Reaction of triphenylphosphine oxide with potassium dichlorodicyanoaurate

The reaction product of propargyltriphenylphosphonium bromide and sodium hydroxide reacts with potassium dichlorodicyanoaurate in acetonitrile to yield an adduct of triphenylphosphine oxide with potassium dichlorodicyanoaurate (Ph3P=О)∙K[Au(CN)2Cl2] (1), which was structurally characterized by X-ray diffraction analysis. Crystallographic characteristics of 1 [C20H15N2OPCl2KAu, M = 637.28 g/mol; monoclinic syngony, space group P21/c; cell parameters: a = 14.7417(10) Å, b = 8.47968(16) Å, c = 25.9453(17) Å; α = γ = 90, β = 138.910(7), V = 2131.6(6) Å3, Z = 4; rcalc = 1.986 g/cm3;  = 7.436 mm–1; F(000) = 1216.0; collection area by q: 2.683–28.281; –19 ≤ h ≤ 19, –11 ≤ k ≤ 11, –34 ≤ l ≤ 34; total reflections 49043; independent reflections 4454 (Rint = 0.0452); GOOF = 1.033; R-factor = 0.0194]. From the X-ray diffraction data, it follows that crystals of 1 consist of triphenylphosphine oxide molecules (P=O 1.4928(18) Å), coordinated by an oxygen atom to a potassium atom (O∙∙∙K distance 2.610(2) Å). The adjacent dichlorodicyanoaurate groups are linked with each other via chlorine atoms (the Cl∙∙∙Au distances Cl∙∙∙Au 3.39(1), 3.54(1) Å). The cyano groups of the anions are coordinated via nitrogen atoms to the μ4-bridging potassium ions (N–K 2.861(2)–2.945(2) Å), thus adduct 1 is a 2D coordination polymer. Complete tables of atomic coordinates, bond lengths and valence angles of compound 1 is deposited in the Cambridge Crystallographic Data Centre (CCDC No. 2477131, deposit@ccdc.cam.ac.uk; http://www.ccdc.cam.ac.uk).