A Three-Dimensional Framework Structure Constructed from 2-(2-Pyridyl-N-oxide) Ethylphosphonic Acid and Nd(III)

A multistep synthesis for 2-(2-pyridyl-N-oxide) ethylphosphonic acid 6-H 2 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 d...

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Bibliographic Details
Published in:Inorganic chemistry 2006-05, Vol.45 (9), p.3741-3745
Main Authors: Gan, Xin-min, Rapko, Brian M, Fox, Jesse, Binyamin, Iris, Pailloux, Sylvie, Duesler, Eileen N, Paine, Robert T
Format: Article
Language:English
Subjects:
08 HYDROGEN
2-Pyridyl-N-Oxide Ethyl Phosphonic Acid
ANIONS
ATOMS
BOND LENGTHS
HYDROGEN
MONOCRYSTALS
Nd(III)
OXYGEN
PHOSPHONATES
PHOSPHONIC ACIDS
PROTONS
SYMMETRY
SYNTHESIS
X-RAY DIFFRACTION
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Summary:A multistep synthesis for 2-(2-pyridyl-N-oxide) ethylphosphonic acid 6-H 2 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 3̄ 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; Nd(2)−O(4), 2.340 (1) Å. The monoanionic ligand (6-H)-1, therefore, serves to bridge the unique Nd(III) centers.
ISSN:0020-1669
1520-510X
DOI:10.1021/ic051937+