Abstract
A reaction of palladium dibromide with HBr and (cyclopropyl)(triphenyl)phosphonium bromide in water followed by recrystallization from acetonitrile or DMF afforded the complexes [Ph3(cyclo-C3H5)P]2+ [PdBr4]2− (I) and [Ph3(cyclo-C3H5)P]]2+ [Pd2Br6]2− (II). Recrystallization of complexes I and II from DMSO gave [Ph3(cyclo-C3H5)P]+[PdBr3(DMSO)]− (III). According to X-ray diffraction data, the P-C bond lengths in the tetrahedral (cyclopropyl)(triphenyl)phosphonium cations of complexes I–III are 1.773(5)–1.802(5) (I), 1.778(5)–1.802(5) (II), 1.767(5)–1.797(5) A III); the angles CPC are 107.4(2)°–111.1(2)° (I), 107.2(2)°–111.2(2)° (II), and 108.4(2)°–110.5(2)° (III), and (CIF file CCDC no. 999905 (I), 1035313 (II), 999907 (III)). In the square anions [PdBr4]2−, the Pd-Br bond length is 2.4333(5)–2.4459(5) A. In the planar centrosymmetric dinuclear anions [Pd2Br6]2−, the bond lengths Pd-Brbrid and Pd-Brterm are 2.4559(7), 2.4600(7) and 2.3952(7), 2.4045(8)A; the angles PdBrPd and BrtermPdBrterm are 92.57(2)° and 91.98(3)°, respectively. In the square anions [PdBr3(DMSO)]−, the DMSO molecule is coordinated by the Pd atom through the sulfur atom (Pd-Br, 2.3986(7)–2.4288(6) A; Pd-S, 2.2633(13) A).
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