New mixed-metal carbonyl tellurido clusters from solvothermal synthesis

Birinchi K. Das, Mercouri G Kanatzidis

Research output: Contribution to journalArticle

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Abstract

Mixed-metal carbonyl telluride clusters (Ph4P)2[Fe2MTe3(CO)11] (M = Mo, (1), W, (2)) and Na(Et4N)2[Fe3W2-Te 8(TeMe)(CO)12]·2H2O (3) have been synthesized methanothermally at 80°C using mixtures of Fe3(CO)12, M(CO)6 (M = Mo, W), and Na2Te2 with Ph4PBr, or Et4NCl·H2O, in a sealed Pyrex tube. Compound 1 crystallizes in the monoclinic space group C2/c with a = 20.379(4) Å, b = 14.724(3) Å, c = 39.298(6) Å, β = 95.22(1)°, V = 11742(7) Å3, and Z = 8. In the anionic [Fe2Mo(Te2)(Te)(CO)6]2- cluster of 1, a [Fe2(Te2)(Te)(CO)6]2- unit is joined to an Mo(CO)5 moiety by its Te22- ligand. Compound 3 crystallizes in the triclinic space group P1 with a = 12.636(3) Å, b = 13.385(4) Å, c = 20.804(7) Å, α = 73.30(3)°, β = 87.24(3)°, γ = 65.40(2)°, V = 3054(4) Å3, and Z = 2. In the [Fe3W2(Te2)3(Te) 2(TeMe)(CO)12]3- anion of 3, a W-W unit is connected to the rest of the cluster through telluride ligands to form an unsymmetrical cagelike structure. 125Te NMR spectral data for 1-3 and (Ph4P)2[Fe2(Te2)(Te)(CO)6] have been obtained in DMSO-d6. Clusters 1, 2, and (Ph4P)2[Fe2-(Te2)(Te)(CO) 6] display three-line spectra, while seven singlets are observed for 3, corresponding to seven different environments for the tellurium atoms in 3.

Original languageEnglish
Pages (from-to)5721-5725
Number of pages5
JournalInorganic Chemistry
Volume34
Issue number23
Publication statusPublished - 1995

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Carbon Monoxide
Metals
tellurides
synthesis
metals
ligands
borosilicate glass
tellurium
line spectra
tubes
anions
Tellurium
nuclear magnetic resonance
Ligands
Dimethyl Sulfoxide
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Anions
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Nuclear magnetic resonance
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  • Inorganic Chemistry

Cite this

New mixed-metal carbonyl tellurido clusters from solvothermal synthesis. / Das, Birinchi K.; Kanatzidis, Mercouri G.

In: Inorganic Chemistry, Vol. 34, No. 23, 1995, p. 5721-5725.

Research output: Contribution to journalArticle

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title = "New mixed-metal carbonyl tellurido clusters from solvothermal synthesis",
abstract = "Mixed-metal carbonyl telluride clusters (Ph4P)2[Fe2MTe3(CO)11] (M = Mo, (1), W, (2)) and Na(Et4N)2[Fe3W2-Te 8(TeMe)(CO)12]·2H2O (3) have been synthesized methanothermally at 80°C using mixtures of Fe3(CO)12, M(CO)6 (M = Mo, W), and Na2Te2 with Ph4PBr, or Et4NCl·H2O, in a sealed Pyrex tube. Compound 1 crystallizes in the monoclinic space group C2/c with a = 20.379(4) {\AA}, b = 14.724(3) {\AA}, c = 39.298(6) {\AA}, β = 95.22(1)°, V = 11742(7) {\AA}3, and Z = 8. In the anionic [Fe2Mo(Te2)(Te)(CO)6]2- cluster of 1, a [Fe2(Te2)(Te)(CO)6]2- unit is joined to an Mo(CO)5 moiety by its Te22- ligand. Compound 3 crystallizes in the triclinic space group P1 with a = 12.636(3) {\AA}, b = 13.385(4) {\AA}, c = 20.804(7) {\AA}, α = 73.30(3)°, β = 87.24(3)°, γ = 65.40(2)°, V = 3054(4) {\AA}3, and Z = 2. In the [Fe3W2(Te2)3(Te) 2(TeMe)(CO)12]3- anion of 3, a W-W unit is connected to the rest of the cluster through telluride ligands to form an unsymmetrical cagelike structure. 125Te NMR spectral data for 1-3 and (Ph4P)2[Fe2(Te2)(Te)(CO)6] have been obtained in DMSO-d6. Clusters 1, 2, and (Ph4P)2[Fe2-(Te2)(Te)(CO) 6] display three-line spectra, while seven singlets are observed for 3, corresponding to seven different environments for the tellurium atoms in 3.",
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AB - Mixed-metal carbonyl telluride clusters (Ph4P)2[Fe2MTe3(CO)11] (M = Mo, (1), W, (2)) and Na(Et4N)2[Fe3W2-Te 8(TeMe)(CO)12]·2H2O (3) have been synthesized methanothermally at 80°C using mixtures of Fe3(CO)12, M(CO)6 (M = Mo, W), and Na2Te2 with Ph4PBr, or Et4NCl·H2O, in a sealed Pyrex tube. Compound 1 crystallizes in the monoclinic space group C2/c with a = 20.379(4) Å, b = 14.724(3) Å, c = 39.298(6) Å, β = 95.22(1)°, V = 11742(7) Å3, and Z = 8. In the anionic [Fe2Mo(Te2)(Te)(CO)6]2- cluster of 1, a [Fe2(Te2)(Te)(CO)6]2- unit is joined to an Mo(CO)5 moiety by its Te22- ligand. Compound 3 crystallizes in the triclinic space group P1 with a = 12.636(3) Å, b = 13.385(4) Å, c = 20.804(7) Å, α = 73.30(3)°, β = 87.24(3)°, γ = 65.40(2)°, V = 3054(4) Å3, and Z = 2. In the [Fe3W2(Te2)3(Te) 2(TeMe)(CO)12]3- anion of 3, a W-W unit is connected to the rest of the cluster through telluride ligands to form an unsymmetrical cagelike structure. 125Te NMR spectral data for 1-3 and (Ph4P)2[Fe2(Te2)(Te)(CO)6] have been obtained in DMSO-d6. Clusters 1, 2, and (Ph4P)2[Fe2-(Te2)(Te)(CO) 6] display three-line spectra, while seven singlets are observed for 3, corresponding to seven different environments for the tellurium atoms in 3.

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