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Synthesis of New Pd II Complexes Containing a Thioether‐Pyrazole Hemilabile Ligand − Structural Analysis by 1 H, 13 C NMR Spectroscopy and Crystal Structure of [PdCl(bdtp)]BF 4 [bdtp = 1,5‐Bis(3,5‐dimethyl‐1‐pyrazolyl)‐3‐thiapentane]
Author(s) -
GarcíaAntón Jordi,
Pons Josefina,
Solans Xavier,
FontBardia Mercè,
Ros Josep
Publication year - 2003
Publication title -
european journal of inorganic chemistry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.667
H-Index - 136
eISSN - 1099-0682
pISSN - 1434-1948
DOI - 10.1002/ejic.200300235
Subject(s) - thioether , chemistry , ligand (biochemistry) , azine , crystallography , crystal structure , nuclear magnetic resonance spectroscopy , infrared spectroscopy , medicinal chemistry , pyrazole , spectroscopy , stereochemistry , organic chemistry , biochemistry , physics , receptor , quantum mechanics
Treatment of the ligand 1,5‐bis(3,5‐dimethyl‐1‐pyrazolyl)‐3‐thiapentane (bdtp) with [PdCl 2 (CH 3 CN) 2 ] led to a [PdCl 2 (bdtp)] complex. Subsequent treatment of this complex with AgBF 4 gave [PdCl(bdtp)](BF 4 ). These Pd II complexes were characterised by elemental analysis, conductivity measurements, IR spectroscopy, and 1 H and 13 C NMR spectroscopy. Complex [PdCl 2 (bdtp)] was again obtained when the complex [PdCl(bdtp)](BF 4 ) was heated under reflux in a solution of NEt 4 Cl in CH 2 Cl 2 /MeOH (1:1). Ligand bdtp in complexes 1 and 2 exhibited a hemilabile character. The X‐ray structure of the complex [PdCl(bdtp)](BF 4 ) was determined. The metal atom is tricoordinated by the two azine nitrogen atoms and one thioether sulfur atom of the thioether‐pyrazole ligand, its coordination (distorted square planar) being completed with one chloride ion. (© Wiley‐VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2003)