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- W2022048085 abstract "The reaction of (Bu4N)[TcOCl4] in methanol with 1-acetyl-2-phenylhydrazine, followed by 1,2-bis(diphenylphosphino)ethane (DPPE) gives the green technetium(V) phenylimido complex [TcCl3(NPh)(DPPE)]. The IR spectrum of this complex shows a characteristic peak at 1110 cm-1 which is assigned to v(TcN) from the linearly coordinated phenylimido unit. The 1H NMR spectrum shows a pair of coupled multiplets at 3.1 and 3.6 ppm from the aliphatic protons plus a series of six multiplets between 6.5 and 8.1 ppm from the aromatic protons of the bidentate phosphine ligand and imido-phenyl groups. The positive mode fast atom bombardment mass spectrum displays a peak at 695 m/z which corresponds to the protonated patent molecule. Also, a peak at 658 m/z corresponds to the fragment generated from the loss of one chloride from the neutral patent molecule. The X-ray crystal structure shows a facial arrangement of chloride ligands, with a TcN bond length of 1.687 Å and a TcNC bond angle of 175.7° indicative of sp hybridization of the linearly coordinated phenylimido unit. Crystal data for TcCl3P2NC32H29: monoclinic space group Pc (No. 7), a=11.177(2), b=10.912(2), c=14.056(2) Å, β=108.34(1)°, V=1627.3(5) Å3, with Dcalc=1.414 g cm−3 to give Z=2. Structure solution based on 3069 reflections converged at R=0.051, Rw=0.072, GOF=2.32. The analogous reaction with triphenylphosphine gives the previously reported Tc(V) phenylimido complex [TcCl3(NPh)(PPh3)2]. This Tc(V) phenylimido complex reacts with pyridine in methanol to give the mixed ligand complex [TcCl3(NPh)(PPh3)(NC5H5)]. The positive mode FAB mass spectrum of this complex shows fragments which correspond to the sodium adducts of the neutral molecule minus one chloride ligand, (Na)[TcCl2(NPh)(PPh3)(C5H5N)]+ at 624 m/z, and the molecule minus two chloride ligands, (Na)[TcCl(NPh)(PPh3)(C5H5N)]+ at 589 m/z. Also present in the mass spectrum are peaks which correspond to the fragments [TcCl3(PPh3)(C5H5N)]+ at 545 m/z and [TcCl2(PPh3)(C5H5N)]+ at 510 m/z. The IR spectrum of this complex shows an absorption at 1090 cm−1 which is assigned to v(TcN) from the linearly coordinated phenylimido unit." @default.
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- W2022048085 title "The synthesis and characterization of [TcCl3(NPh)(Ph2PCH2CH2PPh2)] and [TcCl3(NPh)(PPh3)2]. The single crystal X-ray structure of [TcCl3(NPh)(Ph2PCH2CH2PPh2)]" @default.
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- W2022048085 doi "https://doi.org/10.1016/s0020-1693(00)82956-4" @default.
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