Reactions of Tetraorganylphosphonium and Tetraethylammonium Chloride with Hexachloroplatinic Acid Hexahydrate in Solutions of Acetonitrile and Diethylsulphoxide
Keywords:
ethyltriphenylphosphonium chloride, tetraethylammonium chloride, tetraphenylphosphonium chloride, acetonitrile, diethylsulfoxide, hexachloroplatinic acid, diethylsulfoxidopentachloroplatinate anion, X-ray diffraction analysisAbstract
The interaction of hexachloroplatinic acid with tetraorganylphosphonium, tetraethylammonium chlorides in solutions of acetonitrile in the presence of diethylsulphoxide (deso) synthesized the following complexes: [Ph4P][PtCl6]·CH3CN (1), [Ph3PEt][PtCl5(deso-S)] (2), [Et4N][PtCl5(deso-S)] (3). The structures 1-3 were determined by XRDA and IR. The X-ray diffraction patterns of crystals 1-3 were obtained at 293 K on an automatic diffractometer D8 Quest Broker (MoKα radiation, λ = 0.71073 Å, graphite monochromator) the phosphorus and nitrogen atoms of complexes 1-3 have a distorted tetrahedral configuration in the cations. [C52H46N2Cl6P2Pt](1), M 1168.64; the triclinic syngony, the symmetry group P ; cell parameters: a = 10.200(10), b = 10.960(15), c = 12.160(11) Å; a = 73.65(4) degrees, β = 80.64(3) degrees, g = 77.48(4) degrees; V = 1266(2) Å3; the crystal size is 0.48´0.39´0.13 mm; intervals of reflection indexes -12 ≤ h ≤ 12, -13 ≤ k ≤ 13, -15 ≤ l ≤ 15; total reflections 27973; independent disclosures 5205; Rint 0.0338; GOOF 1.028; R1 = 0.0470; wR2 = 0.1252; residual electron density 6.33/-1.14 e/Å3, C24H30PCl5PtSO (2), M 769.85; the monoclinic syngony, the symmetry group P21/n; cell parameters: a = 12.176(6), b = 14.522(9), c = 16.426(8) Å; a = 90.00 degrees,β = 95.365(16)degrees, g = 90.00 degrees; V = 2892(3) Å3; the crystal size is 0.64´0.39´0.22 mm; intervals of reflection indexes -22 ≤ h ≤ 22, -26 ≤ k ≤ 26,-30 ≤ l ≤ 30; total reflections 147427; independent disclosures 19324; Rint 0.0674; GOOF 1.078; R1 = 0.0642; wR2 = 0.1019; residual electron density 4.49/-2.72 e/Å3, C12H30NCl5PtSO (3), M 608.77; the monoclinic syngony, the symmetry group P21/c; cell parameters: a = 10.535(6), b = 15.206(7), c = 13.149(6) Å;
a = 90.00 degrees, β = 94.12(2) degrees, g = 90.00 degrees; V = 2101.0(19) Å3; the crystal size is 0.52´0.27´0.15 mm; intervals of reflection indexes -19 ≤ h ≤ 19, -28 ≤ k ≤ 28, -24 ≤ l ≤ 22;
total reflections 48540; independent disclosures 14161; Rint 0.0537; GOOF 0.999; R1 = 0.0447; wR2 = 0.0648; residual electron density 1,60/-1,26 e/Å3]. The СРС and CNC valence angles are 107.9(3)°-113.2(3)° for 1, 108.7(2)°-111.2(3)° for 2, 108.6(2)°-111.2(2)° for 3, distance P-С 1.785(6)-1.805(6) Å in 1; 1.789(4)-1.801(5) Å in 2, and distance N-C 1.515(4)-1.524(4) Å in 3. In octahedral anions [PtCl6]2− trans-angles ClPtCl equal 180.0º, distance 2.308(2)–2.327(3) Å in a crystal solvate. In the [PtCl5(dmso-S)]− anions of complexes 2, 3 the SPtCl trans-angles are 175.12(5)°-176.23(3)°, the СlPtCl trans-angles equal 177.12(3)°-178.45(3)°, the distances Pt-Cl and Pt-S are 2.3156(14)-2.3379(14) and 2.3363(14) in 1, 2.3219(12)-2.3459(12) and 2.3424(12) in 2. Complete tables of coordinates of atoms, bond lengths and valence angles are deposited at the Cambridge Structural Data (No. 1865783 for 1, 1854655 for 2, 1854649 for 3,
deposit@ccdc.cam.ac.uk; http://www.ccdc. cam.ac.uk).
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