Abstract
AbstractCrystal structures of partially oxidized cyanoplatinates were determined by single crystal analysis. Rb1.75[Pt(CN)4]·1.25H2O crystallizes monoclinic in the space group P21/c [a = 1171.4(2) pm, b = 3315.3(6) pm, c = 1054.4(2) pm, β = 114.253(2)°, V = 3733.2(11)·106 pm3, Z = 16, Ntotal = 31567, R(F)N = 0.0858]. The compound was obtained by mixing aqueous solutions of Rb2[Pt(CN)4]·1.5H2O and Rb2[Pt(CN)4]Br2. Cs1.75[Pt(CN)4]·0.5H2O crystallizes in the space group Ibam [a = 1266.1(3) pm, b = 1347.5(3) pm, c = 580.4(1) pm, V = 990.2(3)·106 pm3, Z = 4, Ntotal = 5997, R(F)N = 0.0807]. Crystals of the latter were grown by slow electrochemical oxidation of Cs2[Pt(CN)4]·H2O in aqueous solution using platinum wires as electrodes. In both compounds platinum is partially oxidized to Pt+2.25 and the nearly square‐planar tetracyanoplatinate groups are arranged to columns in a staggered conformation. The rubidium compound features a large unit cell with nonlinear chains of platinum atoms and short alternating Pt–Pt distances of 292 and 294 pm, the cesium compound crystallizes more symmetrically with Pt–Pt distances of c/2 = 290 pm. The two compounds were also characterized by differential thermal analysis, thermogravimetry, infrared, and Raman spectroscopy.
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