The first metal phosphate incorporating isonicotinate ligand: synthesis, crystal structure, and solid-state NMR spectroscopy of Zn(HINT)(HPO4)

摘要

The first metal phosphate incorporating isonicotinate ligand, Zn(HINT)(HPO4), was hydrothermally synthesized and characterized by single-crystal X-ray diffraction and solid-state NMR spectroscopy. This compound crystallizes in the monoclinic space group P2(1)/c with cell parameters a = 20.5643(8) Angstrom, b = 8.5169(4) A, c = 10.3928(4) Angstrom, beta = 97.466(1)degrees, and Z = 8. The structure consists of 2D neutral sheets of zinc hydrogen phosphate with the dipolar isonicotinate ligand being coordinated to zinc as a pendent group. Adjacent sheets are connected by hydrogen bonding. The H-1 magic angle spinning NMR spectrum exhibits three resonances at 15.5, 8.1, and 4.8ppm with an intensity ratio close to 1:4:1, corresponding to two different types of protons in isonicotinate ligand and one type of protons in hydrogen phosphate groups. The peak at 15.5 ppm can be assigned to the proton bonded to the pyridine nitrogen atom, which confirms the presence of +HNC5H4COO-. (C) 2003 Elsevier Inc. All rights reserved.