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

doi:10.1016/0022-328X(95)05983-V

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^*

^*Corresponding author for this work

Chemistry

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

18 Scopus citations

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 '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 Te^2- 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 language	English (US)
Pages (from-to)	1-6
Number of pages	6
Journal	Journal of Organometallic Chemistry
Volume	513
Issue number	1-2
DOIs	https://doi.org/10.1016/0022-328X(95)05983-V
State	Published - May 3 1996

Keywords

Chalcogenides
Hydrothermal synthesis
Iron
Metal carbonyls
Metal clusters
Tellurium

ASJC Scopus subject areas

Biochemistry
Physical and Theoretical Chemistry
Organic Chemistry
Inorganic Chemistry
Materials Chemistry

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10.1016/0022-328X(95)05983-V

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@article{a198170efcac4c09bcbf1f81f20ee25a,

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.}",

note = "Funding Information: Financial support from the National Science Foundation is gratefully acknowledged. MGK is a Camille and Henry Dreyfus Teacher Scholar (1993-1995).",

year = "1996",

month = may,

day = "3",

doi = "10.1016/0022-328X(95)05983-V",

language = "English (US)",

volume = "513",

pages = "1--6",

journal = "Journal of Organometallic Chemistry",

issn = "0022-328X",

publisher = "Elsevier",

number = "1-2",

}

TY - JOUR

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.

N1 - Funding Information: Financial support from the National Science Foundation is gratefully acknowledged. MGK is a Camille and Henry Dreyfus Teacher Scholar (1993-1995).

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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U2 - 10.1016/0022-328X(95)05983-V

DO - 10.1016/0022-328X(95)05983-V

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