Reactions of Tetraorganylphosphonium Bromide with Dibromodicyanoaurate Potassium in a Solution of Acetonitrile
Keywords:
carboxymethyltriphenylphosphonium dibromodicyanoaurate, allyltriphenylphosphonium, acetonitrile, synthesis, structure, IR-spectroscopy, X-ray diffraction analysisAbstract
The interaction of tetraorganylphosphonium bromide with dibromodicyanoaurate potassium in acetonitrile solution synthesized the complexes [Ph3PCH2C(O)OH][Au(CN)2Br2] (1), [Ph3PCH2CH = CH2][Au(CN)2] (2). Compounds 1 and 2 were characterized by IR spectroscopy and X-ray diffraction. According to XRD data, carried out at 293 K on an automatic D8 QuestBruker four-circle diffractometer (MoKα radiation, λ = 0.71073 Å, graphite monochromator), phosphorus atoms in cations of complexes 1 and 2 have a distorted tetrahedral configuration [C23H20N2Br2AuO2Р] (1), M = 744.17; monoclinic syngony, P2/с symmetry group; cell parameters: a = 17.87 (3), b = 7.833 (10), c = 19.10 (3) Å; a = 90.00 degrees, β = 112.11 (8) degrees,
g = 90.00 degrees; V = 2477 (6) Å3; crystal size 0.63 ´ 0.52 ´ 0.45 mm; reflection index intervals
–23 ≤ h ≤ 23, –9 ≤ k ≤ 9, –21 ≤ l ≤ 21; total reflections 34113; independent reflections 4592;
Rint 0.1535; GOOF 1.030; R1 = 0.1279; wR2 = 0.2234; residual electron density 3.99/–3.52 e/Å–3, [C23H20N2PAu] (2), M 552.35; monoclinic syngony, symmetry group P21/ n; cell parameters:
a = 9.494 (7), b = 14.956 (13), c = 15.587 (12) Å; a = 90.00 degrees, β = 97.33 (2) degrees,
g = 90.00 degrees; V = 2195 (3) Å3; crystal size 0.31´0.25´0.1 mm; intervals of reflection indices
–13 ≤ h ≤ 13, –21 ≤ k ≤ 21, –22 ≤ l ≤ 21; total reflections 85407; independent reflections 7250; Rint 0.0533; GOOF 1,485; R1 = 0.1932; wR2 = 0.4118; residual electron density of 4.15/–8.01 e / Å–3. Valent angles of CPC in 1 and 2 are 105.7(8)°-114.1(9)° for 1, 107.1(3)°-110.8(3)° for 2, the lengths of the P-C bonds are close to each other: 1.736(18)-1.82(2) Å to 1; 1.794(6) -1.828 (7) Å to 2. Full tables of atomic coordinates, bond lengths and valence angles are deposited in the Cambridge structural data bank (# 1920013 for 1, 1919946 for 2, deposit@ccdc.cam.ac.uk;
http://www.ccdc.cam.ac.uk).
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