Dw. Vongudenberg et al., THE CRYSTAL-STRUCTURES OF (NH4)(2)[RECL6] , [RECL2(CH3CN)(4)](2)[RECL6]CENTER-DOT-2CH(3)CN AND [RECL4(18-CROWN-6)], Zeitschrift fur anorganische und allgemeine Chemie, 621(4), 1995, pp. 525-530
Citations number
18
Categorie Soggetti
Chemistry Inorganic & Nuclear
Journal title
Zeitschrift fur anorganische und allgemeine Chemie
Brown single crystals of (NH4)(2)[ReCl6] are formed by the reaction of
NH4Cl with ReCl5 in a suspension of diethylether. [ReCl2(CH3CN)(4)](2
)[ReCl6] . 2CH(3)CN crystallizes as brown crystal plates from a soluti
on of ReCl5 in acetonitrile. Lustrous green single crystals of [ReCl4(
18-crown-6)] are obtained by the reaction of 18-crown-6 with ReCl5 in
a dichloromethane suspension. All rhenium compounds are characterized
by IR spectroscopy and by crystal structure determinations. (NH4)(2)[R
eCl6]: Space group Fm $($) over bar$$ 3m, Z = 4, 75 observed unique re
flections, R = 0.01. Lattice constant at -70 degrees C: a = 989.0(1) p
m. The compound crystallizes in the (NH4)(2)[PtCl6] type, the Re-Cl di
stance is 235.5(1) pm. [ReCl2(CH3CN)(4)](2)[ReCl6] . 2CH(3)CN: Space g
roup P $($) over bar$$ 1, Z = 1,2459 observed unique reflections, R =
0.12. Lattice dimensions at -60 degrees C: a = 859.0(1), b = 974.2(7),
c = 1287.3(7) pm, alpha = 102.69(5)degrees, beta = 105.24(7)degrees,
gamma = 102.25(8)degrees. The structure consists of two symmetry-indep
endent [ReCl2(CH3CN)(4)](+) ions with trans chlorine atoms, [ReCl6](2-
) ions, and included acetonitrile molecules. In the cations the Re-Cl
bond lengths are 233 pm in average, in the anion they are 235 pm in av
erage. [ReCl4(18-crown-6)]: Space group P2(1)/n, Z = 4, 3633 observed
unique reflections, R = 0.06. Lattice dimensions at -70 degrees C: a =
1040.2(4), b = 1794.7(5), c = 1090.0(5)pm, beta = 108.91(4)degrees. T
he compound forms a molecular structure, in which the rhenium atom is
octahedrally coordinated by the four chlorine atoms and by two oxygen
atoms of the crown ether molecule.