Russian Journal of General Chemistry, Vol. 72, No. 10, 2002, p. 1656. Translated from Zhurnal Obshchei Khimii, Vol. 72, No. 10, 2002, p. 1756.
Original Russian Text Copyright
2002 by Sharutin, Pakusina, Subacheva, Sharutina, Gerasimenko.
LETTERS
TO THE EDITOR
Synthesis and Structure
of -Peroxybis[(4-bromophenoxy)tri(p-tolyl)antimony]
V. V. Sharutin, A. P. Pakusina, O. V. Subacheva,
O. K. Sharutina, and A. V. Gerasimenko
Blagoveshchensk State Pedagogical University, Blagoveshchensk, Russia
Received November 8, 2001
Organoantimony compounds containing Sb O
O C bonds have been reported [1, 3], but only one
compound with antimony atoms intervened by peroxy
bridges is known [4]. The structure of the latter was
established by X-ray diffraction. It was shown that
four antimony atoms are bound with each other by
four oxygen and two peroxy bridges. Binuclear
antimony compounds with a peroxy group between
two antimony atoms have been unknown up to now.
are 1.999(6) and 2.03(1) , respectively. The oxygen
atoms of the peroxo group are also bound with the
antimony atoms by coordination bonds [Sb2,1 O1,2
distances are 2.605 and 2.626(5) , respectively]. The
terminal Sb O3 bond lengths are 2.093(3)
.
-Peroxybis[(4-bromophenoxy)tri(p-tolyl)anti-
mony]. To a mixture of 0.50 g of tri(p-tolyl)antimony
and 0.22 g of 4-bromophenol in 30 ml of ether,
0.22 ml of 30% aqueous hydrogen peroxide was
added, and the resulting mixture was left to stand at
20 C for 12 h. Crystals formed and were filtered off
and dried to obtain 0.48 g (65%) of compound I,
mp 132 C.
We obtained the first representative of this class of
compounds by the reaction of tri(p-tolyl)antimony
with 4-bromophenol in the presence of hydrogen
peroxide (reagent molar ratio 2:2:3) in ether.
2p-Tol3Sb + 2HOC6H4Br-4 + 3H2O2
p-Tol3Sb(OC6H4Br-4)OOSb(OC6H4Br-4)(Tol-p)3
+ 4H2O.
REFERENCES
1. Starikova, Z.A., Shchegoleva, T.M., Trunov, V.K., and
Pokrovskaya, I.E., Kristallografiya, 1978, vol. 23, no. 5,
pp. 969 973.
As tri(p-tolyl)antimony was consumed (reaction
progress was followed by TLC), colorless crystals of
-peroxybis[(4-bromophenoxy)tri(p-tolyl)antimony]
(I) formed (isolable yield 64%).
2. Starikova, Z.A., Shchegoleva, T.M., Trunov, V.K., and
Pokrovskaya, I.E., Kristallografiya, 1979, vol. 24, no. 6,
pp. 1211 1216.
According to preliminary X-ray diffraction data,
the antimony atoms in compound I have the configura-
tion of trigonal bipyramid. The molecule is centro-
symmetric, and the symmetry center is located in the
midpoint of the O O bond. The two antimony atoms
are bound with each other by a peroxy group dis-
ordered by two positions. The Sb O1,2 bond lengths
3. Pokrovskaya, I.E., Dodonov, V.A., Starikova, Z.A.,
Kanunnikova, E.N., Shchegoleva, T.M., and Lebede-
va, G.P., Zh. Obshch. Khim., 1981, vol. 51, no. 6,
pp. 1247 1253.
4. Breunig, H.J., Kruger, T., and Lork, E., Angew. Chem.
Int. Ed. Engl., 1997, vol. 36, no. 6, p. 615.
1070-3632/02/7210-1656$27.00 2002 MAIK Nauka/Interperiodica
Sharutin
