Add time:09/29/2019         Source:infona.pl

Two new proton transfer compounds, (acrH) 2 [Zn(hypydc) 2 ]·10H 2 O 1 and (acrH)[Fe(hypydc) 2 ]·4.5H 2 O 2 [where hypydcH 2 =4-hydroxypyridine-2,6-dicarboxylic acid (Chelidamic acid (cas 138-60-3)) and acr=acridine] have been synthesized and characterized by elemental analysis, spectral (UV–Vis, IR), 1 H NMR, 13 C NMR spectroscopy and single crystal X-ray diffraction. The crystallographic analysis revealed that Zn II and Fe III atoms are coordinated by two N atoms and four O atoms from the carboxylate groups of (hypydc) 2− ligands, forming a distorted octahedral geometry. In the anions two pyridine rings are inclined to one another by 88.10(5)° and 83.95(13)° for 1 and 2, respectively. The (H 2 O) n [n=3–6] cyclic–linear water clusters connected two layers of anionic complexes in 1. The crystal packing of 1 show a 3D network formed through H-bonds involving water molecules, NH groups of acridinium and carboxylate anions. In 2 two types of rubout O–H⋯O hydrogen bond synthons, R44 (16) and R44 (18) link the anions and water molecules to form two-dimensional network parallel to bc plane. In crystal structures of both complexes extensive O–H⋯O, N–H⋯O and C–H⋯O hydrogen bonds as well as electrostatic forces, C–O⋯π and π–π stacking play important roles in stabilizing structures. The protonation constants of hypydc and acr, in all of probability protonated forms, the equilibrium constants for the hypydc–acr proton transfer system and the stoichiometry and stability of complexation of this system with Zn 2+ and Fe 3+ ions in 50% dioxane–50% water (V/V) solvent were investigated by potentiometric pH titration method. The stoichiometries of the most complex species in solution were compared with corresponding crystalline metal ion complexes 1 and 2.

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