ANTIMONY(III) FLUORIDE - INCLUSION COMPLEXES WITH CROWN-ETHERS

Four crystalline molecular complexes between antimony(III) fluoride an d 18-membered crown ethers have been obtained and their structures inv estigated by single crystal X-ray diffraction techniques: [18-crown-6 . SbF3], C12H24F3O6Sb, P2(1)2(1)2(1), a = 8.328(4), b = 11.573(4), c = 18.094(4)Angstrom, V = 1744(1)Angstrom(3), Z = 4; [benzo-18-crown-6 . SbF3], C16H24F3O6Sb, P2(1)/n, a = 10.490(2), b = 13.714(1), c = 13.44 2(2)Angstrom, beta = 101.94(1)degrees, V = 1892(1)Angstrom(3), Z = 4; [cis-syn-cis-dicyclohexano-18-crown-6 . SbF3 . CH3OH], C21H40F3O7Sb, P 2(1)/n, a = 8.270(4), b = 23.386(3), c = 12.772(1)Angstrom, beta = 96. 31(2)degrees, V = 2455(1)Angstrom(3), Z = 4; [cis-anti-cis-dicyclohexa no-18-crown-6 . SbF3], C2OH36F3O6Sb, Pna2(1), a = 21.091(8), b = 12.82 9(5), c = 8.437(3)Angstrom, V = 2283(2)Angstrom(3), Z = 4. All species are the perching-type complexes with the antimony fluoride above the cavity and the metal lone pair pointed toward the center of the crown ring. The antimony atom interacts with all six crown oxygen atoms with Sb-O distances of 2.837(2)-3.344(2)Angstrom. The antimony atom is dis placed from the least square plane of the crown oxygen atoms at the di stances of 1.288-1.383 Angstrom.