A multi-step synthesis for 2-(2-pyridyl N-oxide) ethylphosphonic acid 6-H2 is described along with its spectroscopic (IR, NMR) data and a single crystal x-ray diffraction structure analysis. Combination of the ligand with Nd(OH)3 results in the formation of a complex Nd(6-H)3. Single crystal x-ray diffraction analysis reveals a three-dimensional crystal network generated by hydrogen bonded chains along the crystallographic c axis. The hydrogen bonds are formed between phosphonic acid anion (6-H)-1 protons on one chain and pyridyl N-oxide oxygen atoms in neighboring chains. The asymmetric unit contains 1/3 [Nd(6-H)3] and there are two unique Nd(III) atoms, each with point symmetry. As a result, each Nd(III) ion is bound to six (6-H)-1 ligands and the symmetry about the Nd(III) ion is octahedral with each vertex occupied by a phosphonate oxygen atom. The Nd-O bond lengths are essentially identical: Nd(1)-O(3), 2.336 (1) Å and Nd(2)-O(4), 2.340 (1) Å. The monoanionic ligand (6-H)-1, therefore, serves to bridge the unique Nd(III) centers.
Revised: June 22, 2006 |
Published: May 1, 2006
Citation
Gan X., B.M. Rapko, J. Fox, I. Binyamin, S. Pailloux, E.N. Duesler, and R.T. Paine. 2006.A Three-Dimensional Framework Structure Constructed from 2-(2-Pyridyl-N-oxide) Ethylphosphonic Acid and Nd(III).Inorganic Chemistry 45, no. 9:3741-3745.PNNL-SA-49417.doi:10.1021/ic051937