SYNTHESIS AND X-RAY STRUCTURES OF [H3O-CROWN-6]N [MCL4(N-)] - (M=FE, N=1, M=CO, N=2) - COMPOUNDS WHICH FORM LIQUID CLATHRATES WITH AROMATICSOLUTIONS(.18)

The title compounds, [H3O+ . 18-crown-6][FeCl4-1 (1), and [H3O+ . 18-c rown-6]2[CoCl42-] (2), were prepared by air oxidation of Fe(CO)5 for 1 , and CO2(CO)8 for 2, in the presence of 18-crown-6, H2O and HCl(g) in toluene. Liquid clathrates formed immediately for both species: 1.4.3 C7H8 and 2.3.7 C7H8. 1 crystallizes in the orthorhombic space group P 2(1)ma with a = 10.357(1), b = 11.824(1), c = 8.961 (1) angstrom, and D(c) = 1.46 g cm-3 for Z = 2. Refinement based on 935 observed reflect ions led to a final R value of 0.089. 2 crystallizes in the monoclinic space group C2/c with a = 16.225(1), b = 11.522(1), c = 20.136(1) ang strom, beta = 97.75(2)-degrees, and D(c) = 1.37 g cm-3 for Z = 4. Refi nement based on 1322 observed reflections led to a final R value of 0. 11.