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Synthesis and spectroscopy of diethyl (pyridinylmethyl)phosphates and their palladium (II) complexes: X-ray crystal structures of Pd(II) complexes
Authors:Urszula Kalinowska  Magdalena Ma?ecka  Bernhard Lippert
Institution:a Department of Bioinorganic Chemistry, Medical University, Muszyńskiego 1, 90-151 ?ód?, Poland
b Department of Crystallography and Crystal Chemistry, University of ?ód?, Pomorska 149/153, 90-236 ?ód?, Poland
c Fachbereich Chemie, Universitat Dortmund, Otto-Hahn Str. 6, 44-227 Dortmund, Germany
Abstract:The synthesis of diethyl (pyridin-2-, -3-, -4-ylmethyl)phosphate (2-pmOpe, 3-pmOpe, 4-pmOpe) ligands and their palladium (II) complexes of general formula trans-PdCl2L2] (L = 2-pmOpe, 3-pmOpe,4-pmOpe) has been described. Pyridine phosphate derivatives were synthesized via the condensation of phosphorochloridic acid diethyl ester with an appropriate pyridinylmethanol in the presence of triethylamine. The compounds have been identified and characterized by IR, far-IR, 1H NMR, 31P NMR, 31P CP-MAS NMR and elemental analyses. The crystal and molecular structures of palladium (II) complexes, i.e., PdCl2(2-pmOpe)2] and PdCl2(4-pmOpe)2] determined by the X-ray diffraction method, are presented. In both structures, Pd(II) ions are four-coordinated by two chlorine atoms and two pyridine nitrogen atoms. The geometry of complexes is square-planar and adopt a trans configuration, which is consistent with preparation method.
Keywords:Palladium complexes  Pyridine complexes  Phosphoric acid esters ligands  Crystal structures  trans geometry
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