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Application of technetium and rhenium carbonyl chemistry to nuclear medicine. Preparation of [NEt4]2[TcCl3(CO)3] from [NBu4][TcO4] and structure of [NEt4][Tc2(μ-Cl)3(CO)6]; structures of the model complexes [NEt4][Re2(μ-OEt)2(μ-OAc)(CO)6] and [ReBr({-CH2S(CH2)2Cl}2)(CO)3]

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Abstract

A detailed investigation of the one-pot synthesis of [NEt4]2[MX3(CO)3] [M=Tc (1a) or Re (1b); X= Cl−, Br−] is presented. The intermediates [NEt4][Tc2-(μ-Cl)3(CO)6] (2a), [NBu4][Tc3(μ3-H)(μ-H)3(CO)9] (3) and [Tc3(μ-H)3(CO)12] (4) have been isolated and characterized. The X-ray structure of (2a) is described. Complex (2a) crystallizes in the monoclinic space group P21/c with a=19.491(6), b=18.323(2) and c=17.497(9)AÅ, and β=97.59(2)°. Quantitative conversion of (2a), (3) and (4) into the aqua-ion [M(OH2)3(CO)3]+ [M=Tc (5a) or Re (5b)] is described. To evaluate an optimal and simple chelating group for the “fac-M(CO)3” moiety, the reaction with the bidentate thioether ligand Cl(CH2)2S(CH2)2S(CH2)2Cl (qyp) has been investigated and the structure of the neutral complex [ReBr(qyp)(CO)3] (6) is described. Complex (6) crystallizes in the monoclinic space group P21/c with a=15.935(6), b=2.788(4) and c= 7.955(10)AÅ, and β=98.57(1)°. To extend the knowledge about substitution chemistry of organometallic complexes in aqueous solution, the acetato ligand [OOCCH3]− has been reacted with (1b), resulting in the formation of the dinuclear, acetato-bridged complex [NEt4][Re2(μ-OH)2(μ-OAc)(CO)6], which converted into [Re2(μ-OEt)2(μ-OAc)(CO)6]− (7) after recrystallization from EtOH. The X-ray structure of (7) has been determined. Complex (7) crystallizes in the monoclinic space group P21/c with a=16.288(3), b=12.4272(10) and c=13.620(3)AÅ, and β=76.63(1)°. For a future application of the small “fac-M(CO)3” moiety, it seems thus advantageous to combine these two ligand groups in one simple chelating function.

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Authors and Affiliations

  1. Institute of Inorganic Chemistry, University of Zu¨rich, Winterthurerstr. 190, CH-8057, Zu¨rich, Switzerland

    Roger Alberto

  2. Division of Radiopharmacy, Paul Scherrer Institute, CH-5232, Villigen, Switzerland

    Roger Schibli, Daniela Angst & P. August Schubiger

  3. Institute of Inorganic Chemistry, University of Tu¨bingen, Auf der Morgenstelle 18, D-72076, Tu¨bingen, Germany

    Ulrich Abram & Sonja Abram

  4. Institute of Inorganic Chemistry, University of Basel, Spitalstrasse 51, CH-4056, Basel, Switzerland

    Th. A. Kaden

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  1. Roger Alberto
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  2. Roger Schibli
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  3. Daniela Angst
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  4. P. August Schubiger
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  5. Ulrich Abram
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Alberto, R., Schibli, R., Angst, D. et al. Application of technetium and rhenium carbonyl chemistry to nuclear medicine. Preparation of [NEt4]2[TcCl3(CO)3] from [NBu4][TcO4] and structure of [NEt4][Tc2(μ-Cl)3(CO)6]; structures of the model complexes [NEt4][Re2(μ-OEt)2(μ-OAc)(CO)6] and [ReBr({-CH2S(CH2)2Cl}2)(CO)3]. Transition Metal Chemistry 22, 597–601 (1997). https://doi.org/10.1023/A:1018573026710

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