Synthesis and Structure of Tetra( para -tolyl)antimony Dicyanodiiodoaurate [ p -Tol 4 Sb][Au(CN) 2 I 2 ] and Alkyltriphe
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hesis and Structure of Tetra(para-tolyl)antimony Dicyanodiiodoaurate [p-Tol4Sb][Au(CN)2I2] and Alkyltriphenylphosphonium Dicyanodiiodoaurates [Ph3PAlk][Au(CN)2I2], Alk = Me, CH2CN V. V. Sharutina, O. K. Sharutinaa, A. N. Efremova, *, and O. S. Eltsovb aNational
South Ural State Research University, Chelyabinsk, 454080 Russia Ural Federal University Named after the First President of Russia B.N. Yeltsin, Yekaterinburg, 620002 Russia *e-mail: [email protected]
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Received November 26, 2019; revised February 10, 2020; accepted March 11, 2020
Abstract—Red-colored crystalline gold complexes [p-Tol4Sb][Au(CN)2I2] (I), [Ph3PMe][Au(CN)2I2] (II), and [Ph3PCH2CN][Au(CN)2I2] (III) were synthesized by the reaction of potassium dicyanodiiodoaurate with tetra(para-tolyl)antimony and alkyltriphenylphosphonium halides in water. The structure of the complexes was established by IR and NMR spectroscopy and X-ray diffraction. The tetra(para-tolyl)antimony and alkyltriphenylphosphonium cations have a distorted tetrahedral coordination. The dicyanodiiodoaurate anions have a planar structure with a square coordination of the gold atom. The formation of the 3D crystal network is due to weak CN⋅⋅⋅H−C hydrogen bonds between cations and anions (2.39, 2.59 Å (I), 2.70, 2.48, 2.52, 2.68 Å (II), 2.73, 2.50, 2.67, 2.44 Å (III)). In complex III, anions of one of the two types interact with one another via I⋅⋅⋅I contacts to give 1D ladder-like chains along the crystallographic a axis. Keywords: potassium dicyanodiiodoaurate, tetra(para-tolyl)antimony dicyanodiiodoaurate, methyltriphenylphosphonium dicyanodiiodoaurate, cyanomethyltriphenylphosphonium dicyanodiiodoaurate, X-ray diffraction analysis DOI: 10.1134/S1070328420090031
INTRODUCTION The attention of researchers to gold dicyanide complexes is caused by their application for the manufacture of materials with various photochemical and photophysical properties [1–8]. They were shown to be active metabolites of certain drugs [9]. The [Au(CN)2]− anions can form polymer and oligomer frameworks possessing luminescent properties [4, 5, 8–11]. Gold(III) cyano halide complexes are used as sensors for volatile organic compounds (DMF, dioxane, pyridine, ethylene glycol) [12] and as precursors for dicyanide synthesis [13]. Currently, several gold(I) cyanide complexes [14–16] and gold(III) cyano halide complexes with organic and inorganic cations [12, 13, 17–20] are known; however, complexes [Cat]+[Au(CN)2Hal2]− with organoelement cations have not been studied. For elucidating the details of synthesis and structure of tetraarylantimony and tetraorganylphosphonium dicyanodiiodoaurate complexes, here we synthesized and structurally characterized for the first time tetra(para-tolyl)antimony dicyanodiiodoaurate [p-Tol4Sb][Au(CN)2I2] (I) and alkyltriphenylphos-
phonium dicyanodiiodoaurates [Ph3PAlk][Au(CN)2I2], Alk = Me (II), CH2CN (III). EXPERIMENTAL Synthesis of tetra(para-tolyl)antimony dicyanodiiodoaurate (I). A solution of potassium dicyanodiiodoaurate (104 mg, 0.192 mmol) in water (5 mL) was added
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