Dataset Information

The synthesis and structural characterization of the technetium nitrosyl complexes [TcCl(NO)(SC5H4N)(PPh3)2] and [Tc(NO)(SC5H4N)2(PPh3)].

ABSTRACT: The reaction of the Tc(I) complex [Tc(NO)Cl2(HOMe)(PPh3)2] with stoichiometric amounts of 2-mercatopyridine and a proton scavenger yields [Tc(NO)Cl(Spy)(PPh3)2] or [Tc(NO)(Spy)2(PPh3)], depending upon quantities of ligands employed. These two complexes have been structurally characterized. The small bite angles of the bidentate mercaptopyridine ligands cause significant deviation from octahedral coordination geometry.

SUBMITTER: Nicholson TL

PROVIDER: S-EPMC3676305 | biostudies-literature | 2011 Jan

REPOSITORIES: biostudies-literature

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The synthesis and structural characterization of the technetium nitrosyl complexes [TcCl(NO)(SC5H4N)(PPh3)2] and [Tc(NO)(SC5H4N)2(PPh3)].

Nicholson Terrence L TL Mahmood Ashfaq A Muller Peter P Davison Alan A Storm-Blanchard Shannon S Jones Alun G AG

Inorganica chimica acta 20110101 1

The reaction of the Tc(I) complex [Tc(NO)Cl2(HOMe)(PPh3)2] with stoichiometric amounts of 2-mercatopyridine and a proton scavenger yields [Tc(NO)Cl(Spy)(PPh3)2] or [Tc(NO)(Spy)2(PPh3)], depending upon quantities of ligands employed. These two complexes have been structurally characterized. The small bite angles of the bidentate mercaptopyridine ligands cause significant deviation from octahedral coordination geometry. ...[more]

PMID: 23750048

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Project description:A pentapeptide macrocyclic ligand, KYCAR (lysyl-tyrosyl-cystyl-alanyl-arginine), has been designed as a potential chelating ligand for SPECT imaging and therapeutic in vivo agents. This study shows the synthesis and characterization of KYCAR complexes containing nonradioactive rhenium, 99mTc, or 188Re. The metal complexes were also biologically evaluated to determine in vivo distribution in healthy mice. The overall goals of this project were (1) to synthesize the Tc/Re pentapeptide complexes, (2) to identify spectroscopic methods for characterization of syn versus anti rhenium peptide complexes, (3) to analyze the ex vivo stability, and (4) to assess the biological properties of the [99mTc]TcO-KYCAR and [188Re]ReO-KYCAR complexes in vivo. Details on these efforts are provided below.MethodsNatRe/99mTc/188ReO-KYCAR complexes were synthesized, and macroscopic species were characterized via HPLC, IR, NMR, and CD. These characterization data were compared to the crystallographic data of ReO-KYC to assist in the assignment of diastereomers and to aid in the determination of the structure of the complex.ResultsThe radiometal complexes were synthesized with high purity (>95%). HPLC, IR, NMR and CD data on the macroscopic natReO-KYCAR complexes confirm the successful complexation as well as the presence of two diastereomers in syn and anticonformations. Tracer level complexes show favorable stabilities ex vivo for 2+ h.ConclusionMacroscopic metal complexes form diastereomers with the KYCAR ligand; however, this phenomenon is not readily observed on the tracer level due to the rapid interconversion. It was determined through pKa measurements that the macroscopic natReO-KYCAR complex is 0 at physiological pH. The [99mTc]TcO-KYCAR is stable in vitro while the [188Re]ReO-KYCAR shows 50% decomposition in PBS and serum. Biologically, the tracer level complexes clear through the hepatobiliary pathway. Some decomposition of both tracers is evident by uptake in the thyroid and stomach.

Dataset Information

The synthesis and structural characterization of the technetium nitrosyl complexes [TcCl(NO)(SC5H4N)(PPh3)2] and [Tc(NO)(SC5H4N)2(PPh3)].

Publications

The synthesis and structural characterization of the technetium nitrosyl complexes [TcCl(NO)(SC<sub>5</sub>H<sub>4</sub>N)(PPh<sub>3</sub>)<sub>2</sub>] and [Tc(NO)(SC<sub>5</sub>H<sub>4</sub>N)<sub>2</sub>(PPh<sub>3</sub>)].

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