Multiple bonds between main group elements and transition metals. 95. Synthesis and reactivity of TcCl(CO)3[P(C6H5)3]2: Novel technetium complexes of 1, 4, 7-triazacyclononane and hydridotris(pyrazolyl)borate

Roger Alberto, Wolfgang A. Herrmann, Paul Kiprof, Franz Baumgärtner

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Abstract

Trans-TcCl(CO)3[P(C6H5)3]2 (2) is accessible in 95% yield by treatment of the easily available Tc(V) ionic precursor [TcOCl4]-(1) with triphenylphosphine in an atmosphere of carbon monoxide (1 atm). 2 is recognized as a useful starting material for subsequent substitution reactions, especially with tridentate nitrogen ligands. Thus, the compounds [(C6H15N3)Tc(CO)2|P(C6-H5)3|]Cl (5) and [HB(C3H3N2)3]Tc(CO)2(P(C6H5)3|] (6) were synthesized in good yields. The structures of compounds 2, 5, and 6 were determined by single-crystal X-ray diffraction techniques. 2 crystallizes in the triclinic space group P1 (No. 2) with a = 10.245 (1) Å,b = 12.744 (1) Å, c = 14.423 (1) Å, α = 69.42 (1)°, β = 74.89 (1)°, γ = 81.51 (1)°, R = 0.029, and = 0.025. Compound 5 crystallizes in the monoclinic space group P2Jc (No. 14) with a = 12.997 (5) Å, b = 8.680 (1) Å, c = 25.189 (5) Å, β = 101.13 (4)°, R = 0.059, and Rw = 0.037. Compound 6 crystallizes in the monoclinic space group C2/c (No. 15) with a = 31.191 (8) Å, b = 9.7252 (6) Å, c = 18.818 (5) Å, β = 93.36 (1)°, R = 0.045, and Rw = 0.033.

Original languageEnglish (US)
Pages (from-to)895-899
Number of pages5
JournalInorganic Chemistry
Volume31
Issue number5
DOIs
StatePublished - Mar 1 1992

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