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Synthesis and Molecular and Crystal Structure of K4.5{[Mo33-Te)(μ2-Te2)3(CN)6]I}I1.5·3H2O and Cs3{[Mo33-Te)(μ2-Te2)3(CN)6]I}·2H2O

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Abstract

Crystal structures of two new compounds containing trigonal tellurium-bridged cluster fragments [Mo33-Te)(μ2-Te2)3]4+ were investigated. Crystal data for K4.5{[Mo33-Te)(μ2-Te2)3(CN)6]I}I1.5·3H2O: space group \(P\bar 3c1\), Z = 4, a = 13.280(1), c = 23.800(3) Å, V = 3635.0(6) Å3, d calc = 3.432 g/cm3, R 1 = 0.0335, wR2 = 0.0912 for 1378 I hkl > 2 σI from 3545 measured I hkl ; for Cs3{[Mo33-Te)(μ2-Te2)3(CN)6]I}·2H2O: space group P2 1 /n, Z = 2, a= 9.650(2) , b = 22.297(5), c = 27.446(7) Å, β = 94.10(2)°, V = 5890(2) Å3, d calc = 4.273 g/cm 3, R 1 = 0.0384, wR 2 = 0.0744 for 957 I hkl > 2 σI from 3758 measured I hkl (Enraf-Nonius CAD-4 diffractometer, λMoK α, graphite monochromator). In both compounds, ionic pairs {[Mo3Te7(CN)6]I}3– with Teax...I distances of 3.358-3.676 Å are formed. In the potassium salt, the {[Mo3Te7(CN)6]I}3– anion pairs are linked by the additional Teeq⋯I short contacts of 3.460 Å into two-dimensional corrugated layers perpendicular to the c axis of the unit cell. The structure of the cesium salt is ionic with interstitial H2O molecules and double-layer closest packing of anions.

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Pervukhina, N.V., Podberezskaya, N.V., Kalinina, I.V. et al. Synthesis and Molecular and Crystal Structure of K4.5{[Mo33-Te)(μ2-Te2)3(CN)6]I}I1.5·3H2O and Cs3{[Mo33-Te)(μ2-Te2)3(CN)6]I}·2H2O. Journal of Structural Chemistry 41, 843–850 (2000). https://doi.org/10.1023/A:1004870421141

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