NDLI: Mn $^{2+}$ complexes of 1-oxa-4,7-diazacyclononane based ligands with acetic, phosphonic and phosphinic acid pendant arms: Stability and relaxation studies

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Mn $^{2+}$ complexes of 1-oxa-4,7-diazacyclononane based ligands with acetic, phosphonic and phosphinic acid pendant arms: Stability and relaxation studies

Content Provider	World Health Organization (WHO)-Global Index Medicus
Author	Lukes, Ivan Tóth, Eva Havlícková, Jana Hermann, Petr Pniok, Miroslav Císarová, Ivana Drahos, Bohuslav Kotek, Jan
Description	Author Affiliation: Drahos B ( Department of Inorganic Chemistry, Faculty of Science, Universita Karlova (Charles University), Hlavova, 2030, 128 43, Prague 2, Czech Republic.)
Abstract	A new class of macrocyclic ligands based on 1-oxa-4,7-diazacyclononane was synthesized and their Mn $^{2+}$ complexes were investigated with respect to stability and relaxation properties. Each ligand has two pendant arms involving carboxylic ( H $_{2}$ L $^{1}$ — 1-oxa-4,7-diazacyclononane-4,7-diacetic acid ), phosphonic ( H $_{4}$ L $^{2}$ — 1-oxa-4,7-diazacyclononane-4,7-bis(methylenephosphonic acid) ), phosphinic ( H $_{2}$ L $^{3}$ — 1-oxa-4,7-diazacyclononane-4,7-bis(methylenephosphinic acid) ) or phenylphosphinic ( H $_{2}$ L $^{4}$ — 1-oxa-4,7-diazacyclononane-4,7-bis[methylene(phenyl)phosphinic acid] ) acid moieties. H $_{2}$ L $^{3}$ and H $_{2}$ L $^{4}$ were synthesized for the first time. The crystal structure of the Mn $^{2+}$ complex with H $_{2}$ L $^{4}$ confirmed a coordination number of 6 for Mn $^{2+}$ . The protonation constants of all ligands and the stability constants of their complexes with Mn $^{2+}$ and some biologically or biomedically relevant metal ions were determined by potentiometry . The protonation sequence of H $_{2}$ L $^{3}$ was followed by $^{1}H$ and $^{31}P$ NMR titration and the second protonation step was attributed to the second macrocyclic nitrogen atom . The potentiometric data revealed a relatively low thermodynamic stability of the Mn $^{2+}$ complexes with all ligands investigated. For H $_{2}$ L $^{3}$ and H $_{2}$ L $^{4}$ , full Mn $^{2+}$ complexation cannot be achieved even with 100% ligand excess. The transmetallation of Mn L $^{1}$ and Mn L $^{2}$ with Zn $^{2+}$ was too fast to be followed at pH 6. Variable temperature $^{1}H$ NMRD and $^{17}O$ NMR measurements have been performed on Mn L $^{1}$ and Mn L $^{2}$ to provide information on water exchange and rotational dynamics. The $^{17}O$ chemical shifts indicate hydration equilibrium between mono- and bishydrated species for Mn L $^{1}$ , while Mn L $^{2}$ is monohydrated. The water exchange is considerably faster on Mn L $^{1}$ $(k_{ex}^{298}$ = 1.2 × $10^{9}$ $s^{−1})$ than on Mn L $^{2}$ $(k_{ex}^{298}$ = 1.2 × $10^{7}$ $s^{−1}).$ Small endogenous anions ( phosphate , carbonate , citrate ) do not replace the coordinated water in either of the complexes, but they induce their slow decomposition . All Mn $^{2+}$ complexes are stable toward air- oxidation .
ISSN	14779226
Issue Number	39
Volume Number	40
e-ISSN	13645447
Journal	Dalton Trans.
Language	English
Publisher	Royal Society of Chemistry
Publisher Date	2011-10-21
Publisher Place	Great Britain (UK)
Access Restriction	Subscribed
Subject Keyword	Acetic Acid Chemistry Coordination Complexes Manganese Organometallic Compounds Organophosphonates Phosphinic Acids Crystallography, X-Ray Kinetics Ligands Magnetic Resonance Spectroscopy Molecular Conformation Journal Article Research Support, Non-U.S. Gov't
Content Type	Text
Resource Type	Article
Subject	Inorganic Chemistry

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