Preparation and structural characterization of salts of oxotetrachlorotechnetate(V)

trans-Dichlorobis[o-phenylenebis(dimethylarsine)]technetium(III), perchlorate and chloride salts

“…The average Tc-C1 lengths found here [C1-salt, 2-329 (1)/~; CIO~-salt, 2.318 (6) A] may be compared with recently determined values for (NH4)2[TcCI6], 2.353 (1) /~, , for [TcCI40]-, 2.31 (1)/~, (Cotton, Davison, Day, Gage & Trop, 1979) and for [TcC12(HbPz3)O], 2.328 (6) /~ (Thomas, Estes, Elder & Deutsch, 1979). Thus the Tcm-Cl bond length determined here falls within the range of those found for Tc~v-Cl and Tcv-Cl and indicates that the Tc-C1 distance does not vary systematically with oxidation state.…”

The Present Status of Technetium Chemistry

“…hydrochloric or hydrobromic acid at room temperature yields the oxotetrahalotechnetate(V) complexes [TcOCl 4 ]" and [TcOBr 4 which can be isolated as n-Bu 4 N + -or (Ph 3 P) 2 N + -salts [126][127][128], whereas n-Bu 4 N[TcOI 4 ] has been synthesized from the corresponding oxotetrachloride complex salt by ligand exchange reaction with Nal in acetone [129]. The [TcOCl 4 ion is to the first approximation square pyramidal [126].…”

Final Report, Research Program to Investigate the Fundamental Chemistry of Technetium

“…In order to pursue these investigations, however, it was first necessary to devise improved methods for preparation of common starting materials. A number of technetium and rhenium complexes possessing terminal oxo or nitrido groups and halide ligands have been reported in the literature, but their widespread use has been hindered by difficult and low-yield syntheses (Cotton 1979, Davison 1982, Nelson 1954, Rulfs 1955, Liese 1981, Baldas 1991, Cotton 1966, Rose 1996, Baldas 1984 -, and MOX 3 (L) 2 (M = Tc, Re; X = Cl, Br, I; L = THF, MeCN) were devised. Vibrational and electronic spectroscopies proved best suited to characterize the metal oxohalide complexes; EPR spectroscopy was also utilized to examine the paramagnetic species in the series.…”