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Synthesis and Crystal Structures of Dinuclear Palladium and Mononuclear Nickel Complexes of Macrocyclic N 8 S 4 Ligands
Author(s) -
Lozan Vasile,
Kersting Berthold
Publication year - 2008
Publication title -
zeitschrift für anorganische und allgemeine chemie
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.354
H-Index - 66
eISSN - 1521-3749
pISSN - 0044-2313
DOI - 10.1002/zaac.200700546
Subject(s) - chemistry , ligand (biochemistry) , crystal structure , palladium , nickel , perchlorate , ethylene , metal , crystallography , salt (chemistry) , ring (chemistry) , stereochemistry , catalysis , organic chemistry , ion , biochemistry , receptor
The N 8 S 4 donor ligand L 1 has been investigated regarding its capability to support the formation of coordinatively unsaturated Pd 2 complexes and its use as a starting material for functionalized N 8 S 4 systems. L 1 represents a macrotricyclic ligand comprising four 4‐ tert ‐butyl‐2,6‐bis(aminomethyl)thiophenolate units, whose N and S atoms are linked by ethylene units. Treatment of L 1 with [Pd(NCMe) 2 Cl 2 ] produced the dinuclear complex [Pd 2 Cl 2 (H 2 L 1 )] 4+ , which was isolated as its pale‐yellow perchlorate salt [Pd 2 Cl 2 (H 2 L 1 )](ClO 4 ) 4 (H 2 1 ) and characterized by elemental analysis, IR, NMR and MS spectroscopy and X‐ray crystallography. The structure shows two planar PdN 2 SCl units which are located in the central 24‐membered ring of L 1 . Reaction of L 1 with CH 2 O/HCO 2 H under Eschweiler‐Clarke conditions followed by deprotection with sodium in liquid ammonia furnished the permethylated octaamine‐tetrathiophenol H 4 L 4 . The identity of H 4 L 4 was ascertained by an X‐ray crystal structure determination of one of its metal complexes.