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
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