1. Synthesis and structure of methyltriphenylphosphonium dicyanodibromoaurate [Ph3PCH3] [Au(CN)2Br2]
- Author
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Efremov, A. N., Sharutin, V. V., Sharutina, O. K., Andreev, P. V., Eltsov, O. S., Efremov, A. N., Sharutin, V. V., Sharutina, O. K., Andreev, P. V., and Eltsov, O. S.
- Abstract
Methyltriphenylphosphonium dicyanodibromoaurate (1) [Ph3PMe]+[Au(CN)2Br2]- was synthesized by the reaction of potassium dicyanodibromoaurate with methyltriphenylphosphonium bromide in an aqueous solution and was structurally characterized. The complex is a yellow-col-ored, air-resistant crystalline substance with a clear melting point. The structure of the compound was established by IR spectroscopy, NMR spectroscopy and X-ray diffraction analysis. An intense absorption band was observed in the IR spectrum of compound at 2220 cm-1, corresponding to the stretching vibrations of cyano groups. The absorption band of the deformation vibrations of the P-SPh bonds in the IR spectrum is at 1438 cm-1. In the recorded 1N, 13S, and 31R NMR spectra, signals are observed for the number, value of chemical shifts and integral intensity that do not contradict the proposed complex structure. The X-ray diffraction analysis of crystal 1 was carried out on a Bruker D8 QUEST diffractometer (MoKα radiation, λ = 0.71073 A, graphite monochrom-ator). [C21H18AuBr2N2P, M = 686.13, crystal system triclinic, space group P-1, a = 8.802(5), b = 8.989(5), c = 15.233(11) A, V = 1143.8(13) A3, Z = 2, μ = 10.002 mm-1, F(000) = 644, crystal size 0.41x0.30x0.22 mm]. According to the X-ray diffraction analysis (XRDA) data there are two types of centrosymmetric crystallographically independent monomeric dicyanodibromoaurate anions and methyltriphenylphosphonium cations in the crystal of compound MFDDA. The cations have a distorted tetrahedral configuration: the CPC angles equal 108.8(2)°-110.0(2)°, the P-S distances are 1.791(5)-1.800(5) A. All SAuC and BrAuBr trans-angles are 180.0° in the [Au(CN)2Br2]-an-ions. The Au-C distances in anions differ from each other and equal 2.040(7), 2.024(1), 1.991(2) A. These values are close to the sum of the covalent radii of atoms (2.03 A). The Au-Br bond lengths are equal to 2.4162(14), 2.4591, 2.474(5) A in dicyanodibromoaurate anions. Formation of the crystal str
- Published
- 2020