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
M3 - Article
AN - SCOPUS:0030567475
VL - 513
SP - 1
EP - 6
JO - Journal of Organometallic Chemistry
JF - Journal of Organometallic Chemistry
SN - 0022-328X
IS - 1-2
ER -