The structures of X2[(Mo6Cl8)Cl6]·nH2O, X=NH4, K, Rb, Cs
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Introduction
This study is part of an ongoing project that deals with supramolecular compounds based on the Mo6Cl142− cluster and derivatives thereof. The Mo6Cl142− entity shows remarkable stability, and may be handled as a building block for extended molecular assemblies from solution as well as in solid state reaction. Together with cations containing hydrogen it has a propensity for remarkably strong and rigid hydrogen bonded networks [1], [2]. The similarities in the hydrogen bonding motif are remarkable even when structures containing counterions of different size are used.
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Synthesis
MoCl2 was synthesized from MoCl5 and Mo metal [3]. (NH4)2[(Mo6Cl8)Cl6]·H2O was synthesized from a mixture (1:1 vol) of a hot saturated solution of (H3O)2[(Mo6Cl8)Cl6]·7H2O and NH4Cl in 2M HCl. Yellow tabular crystals precipitated after slow cooling to room temperature. K2[(Mo6Cl6]·H2O was synthesized by dissolving (H3O)2[(Mo6Cl8)Cl6]·7H2O and KCl in hot 1M HCl. Slow cooling to room temperature yielded yellow needle-shaped crystals. Rb2[(Mo6Cl8)Cl6]·H2O and Cs2[(Mo6Cl8)Cl6]·3H2O were synthesized
Results and discussion
Fractional atomic coordinates for the four compounds are given in Table 2a, Table 2b, Table 2c, Table 2d. Since hydrogen positions are calculated, ESD's are not applicable. Isotropic displacement parameters for the calculated positions where determined, and for these ESD's are given. As in all known compounds containing the Mo6Cl142− unit, this entity is highly regular with MoMo distances close to 2.6 Å and MoCl distances around 2.5 Å. The Mo6Cl142− cluster has a coordination from H2O
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