TY - JOUR
T1 - Synthesis, X-ray Crystal Structures, and NMR Spectroscopy of [PPh4]2[M(Te4)2], M = Hg, Cd, Zn
AU - Bollinger, John C.
AU - Roof, Lisa C.
AU - Smith, Donna M.
AU - McConnachie, Jonathan M.
AU - Ibers, James A.
PY - 1995/3/1
Y1 - 1995/3/1
N2 - The compounds [PPh4]2[M(Te4)2], M = Hg, Cd, Zn, have been prepared by reactions in DMF of appropriate metal salts with polytelluride solutions. X-ray crystal structure determinations were performed on single crystals of each compound. Crystal data for [PPh4]2[Hg(Te4)2]: tetragonal, P4, a = 21.365(3) Å, c = 11.268(2) Å, V = 5143 Å3, R = 0.079. Crystal data for [PPh4]2[Cd(Te4)2]: tetragonal, I4, a = 21.442(3) Å, c = 11.259(2) Å, V = 5176 Å3, R = 0.045. Crystal data for [PPh4]2[Zn(Te4)2]: tetragonal, I4, a = 21.396(4) Å, c = 11.169(2) Å, V = 5113 Å3, R = 0.094. These crystal structures are surprisingly complex, and the anions exhibit disorder; nevertheless, the anions have the expected structure of metal atoms coordinated tetrahedrally by two Te42− chelates. 125Te NMR spectra of these compounds and of [PPh4]2[Pd(Te4)2] are reported, and assignments of metal-bound and ring-bound Te nuclei are given. The resulting trends in the 125Te chemical shifts parallel those noted previously for the 77Se chemical shifts in the selenometalate analogues.
AB - The compounds [PPh4]2[M(Te4)2], M = Hg, Cd, Zn, have been prepared by reactions in DMF of appropriate metal salts with polytelluride solutions. X-ray crystal structure determinations were performed on single crystals of each compound. Crystal data for [PPh4]2[Hg(Te4)2]: tetragonal, P4, a = 21.365(3) Å, c = 11.268(2) Å, V = 5143 Å3, R = 0.079. Crystal data for [PPh4]2[Cd(Te4)2]: tetragonal, I4, a = 21.442(3) Å, c = 11.259(2) Å, V = 5176 Å3, R = 0.045. Crystal data for [PPh4]2[Zn(Te4)2]: tetragonal, I4, a = 21.396(4) Å, c = 11.169(2) Å, V = 5113 Å3, R = 0.094. These crystal structures are surprisingly complex, and the anions exhibit disorder; nevertheless, the anions have the expected structure of metal atoms coordinated tetrahedrally by two Te42− chelates. 125Te NMR spectra of these compounds and of [PPh4]2[Pd(Te4)2] are reported, and assignments of metal-bound and ring-bound Te nuclei are given. The resulting trends in the 125Te chemical shifts parallel those noted previously for the 77Se chemical shifts in the selenometalate analogues.
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U2 - 10.1021/ic00110a021
DO - 10.1021/ic00110a021
M3 - Article
AN - SCOPUS:0000979009
SN - 0020-1669
VL - 34
SP - 1430
EP - 1434
JO - Inorganic Chemistry
JF - Inorganic Chemistry
IS - 6
ER -