TY - JOUR
T1 - New Mixed-Metal Carbonyl Tellurido Clusters from Solvothermal Synthesis
AU - Das, Birinchi K.
AU - Kanatzidis, Mercouri G.
PY - 1995/10/1
Y1 - 1995/10/1
N2 - Mixed-metal carbonyl telluride clusters (Ph4P)2[Fe2MTe3(CO)11] (M = Mo, (1), W, (2)) and Na(Et4N)2[Fe3W2-Te8(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,ß = 95.22(1)°, V = 11742(7) Å3, and Z = 8. In the anionic [Fe2Mo(Te2)(Te)(CO)11]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 Pi with a = 12.636(3) Å, b = 13.385(4) Å, c = 20.804(7) Å, a = 73.30(3)°,ß = 87.24(3)°, ? = 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.
AB - Mixed-metal carbonyl telluride clusters (Ph4P)2[Fe2MTe3(CO)11] (M = Mo, (1), W, (2)) and Na(Et4N)2[Fe3W2-Te8(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,ß = 95.22(1)°, V = 11742(7) Å3, and Z = 8. In the anionic [Fe2Mo(Te2)(Te)(CO)11]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 Pi with a = 12.636(3) Å, b = 13.385(4) Å, c = 20.804(7) Å, a = 73.30(3)°,ß = 87.24(3)°, ? = 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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U2 - 10.1021/ic00127a008
DO - 10.1021/ic00127a008
M3 - Article
AN - SCOPUS:0001284840
SN - 0020-1669
VL - 34
SP - 5721
EP - 5725
JO - Inorganic Chemistry
JF - Inorganic Chemistry
IS - 23
ER -