Vo. Gel'Mbol'Dt et al., Synthesis and structure of the [(18C6) center dot (H3O)(2)(Hf2F10 center dot 2H(2)O)center dot 4H(2)O] complex, RUSS J IN C, 46(11), 2001, pp. 1666-1673
The complex [(18C6) (.) (H3O)(2)(Hf2F10 (.) 2H(2)O) (.) 4H(2)O] was synthes
ized and characterized by X-ray diffraction analysis, IR spectroscopy, and
thermogravimetry. The crystals are triclinic: a = 7.932(3) Angstrom, b = 8.
808(3) Angstrom, c = 11.703(3) Angstrom, alpha = 86.47(2)',degrees beta = 8
7.31(2)degrees, gamma= 64.31(2)degrees, Z = 1, space group P (1) over bar I
n the crystal structure, the 18C6 molecules, the water molecules, the diaqu
adecafluorodihafnium anions, and hydroxonium cations are combined by a syst
em of hydrogen bonds to give a three-dimensional framework. The macrocycle
in the complex acquires a conformation close to D-3d. Thermolysis of the co
mplex occurs stepwise and is accompanied by dehydration and dehydrofluorina
tion.