Reactions of the precursor complexes [99gTc(N)Cl2(PPh3)2] and [99gTc(N)Cl4]- with phosphine-thiol ligands (HLn) of the type R2PCH2CH2SH (R ) phenyl, methoxypropyl), R2¢PCH2CH2CH2SH (R¢ ) phenyl, tolyl), and R2¢¢Po- C6H4SH (R¢¢ ) phenyl) afforded the five-coordinated, disubstituted nitrido technetium(V) complexes [99gTc- (N)(Ln)2]. The complexes were characterized by elemental analysis, 1H and 31P NMR spectroscopy, FT IR, and positive FAB MS spectra. Structural characterization of [99gTc(N)(L1)2] (1) [HL1 ) (C6H5)2PCH2CH2SH] and [99gTc(N)(L5)2] (5) [HL5 ) (o-CH3C6H4)2PCH2CH2CH2SH] 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, â ) 111.06(10)°, and Z ) 8. Compound 5 crystallizes in the monoclinic space group P21/n, a ) 11.090(1) Å, b ) 14.387(2) Å, c ) 11.087(1) Å, â ) 113.62(1)°, and Z ) 2.

Synthesis of a novel class of trigonal bipyramidal nitrido Tc(V) complexes with phosphino-thiol ligands. Crystal structure of [Tc-99g(N)(L-1)(2)] [L-1=2-(diphenylphosphino)ethanethiolato] and [Tc-99g(N)(L-5)(2)] [L5=2-(ditolylphosphino)propanethiolato]

A. BOSCHI
Secondo
;
L. UCCELLI;A. DUATTI
Ultimo
1999

Abstract

Reactions of the precursor complexes [99gTc(N)Cl2(PPh3)2] and [99gTc(N)Cl4]- with phosphine-thiol ligands (HLn) of the type R2PCH2CH2SH (R ) phenyl, methoxypropyl), R2¢PCH2CH2CH2SH (R¢ ) phenyl, tolyl), and R2¢¢Po- C6H4SH (R¢¢ ) phenyl) afforded the five-coordinated, disubstituted nitrido technetium(V) complexes [99gTc- (N)(Ln)2]. The complexes were characterized by elemental analysis, 1H and 31P NMR spectroscopy, FT IR, and positive FAB MS spectra. Structural characterization of [99gTc(N)(L1)2] (1) [HL1 ) (C6H5)2PCH2CH2SH] and [99gTc(N)(L5)2] (5) [HL5 ) (o-CH3C6H4)2PCH2CH2CH2SH] 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, â ) 111.06(10)°, and Z ) 8. Compound 5 crystallizes in the monoclinic space group P21/n, a ) 11.090(1) Å, b ) 14.387(2) Å, c ) 11.087(1) Å, â ) 113.62(1)°, and Z ) 2.
1999
Bolzati, C.; Boschi, A.; Uccelli, L.; Malago, E.; Bandoli, G.; Tisato, F.; Refosco, F.; Pasqualini, R.; Duatti, A.
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Utilizza questo identificativo per citare o creare un link a questo documento: https://hdl.handle.net/11392/1201652
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