Syn−Anti Isomerism in a Mixed-Ligand Oxorhenium Complex, ReO[SN(R)S][S]
- 1 January 1996
- journal article
- research article
- Published by American Chemical Society (ACS) in Inorganic Chemistry
- Vol. 35 (25), 7377-7383
- https://doi.org/10.1021/ic9604167
Abstract
The simultaneous action of the tridentate ligand (C2H5)2NCH2CH2N(CH2CH2SH)2 and the monodentate coligand HSC6H4OCH3 on a suitable ReO3+ precursor results in a mixture of syn- and anti-oxorhenium complexes, ReO[(C2H5)2NCH2CH2N(CH2CH2S)2] [SC6H4OCH3], in a ratio of 25/1. The complexes are prepared by a ligand exchange reaction using ReO(eg)2 (eg = ethylene glycol), ReOCl3(PPh3)2, or Re(V)−citrate as precursor. Both complexes have been characterized by elemental analysis, FT-IR, UV−vis, X-ray crystallography, and NMR spectroscopy. The syn isomer C17H29N2O2S3Re crystallizes in the monoclinic space group P21/n, a = 14.109(4) Å, b = 7.518(2) Å, c = 20.900(5) Å, β = 103.07(1)°, V = 2159.4(9) Å3, Z = 4. The anti isomer C17H29N2O2S3Re crystallizes in P21/n, a = 9.3850(7) Å, b = 27.979(2) Å, c = 8.3648(6) Å, β = 99.86(1)°, V = 2163.9(3) Å3, Z = 4. Complete NMR studies show that the orientation of the N substituent chain with respect to the ReO core greatly influences the observed chemical shifts. Complexes were also prepared at the tracer (186Re) level by using 186Re-citrate as precursor. Corroboration of the structure at tracer level was achieved by comparative HPLC studies.Keywords
This publication has 23 references indexed in Scilit:
- A New Donor Atom System [(SNN)(S)] for the Synthesis of Neutral Oxotechnetium(V) Mixed-Ligand ComplexesInorganic Chemistry, 1996
- 1H and 13C NMR structural studies in solution of oxotechnetium(V) complexes with N,N‐bis(2‐mercaptoethyl)‐N′,N′‐diethylethylenediamine and N,N‐bis(2‐mercaptoethyl)‐2‐ethylthioethylamineMagnetic Resonance in Chemistry, 1994
- Tridentate ligands containing the SNS donor atom set as a novel backbone for the development of technetium brain-imaging agentsJournal of Medicinal Chemistry, 1994
- Preparation and structural characterization of monoamine-monoamide bis(thiol) oxo complexes of technetium(V) and rhenium(V)Inorganic Chemistry, 1994
- Synthesis and characterization of neutral MVO (M = technetium, rhenium) amine-thiol complexes containing a pendant phenylpiperidine groupInorganic Chemistry, 1993
- Synthesis and characterization of diamide dithiol complexes of technetium(V) and rhenium(V). Assignment of the stereochemistry of the chelate epimers by NMR spectroscopyInternational Journal of Radiation Applications and Instrumentation. Part A. Applied Radiation and Isotopes, 1991
- Lipophilic technetium complexes—VII. Neutral oxotechnetium(V) complexes of tridentate Schiff-bases containing monothioles as co-ligandsInternational Journal of Radiation Applications and Instrumentation. Part A. Applied Radiation and Isotopes, 1990
- New brain perfusion imaging agents based on technetium-99m bis(aminoethanethiol) complexes: stereoisomers and biodistributionJournal of Medicinal Chemistry, 1989
- Brain imaging agents: Synthesis and characterization of (N-piperidinylethyl) hexamethyl diaminodithiolate oxo technetium(V) complexesApplied Radiation and Isotopes, 1987
- Synthesis, structure, and spectroscopic properties of copper(II) compounds containing nitrogen–sulphur donor ligands; the crystal and molecular structure of aqua[1,7-bis(N-methylbenzimidazol-2′-yl)-2,6-dithiaheptane]copper(II) perchlorateJ. Chem. Soc., Dalton Trans., 1984