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Synthesis of a Novel Class of Trigonal Bipyramidal Nitrido Tc(V) Complexes with Phosphino−Thiol Ligands. Crystal Structure of [ 99g Tc(N)(L 1 ) 2 ] [L 1 = 2-(Diphenylphosphino)ethanethiolato] and [ 99g Tc(N)(L 5 ) 2 ] [L 5 = 2-(Ditolylphosphino)propanethiolato]

1999; American Chemical Society; Volume: 38; Issue: 20 Linguagem: Inglês

10.1021/ic9903477

1520-510X

Cristina Bolzati, Alessandra Boschi, Licia Uccelli, Erica Malagò, Giuliano Bandoli, Francesco Tisato, Fiorenzo Refosco, Roberto Pasqualini, Adriano Duatti,

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Reactions of the precursor complexes [(99g)Tc(N)Cl(2)(PPh(3))(2)] and [(99g)Tc(N)Cl(4)](-) with phosphine-thiol ligands (HL(n)()) of the type R(2)PCH(2)CH(2)SH (R = phenyl, methoxypropyl), R(2)'PCH(2)CH(2)CH(2)SH (R' = phenyl, tolyl), and R(2)' 'P-o-C(6)H(4)SH (R' ' = phenyl) afforded the five-coordinated, disubstituted nitrido technetium(V) complexes [(99g)Tc(N)(L(n)())(2)]. The complexes were characterized by elemental analysis, (1)H and (31)P NMR spectroscopy, FT IR, and positive FAB MS spectra. Structural characterization of [(99g)Tc(N)(L(1))(2)] (1) [HL(1) = (C(6)H(5))(2)PCH(2)CH(2)SH] and [(99g)Tc(N)(L(5))(2)] (5) [HL(5) = (o-CH(3)C(6)H(4))(2)PCH(2)CH(2)CH(2)SH] showed that the bidentate phosphino-thiol ligands are coordinated to the technetium center through the neutral phosphorus atom and the deprotonated thiol sulfur atom. These complexes possess an uncommon trigonal bipyramidal geometry with the two phosphorus atoms occupying the two transaxial positions and the two sulfur atoms on the equatorial plane along with the nitrido nitrogen atom. Compound 1 crystallizes in the monoclinic space group C2/c, a = 24.84(2) Å, b = 7.327(6) Å, c = 31.52(2) Å, beta = 111.06(10) degrees, and Z = 8. Compound 5 crystallizes in the monoclinic space group P2(1)/n, a = 11.090(1) Å, b = 14.387(2) Å, c = 11.087(1) Å, beta = 113.62(1) degrees, and Z = 2.