Abstract
The crystal structures of three series of clathrate compounds with organic guest molecules G have been determined, Cd(CN)2·G, [CdM(CN)4]·2G (M = Hg or Zn) and [NMe4·G][CuM(CN)4](M = Cd or Zn). The cubic Fdmunit-cell parameter for the first series (Z= 8) ranges from 12.647(6)A for G = CHCl3 to 12.767(2)A for CCl3CF3, depending on the molecular size and orientation of the guest in the cavity. In the second series the space group Fdm is unchanged upon 50% substitution of Cd in the first with Hg or Zn owing to the random distribution of the tetrahedral centres; the lattice parameter varies little when M = Hg, but when M = Zn a= 12.243(2)A, a decrease of 0.5 A from the value for Cd(CN)2·CCl4. The anionic host in the third series accommodates the NMe4+ guest together with neutral CCl4; the lattice parameter of the cubic F3munit cell decreases by ca. 0.6 A in comparison with the values in the first two series. The X-ray data for 24 single crystals are discussed in terms of the crystallographic discrimination between C and N of the linking CN groups and the orientation of the guest molecules, in particular of the tetrahedral and pseudo-tetrahedral guest molecules, in the cavity approximating to a tetrahedron.
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