Abstract
AbstractThe N8S4 donor ligand L1 has been investigated regarding its capability to support the formation of coordinatively unsaturated Pd2 complexes and its use as a starting material for functionalized N8S4 systems. L1 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 L1 with [Pd(NCMe)2Cl2] produced the dinuclear complex [Pd2Cl2(H2L1)]4+, which was isolated as its pale‐yellow perchlorate salt [Pd2Cl2(H2L1)](ClO4)4 (H21) and characterized by elemental analysis, IR, NMR and MS spectroscopy and X‐ray crystallography. The structure shows two planar PdN2SCl units which are located in the central 24‐membered ring of L1. Reaction of L1 with CH2O/HCO2H under Eschweiler‐Clarke conditions followed by deprotection with sodium in liquid ammonia furnished the permethylated octaamine‐tetrathiophenol H4L4. The identity of H4L4 was ascertained by an X‐ray crystal structure determination of one of its metal complexes.
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