands. Preparation and structure of [W3O2(O2CCH3)6(H2O)(OH)2]·16H2O and [W3O2(O2CCH3)6(H2O)(OH)2]·KBr·15H2O

Avi Bino; Dan Gibson

doi:10.1016/S0020-1693(00)86765-1

Tritungsten(IV) cluster compounds with hydroxo ligands. Preparation and structure of [W₃O₂(O₂CCH₃)₆(H₂O)(OH)₂]·16H₂O and [W₃O₂(O₂CCH₃)₆(H₂O)(OH)₂]·KBr·15H₂O

Avi Bino^*
, Dan Gibson

^*Corresponding author for this work

Research output: Contribution to journal › Article › peer-review

4 Scopus citations

Abstract

The trinuclear tritungsten(IV) cluster ion, [W₃O₂(OAc)₆(H₂O)₃]²⁺ acts as a polyprotic acid in aqueous solution. If the pH of the solution is about 6, brown yellow crystals of [W₃O₂(OAc)₆(H₂O)·(OH)₂]· 16H₂O, 2, are obtained. In the presence of KBr, crystals of the double salt, [W₃O₂(OAc)₆(H₂O)(OH)₂]· KBr·15H₂O, 3, precipitate upon evaporation of the solution. X-ray structural analyses of the two compounds revealed that compound 2 is monoclinic, space group C2/m with a = 18.845(2) Å, b = 19.001(3) Å, c = 10.862(1) Å, β = 95.60(3)°, V = 3871(1) Å³ and Z = 4. Compound 3 is monoclinic, space group P2₁/c with a = 10.984(1) Å, b = 18.440(2) Å c = 19.305(2) Å, β = 95.63(2)° V = 3891(1) Å³ and Z = 4. The structures were refined by a full-matrix least-squares technique, using 2996 and 3871 reflections to R values of 3.7% and 4.6% respectively. In both structures the presence of the two hydroxo ligands in the cluster causes a considerable increase in the WW bond lengths relative to the triaqua complex. In 3, the potassium cation is bonded to two hydroxo oxygen atoms from neighbouring clusters, forming infinite chains of ··O(H)W₃O(H)⋯K⋯O(H)W₃O(H)⋯ units in the crystal.

Original language	English
Pages (from-to)	155-160
Number of pages	6
Journal	Inorganica Chimica Acta
Volume	104
Issue number	3
DOIs	https://doi.org/10.1016/S0020-1693(00)86765-1
State	Published - 1 Nov 1985

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@article{4a225bef08e94b43a008d8afda83301a,

title = "Tritungsten(IV) cluster compounds with hydroxo ligands. Preparation and structure of [W3O2(O2CCH3)6(H2O)(OH)2]·16H2O and [W3O2(O2CCH3)6(H2O)(OH)2]·KBr·15H2O",

abstract = "The trinuclear tritungsten(IV) cluster ion, [W3O2(OAc)6(H2O)3]2+ acts as a polyprotic acid in aqueous solution. If the pH of the solution is about 6, brown yellow crystals of [W3O2(OAc)6(H2O)·(OH)2]· 16H2O, 2, are obtained. In the presence of KBr, crystals of the double salt, [W3O2(OAc)6(H2O)(OH)2]· KBr·15H2O, 3, precipitate upon evaporation of the solution. X-ray structural analyses of the two compounds revealed that compound 2 is monoclinic, space group C2/m with a = 18.845(2) {\AA}, b = 19.001(3) {\AA}, c = 10.862(1) {\AA}, β = 95.60(3)°, V = 3871(1) {\AA}3 and Z = 4. Compound 3 is monoclinic, space group P21/c with a = 10.984(1) {\AA}, b = 18.440(2) {\AA} c = 19.305(2) {\AA}, β = 95.63(2)° V = 3891(1) {\AA}3 and Z = 4. The structures were refined by a full-matrix least-squares technique, using 2996 and 3871 reflections to R values of 3.7\% and 4.6\% respectively. In both structures the presence of the two hydroxo ligands in the cluster causes a considerable increase in the WW bond lengths relative to the triaqua complex. In 3, the potassium cation is bonded to two hydroxo oxygen atoms from neighbouring clusters, forming infinite chains of ··O(H)W3O(H)⋯K⋯O(H)W3O(H)⋯ units in the crystal.",

author = "Avi Bino and Dan Gibson",

year = "1985",

month = nov,

day = "1",

doi = "10.1016/S0020-1693(00)86765-1",

language = "אנגלית",

volume = "104",

pages = "155--160",

journal = "Inorganica Chimica Acta",

issn = "0020-1693",

publisher = "Elsevier B.V.",

number = "3",

}

TY - JOUR

T1 - Tritungsten(IV) cluster compounds with hydroxo ligands. Preparation and structure of [W3O2(O2CCH3)6(H2O)(OH)2]·16H2O and [W3O2(O2CCH3)6(H2O)(OH)2]·KBr·15H2O

AU - Bino, Avi

AU - Gibson, Dan

PY - 1985/11/1

Y1 - 1985/11/1

N2 - The trinuclear tritungsten(IV) cluster ion, [W3O2(OAc)6(H2O)3]2+ acts as a polyprotic acid in aqueous solution. If the pH of the solution is about 6, brown yellow crystals of [W3O2(OAc)6(H2O)·(OH)2]· 16H2O, 2, are obtained. In the presence of KBr, crystals of the double salt, [W3O2(OAc)6(H2O)(OH)2]· KBr·15H2O, 3, precipitate upon evaporation of the solution. X-ray structural analyses of the two compounds revealed that compound 2 is monoclinic, space group C2/m with a = 18.845(2) Å, b = 19.001(3) Å, c = 10.862(1) Å, β = 95.60(3)°, V = 3871(1) Å3 and Z = 4. Compound 3 is monoclinic, space group P21/c with a = 10.984(1) Å, b = 18.440(2) Å c = 19.305(2) Å, β = 95.63(2)° V = 3891(1) Å3 and Z = 4. The structures were refined by a full-matrix least-squares technique, using 2996 and 3871 reflections to R values of 3.7% and 4.6% respectively. In both structures the presence of the two hydroxo ligands in the cluster causes a considerable increase in the WW bond lengths relative to the triaqua complex. In 3, the potassium cation is bonded to two hydroxo oxygen atoms from neighbouring clusters, forming infinite chains of ··O(H)W3O(H)⋯K⋯O(H)W3O(H)⋯ units in the crystal.

AB - The trinuclear tritungsten(IV) cluster ion, [W3O2(OAc)6(H2O)3]2+ acts as a polyprotic acid in aqueous solution. If the pH of the solution is about 6, brown yellow crystals of [W3O2(OAc)6(H2O)·(OH)2]· 16H2O, 2, are obtained. In the presence of KBr, crystals of the double salt, [W3O2(OAc)6(H2O)(OH)2]· KBr·15H2O, 3, precipitate upon evaporation of the solution. X-ray structural analyses of the two compounds revealed that compound 2 is monoclinic, space group C2/m with a = 18.845(2) Å, b = 19.001(3) Å, c = 10.862(1) Å, β = 95.60(3)°, V = 3871(1) Å3 and Z = 4. Compound 3 is monoclinic, space group P21/c with a = 10.984(1) Å, b = 18.440(2) Å c = 19.305(2) Å, β = 95.63(2)° V = 3891(1) Å3 and Z = 4. The structures were refined by a full-matrix least-squares technique, using 2996 and 3871 reflections to R values of 3.7% and 4.6% respectively. In both structures the presence of the two hydroxo ligands in the cluster causes a considerable increase in the WW bond lengths relative to the triaqua complex. In 3, the potassium cation is bonded to two hydroxo oxygen atoms from neighbouring clusters, forming infinite chains of ··O(H)W3O(H)⋯K⋯O(H)W3O(H)⋯ units in the crystal.

UR - https://www.scopus.com/pages/publications/46549094439

U2 - 10.1016/S0020-1693(00)86765-1

DO - 10.1016/S0020-1693(00)86765-1

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AN - SCOPUS:46549094439

SN - 0020-1693

VL - 104

SP - 155

EP - 160

JO - Inorganica Chimica Acta

JF - Inorganica Chimica Acta

IS - 3

ER -

Tritungsten(IV) cluster compounds with hydroxo ligands. Preparation and structure of [W₃O₂(O₂CCH₃)₆(H₂O)(OH)₂]·16H₂O and [W₃O₂(O₂CCH₃)₆(H₂O)(OH)₂]·KBr·15H₂O

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