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Reaction of the potassium salt of N‐thiophosphorylated thiourea α‐naphthylNHC(S)NHP(S)(OiPr)2 (HL) with Cu(PPh3)3I in aqueous EtOH/CH2Cl2 leads to the mononuclear complex [Cu(PPh3)2L–S,S′]. By using copper(I) iodide instead ofCu(PPh3)3I, the polynuclear complex [Cun(L–S,S′)n] was obtained. The structures of these compounds were investigated by elemental analysis, 1H and 31P{1H} NMR and IR spectroscopy. The crystal structures of HL and Cu(PPh3)2L were determined by single‐crystal X‐ray diffraction.

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The complex [Cu(en) 2 (H 2 O)](sy) 2 (en)(H 2 O) 2 has been synthesized and characterized by its electronic and vibrational spectra. The molecular structure of the complex has been determined by X-ray diffraction methods. The complex crystallizes in the orthorhombic space group Pnma with unit-cell parameters a = 10.7236 (5), b = 20.4660(10), c = 14.4523(11)Å and Z = 4. In the cation, the Cu(II) ion has a distorted square pyramidal coordination with two bidendate (en) ligands forming the basal plane and a H 2 O molecule in the apical position. The complex cations and syringate anions constitute chains along the b axis in -A-B-A-fashion. The members of the chains are linked by through N-H···O hydrogen bonds. The (en) molecules are responsible for connecting adjacent layers.