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Synthesis, Structure, and Decomposition of (NH4)2[Mo6Cl14] · H2O

✍ Scribed by Andreas Nägele; Katharina Gibson; Abdessadek Lachgar; H.-Jürgen Meyer

Publisher
John Wiley and Sons
Year
1999
Tongue
German
Weight
106 KB
Volume
625
Category
Article
ISSN
0372-7874

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✦ Synopsis

NH 4 ) 2 [Mo 6 Cl 14 ] ´H2 O (1) was prepared from reactions of MoCl 2 in ethanol with aqueous NH 4 Cl solution. It crystallizes in the monoclinic space group I2/a (no. 15), Z = 4 with a = 912.3(1), b = 1491.2(2), c = 1724.8(2) pm, b = 92.25(1)°; R1 = 0.023 (based on F values) and wR2 = 0.059 (based on F 2 values), for all measured X-ray reflections. The structure of the cluster anion can be given as [(Mo 6 Cl i 8 )Cl a 6 ] 2± (i = inner, a = outer ligands). Thermal stability studies show that 1 loses crystal water followed by the loss of NH 4 Cl above 350 °C to yield MoCl 2 . The water-free compound (NH 4 ) 2 [Mo 6 Cl 14 ] (2) was synthesized by solid state reaction of MoCl 2 and NH 4 Cl in a sealed quartz ampoule at 270 °C. No single-crystals could be obtained. Decompositions of 1 and 2 under nitrogen and argon exhibited the loss of NH 4 Cl at about 350 °C. Decomposition under NH 3 resulted in the formation of MoN and Mo 2 N at 540 °C and 720 °C, respectively.

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