Complexes of lead(II) bis(O,O′-dialkyl dithiophosphates) with nitrogen donor ligands. The crystal structures of Pb[S2P(OEt)2]2·en (en = ethylenedianine), Pb[S2P(OEt)2]2·bipy (bipy = 2,2′-bipyridine), and {Pb[S2P(OEt)2]2}2·en
Abstract
Ten complexes of lead(II) bis(O,O′-dialkyl dithiophosphates) with nitrogen donor molecules of the type Pb[S2P(OR)2]2·L [R = Et or Pri; L = ethylenediamine (en), 2,2′-bipyridine (bipy), N,N′-diethylethylenediamine (deen), 1,10-phenanthroline (phen), or 2,2′;6′,2″-terpyridine (terpy)] have been prepared by mixing the components in a 1 : 1 molar ratio in ethanol–dichloromethane (1 : 1). Mixing en with Pb[S2P(OEt)2]2 in a 1 : 1 molar ratio in xylene affords the complex {Pb[S2P(OEt)2]2}2·en. The crystal structures of three of the complexes, Pb[S2P(OEt)2]2·en (1), Pb[S2P(OEt)2]2·bipy (2), and {Pb[S2P(OEt)2]2}2·en (3) have been determined by the heavy-atom method from diffractometer data using Mo-Kαradiation (λ= 0.7107 Å). Crystal data: (1) monoclinic, space group P21/c, with a= 14.727(2), b= 14.490(2), c= 11.616(2)Å, β= 110.72(2)°, and Z= 4; (2) triclinic, space group P, with a= 10.933(2), b= 13.257(2), c= 13.705(2)Å, α= 103.58(2), β= 132.24(2), γ= 91.50(2)°, and Z= 2; (3) triclinic, space group P, with a= 9.997(2), b= 14.875(2), c= 15.000(2)Å, α= 98.54(2), β= 100.77(2), γ= 95.64(2)°, and Z= 2. Crystals of (2) comprise discrete centrosymmetric dimer molecules, the central feature of which is a rectangular four-membered Pb2S2ring. Both en complexes (1) and (3) exhibit polymeric structures.