113945-92-9Relevant articles and documents
Studies of technetium complexes. 9. Use of the tetrachloronitridotechnetate(VI) anion for the preparation of nitrido complexes of technetium. Crystal structure of bis(8-quinolinethiolato)nitridotechnetium(V)
Baldas, John,Bonnyman, John,Williams, Geoffrey A.
, p. 150 - 153 (2008/10/08)
The TcVINCl4- anion is shown to be a useful intermediate for the preparation of Tc≡N complexes. Reaction of AsPh4[TcNCl4] with LiBr in acetone gives AsPh4[TcNBr4], and reaction of TcNCl4- with CsCl gives Cs2[TcNCl5]. The TcNCl4- anion undergoes reduction on reaction with PPh3, KNCS, Na[S2CNEt2], and 8-quinolinethiol (C9H6NSH) to give the TcV≡N complexes [TcNCl2(PPh3)2], [NEt4]2[TcN(NCS)4(CH3CN)], [TcN(S2CNEt2)2], and [TcN(C9H6NS)2], respectively. A single-crystal X-ray structure determination of bis(8-quinolinethiolato)nitridotechnetium(V), [TcN(C9H6NS)2], is reported. Crystals are monoclinic, space group C2/c, with a = 15.92 (1) ?, b = 7.347 (6) ?, c = 15.33 (2) ?, β = 110.89 (8)°, and Z = 4. Full-matrix least-squares refinement gave R = 0.029 for 1618 independent reflections. The coordination geometry of technetium is distorted square pyramidal with the apical Tc≡N bond of length 1.623 (4) ?. Tc-S and Tc-N(quinoline) bond distances are 2.3559 (7) and 2.135 (2) ?, respectively.