Solvothermal synthesis, molecular structures and spectroscopic characterization of the cluster compounds (Ph4P) 2[Fe4Te2(CO)14] and Cs[HFe3Te(CO)9]

Birinchi K. Das, Mercouri G Kanatzidis

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Abstract

The iron carbonyl tellurido cluster (Ph4P)2[Fe4Te2(CO)14] (1) has been synthesized at 80°C in moderate yield by heating a mixture of Fe3(CO)12, Na2Te2, and Ph4PBr in a 2:1:6 molar ratio in a sealed Pyrex tube containing 0.4 ml of methanol. Another cluster, Cs[HFe3Te(CO)9] (2) has been prepared similarly by allowing Fe3(CO)12 to react with Cs2Te3 (4: 1 molar ratio) in 0.2 ml of H2O at 130°C. Compound 1 crystallizes in the monoclinic space group C2/c (No. 15) with a = 23.324(3) Å, b = 11.793(2) Å, c = 23.499(5) Å, β = 102.02(1)°, V = 6322(2) Å3, Z = 4. A central 'Fe23-Te)2(CO)6' butterfly unit remains connected to two Fe(CO)4 fragments through the tellurium atoms in the anion of 1. Compound 2 crystallizes in the orthorhombic space group Pbca (No. 61) with a = 9.672(2) Å, b = 15.816(4) Å, c = 21.430(5) Å, V = 3278(2) Å3, Z = 8. In the anion of this compound, a Te2- ligand caps a triiron triangle to form an approximate tetrahedron, with a hydride ligand bridging one of the Fe-Fe bonds. Both compounds have been characterized by solid state and solution infrared spectroscopy and 125Te NMR spectroscopy.

Original languageEnglish
Pages (from-to)1-6
Number of pages6
JournalJournal of Organometallic Chemistry
Volume513
Issue number1-2
Publication statusPublished - May 3 1996

Fingerprint

Carbon Monoxide
Molecular Structure
Molecular structure
molecular structure
Negative ions
Ligands
anions
ligands
Tellurium
borosilicate glass
tellurium
synthesis
caps
Hydrides
triangles
tetrahedrons
Nuclear magnetic resonance spectroscopy
hydrides
Anions
Infrared spectroscopy

Keywords

  • Chalcogenides
  • Hydrothermal synthesis
  • Iron
  • Metal carbonyls
  • Metal clusters
  • Tellurium

ASJC Scopus subject areas

  • Biochemistry
  • Inorganic Chemistry
  • Organic Chemistry
  • Physical and Theoretical Chemistry
  • Materials Chemistry

Cite this

@article{b07354b1331b43c6b022b75e944cc2d1,
title = "Solvothermal synthesis, molecular structures and spectroscopic characterization of the cluster compounds (Ph4P) 2[Fe4Te2(CO)14] and Cs[HFe3Te(CO)9]",
abstract = "The iron carbonyl tellurido cluster (Ph4P)2[Fe4Te2(CO)14] (1) has been synthesized at 80°C in moderate yield by heating a mixture of Fe3(CO)12, Na2Te2, and Ph4PBr in a 2:1:6 molar ratio in a sealed Pyrex tube containing 0.4 ml of methanol. Another cluster, Cs[HFe3Te(CO)9] (2) has been prepared similarly by allowing Fe3(CO)12 to react with Cs2Te3 (4: 1 molar ratio) in 0.2 ml of H2O at 130°C. Compound 1 crystallizes in the monoclinic space group C2/c (No. 15) with a = 23.324(3) {\AA}, b = 11.793(2) {\AA}, c = 23.499(5) {\AA}, β = 102.02(1)°, V = 6322(2) {\AA}3, Z = 4. A central 'Fe2(μ3-Te)2(CO)6' butterfly unit remains connected to two Fe(CO)4 fragments through the tellurium atoms in the anion of 1. Compound 2 crystallizes in the orthorhombic space group Pbca (No. 61) with a = 9.672(2) {\AA}, b = 15.816(4) {\AA}, c = 21.430(5) {\AA}, V = 3278(2) {\AA}3, Z = 8. In the anion of this compound, a Te2- ligand caps a triiron triangle to form an approximate tetrahedron, with a hydride ligand bridging one of the Fe-Fe bonds. Both compounds have been characterized by solid state and solution infrared spectroscopy and 125Te NMR spectroscopy.",
keywords = "Chalcogenides, Hydrothermal synthesis, Iron, Metal carbonyls, Metal clusters, Tellurium",
author = "Das, {Birinchi K.} and Kanatzidis, {Mercouri G}",
year = "1996",
month = "5",
day = "3",
language = "English",
volume = "513",
pages = "1--6",
journal = "Journal of Organometallic Chemistry",
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T1 - Solvothermal synthesis, molecular structures and spectroscopic characterization of the cluster compounds (Ph4P) 2[Fe4Te2(CO)14] and Cs[HFe3Te(CO)9]

AU - Das, Birinchi K.

AU - Kanatzidis, Mercouri G

PY - 1996/5/3

Y1 - 1996/5/3

N2 - The iron carbonyl tellurido cluster (Ph4P)2[Fe4Te2(CO)14] (1) has been synthesized at 80°C in moderate yield by heating a mixture of Fe3(CO)12, Na2Te2, and Ph4PBr in a 2:1:6 molar ratio in a sealed Pyrex tube containing 0.4 ml of methanol. Another cluster, Cs[HFe3Te(CO)9] (2) has been prepared similarly by allowing Fe3(CO)12 to react with Cs2Te3 (4: 1 molar ratio) in 0.2 ml of H2O at 130°C. Compound 1 crystallizes in the monoclinic space group C2/c (No. 15) with a = 23.324(3) Å, b = 11.793(2) Å, c = 23.499(5) Å, β = 102.02(1)°, V = 6322(2) Å3, Z = 4. A central 'Fe2(μ3-Te)2(CO)6' butterfly unit remains connected to two Fe(CO)4 fragments through the tellurium atoms in the anion of 1. Compound 2 crystallizes in the orthorhombic space group Pbca (No. 61) with a = 9.672(2) Å, b = 15.816(4) Å, c = 21.430(5) Å, V = 3278(2) Å3, Z = 8. In the anion of this compound, a Te2- ligand caps a triiron triangle to form an approximate tetrahedron, with a hydride ligand bridging one of the Fe-Fe bonds. Both compounds have been characterized by solid state and solution infrared spectroscopy and 125Te NMR spectroscopy.

AB - The iron carbonyl tellurido cluster (Ph4P)2[Fe4Te2(CO)14] (1) has been synthesized at 80°C in moderate yield by heating a mixture of Fe3(CO)12, Na2Te2, and Ph4PBr in a 2:1:6 molar ratio in a sealed Pyrex tube containing 0.4 ml of methanol. Another cluster, Cs[HFe3Te(CO)9] (2) has been prepared similarly by allowing Fe3(CO)12 to react with Cs2Te3 (4: 1 molar ratio) in 0.2 ml of H2O at 130°C. Compound 1 crystallizes in the monoclinic space group C2/c (No. 15) with a = 23.324(3) Å, b = 11.793(2) Å, c = 23.499(5) Å, β = 102.02(1)°, V = 6322(2) Å3, Z = 4. A central 'Fe2(μ3-Te)2(CO)6' butterfly unit remains connected to two Fe(CO)4 fragments through the tellurium atoms in the anion of 1. Compound 2 crystallizes in the orthorhombic space group Pbca (No. 61) with a = 9.672(2) Å, b = 15.816(4) Å, c = 21.430(5) Å, V = 3278(2) Å3, Z = 8. In the anion of this compound, a Te2- ligand caps a triiron triangle to form an approximate tetrahedron, with a hydride ligand bridging one of the Fe-Fe bonds. Both compounds have been characterized by solid state and solution infrared spectroscopy and 125Te NMR spectroscopy.

KW - Chalcogenides

KW - Hydrothermal synthesis

KW - Iron

KW - Metal carbonyls

KW - Metal clusters

KW - Tellurium

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