화학공학소재연구정보센터
Inorganic Chemistry, Vol.34, No.6, 1430-1434, 1995
Synthesis, X-Ray Crystal-Structures, and NMR-Spectroscopy of (Pph(4))2(M(Te4)2), M=hg, Cd, Zn
The compounds [PPh(4)](2)[M(Te-4)(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 [PPh(4)](2)[Hg(Te-4)(2)] : tetragonal, P $($) over bar$$ 4, a = 21.365(3) Angstrom, c = 11.268(2) Angstrom, V = 5143 Angstrom(3), R = 0.079. Crystal data for [PPh(4)](2)[Cd(Te-4)(2)] : tetragonal, I $($) over bar$$ 4, a = 21.442(3) Angstrom, c = 11.259(2) Angstrom, V = 5176 Angstrom(3), R = 0.045. Crystal data for [PPh(4)](2)[Zn(Te-4)(2)] : tetragonal, I $($) over bar$$ 4, n = 21.396(4) Angstrom, c = 11.169(2) Angstrom, V = 5113 Angstrom(3), 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 Te-4(2-) chelates. Te-125 NMR spectra of these compounds and of [PPh(4)](2)[Pd(Te-4)(2)] are reported, and assignments of metal-bound and ring-bound Te nuclei are given. The resulting trends in the Te-125 chemical shifts parallel those noted previously for the Se-77 chemical shifts in the selenometalate analogues.