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An ampule reaction between Mo and PCl5 at 200 °C yielded (PCl4)2[Mo2Cl10], the first ternary compound in Mo–P–Cl system. Single crystal X-ray diffraction gave a triclinic unit cell: a = 6.870(1), b = 8.892(2), c = 9.423(2) Å, α = 100.24(2), β = 95.55(2), γ = 96.12(2)° (V = 559.3(2) Å3, Z = 1, sp. gr. P1, wR2 = 0.0575 and R1 = 0.0279. The ionic compound is built from edge sharing bioctahedra [Mo2Cl10]2– and two tetrahedra PCl4+. The averaged Mo–Clb distance, 2.503(1) Å, is longer than the Mo–Clt distance, 2.33(2) Å. The Mo … Mo distance, 3.77 Å, indicates the absence of a direct Mo–Mo interaction. Semiempirical and ab initio calculations showed the possibility for [Mo2Cl10]2– to exist with long and short Mo to Mo distances, the letter corresponding to the Mo–Mo bond. 相似文献
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