Base Hydrolysis of Pentaaminecobalt(III) Complexes: The [CoX(dien) (dapo)]n+ system. Part 1. Syntheses, structures, configuration, and spectroscopy
Abstract
Abstract Oxygentation of aqueous solutions of CoIII in presence of stoichiometric amounts of N‐(2‐aminoethyl)ethane‐1,2‐diamine (dien) and 1,3‐diaminopropan‐2‐ol (dapo) produces μ‐peroxocobalt(III) dimers. Acid cleavage (HCI) yields mer‐exo(H)‐, mer‐endo (H)‐, unsym‐fac‐exo(OH)‐, and unsym‐fac‐endo(OH)‐[CoCl(dien)(dapo)]2+ (A–D)(X = Cl), resp. and unsym‐fac‐[Co‐(dien)(dapo‐N,N′,O)]3+ (G). Isomer seperation was achieved by fractional crystallization as ZnCl and ClO salts and by ion‐exchange chromatography. The corresponding bromo, azido, nitrito‐O, nitro‐N, thiocyanato, hydroxo, and aqua complexes were also synthesized. Optically resolved samples were prepared for chiral compounds, and the complexes were structurally characterized by X‐ray analyses (\documentclass{article}\pagestyle{empty}\begin{document}$ \mathop {\it \Lambda} \limits^ \to $\end{document} (−)436(CD)‐A (X = N3)), (\documentclass{article}\pagestyle{empty}\begin{document}$ \mathop {\it \Delta} \limits^ \to $\end{document} (−)436(CD)‐B). (X = N3), \documentclass{article}\pagestyle{empty}\begin{document}$ \mathop {\it \Delta} \limits^ \to $\end{document} (+)436(CD)‐B by their chiroptical properties, and by 13C‐NMR spectroscopy supported by 1H‐NMR, IR, CD, and UV/VIS spectroscopy. \documentclass{article}\pagestyle{empty}\begin{document}$ \mathop {\it \Lambda} \limits^ \to $\end{document} (−)436(CD)‐mer‐exo(H)‐[Co(N3)(dien)(dapo)](hydrogen di‐O‐benzoyl‐L‐tartrate)2.4 H2O crystallizes in the orthorhombic space group…
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