SYNTHESES, PROPERTIES AND CRYSTAL-STRUCTURES OF IONIC [AL-2(MU,ETA(2)-THFFO)(2)(ETOH)(4)CL-2]CL-2, [AL-3(MU,ETA(2)-THFFO)(4)CL-4][ALETCL3] AND TETRANUCLEAR [AL-4(MU,ETA(2)-THFFO)(4)(MU-OET)(2)CL-6] (THFFO = OCH2CH(CH2)(3)O) COMPOUNDS
P. Sobota et al., SYNTHESES, PROPERTIES AND CRYSTAL-STRUCTURES OF IONIC [AL-2(MU,ETA(2)-THFFO)(2)(ETOH)(4)CL-2]CL-2, [AL-3(MU,ETA(2)-THFFO)(4)CL-4][ALETCL3] AND TETRANUCLEAR [AL-4(MU,ETA(2)-THFFO)(4)(MU-OET)(2)CL-6] (THFFO = OCH2CH(CH2)(3)O) COMPOUNDS, Journal of organometallic chemistry, 553(1-2), 1998, pp. 379-385
The furyloxo-O,O')tetraethanoldichlorodialuminium(III) dichlorate [Al-
2(mu,eta(2)-thffo)(2)(EtOH)(4)Cl-2]Cl-2 (1), tetra-mu- trahydrofurylox
o-O,O')tetrachlorotrialuminium(III) trichloroethylo aluminate(III) dic
hloromethane(1/1), [Al-3(mu,eta(2)thffo)(4)Cl-4][AlEtCl3] . CH2C2 (2)
salts are synthesized in direct reaction of AlCl3(THF)(2) with Nathffo
and AlEtCl2 with thffo in THF or benzene, respectively. The addition
of AlCl3(THF)(2) to the Mg(thffo)(2) results in the formation of tetra
kis-mu-(2-tetrahydrofuryloxo-O,O') di-mu-ethoxo-hexachlorotetraalumini
um(III) tetrahydrofuran (1/1) [Al-4(mu,eta(2)-thffo)(4)(mu-OEt)(2)Cl-6
] . THF (3) species. Compound 1 crystallized in the space group P2(1)/
n, with a = 8.615(2), b = 16.445(3), c = 10.052(2) Angstrom and beta =
90.53(3)degrees. Compound 2 belongs to the C2/c space group with a =
32.046(5), b = 14.255(3), c = 15.443(3) Angstrom and beta = 123.85(3)d
egrees. Crystals of 3 are triclinic, space group P (1) over bar, a = 1
0.365(2), b = 10.854(2), c = 11.880(3) Angstrom and alpha = 70.40(2),
beta = 65.19(2), gamma = 80.18(2)degrees. The centrosymmetric cation o
f the salt 1, in the crystalline state is a dimer composed of two octa
hedra related by a crystallographic inversion centre and sharing an ed
ge. The [Al-3(mu,eta(2)-thffo)(4)Cl-4](+) cation of the species 2 is a
centrosymmetrical with an aluminium-oxygen framework, which consists
of the central octahedral atom linked to two five-coordinate aluminium
sites by mu-alkoxo bridges. The structure of 3 includes two five-coor
dinate and two six-coordinate Al atoms linked by mu-alkoxo bridges to
form tetranuclear chains with a symmetry center. (C) 1998 Elsevier Sci
ence S.A.