Synthesis and Crystal Structure of theTris-bidentate Carbonatobis-(1,10-phenanthroline-N,N′)nickel(II), [Ni(C12H8N2)2(CO3)

Abstract

The tris-bidentate complex [Ni(C12H8N2)2(CO3)] was synthesized by the reaction of Na2CO3, 1,10-phenanthroline (phen = C12H8N2) and NiSO4 · 6 H2O in the presence of succinic acid in a CH3OH–H2O solution. The compound crystallizes as heptahydrate. The crystal structure (monoclinic, P21/c (no. 14), a = 9.897(1), b = 26.384(2), c = 10.582(1) A, β = 105.87(1)°, Z = 4, R = 0.0505, wR2 = 0.1029 for 3166 observed reflections (F ≥ 2σ(F) out of 6100 unique reflections) consists of hydrogen bonded water molecules and [Ni(phen)2(CO3)] complex molecules. The Ni atoms are sixfold octahedrally coordinated by the four N atoms of two bidentate chelating phen ligands and by two O atoms of the bidentate chelating carbonate group with d(Ni–N) = 2.092–2.100 A, d(Ni–O) = 2.051, 2.079 A. The complex molecules are stacked into 2D corrugated layers parallel to (010) via two types of intermolecular π-π stacking interactions. One occurs between two quinoline rings of neighboring phen ligands at the distance of 3.63 A in [010] direction and the other results from 1D π-π stacking interactions through partially covered phen rings at alternative distances of 3.26 A and 3.33 A in [001] direction. The water molecules are sandwiched between 2D layers.