Russian Journal of General Chemistry, Vol. 72, No. 3, 2002, pp. 392 393. Translated from Zhurnal Obshchei Khimii, Vol. 72, No. 3, 2002,
pp. 421 422.
Original Russian Text Copyright
2002 by Sharutin, Sharutina, Pakusina, Platonova, Bel’skii.
Synthesis and Structure of Tri(p-tolyl)antimony Dichloride
V. V. Sharutin, O. K. Sharutina, A. P. Pakusina, T. P. Platonova, and V. K. Bel’skii
Blagoveshchensk State Pedagogical University, Blagoveshchensk, Russia
Received July 18, 2000
Abstract Tri(p-tolyl)antimony dichloride was prepared by oxidation of tri(p-tolyl)stibine with chlorine
or copper(II) chloride. As found by X-ray diffraction analysis, the antimony atom in tri(p-tolyl)antimony
dichloride has the configuration of trigonal bipyramid with axially located chlorine atoms. The Sb Cl and
Sb C distances are 2.476(2) and 2.104(7) , and the CSbC and ClSbCl angles are 120 and 180 , respectively.
The structure of phenyl derivatives of pentavalent
antinmony of the general formula Ph SbX , where X
3
2
is an electronegative substituent, has been described in
1, 2]. The majority of compounds of this type feature
[
trigonal-bipyramidal coordination of the central atom
with the electronegative ligands in the axial positions.
In triphenylantimony dichloride, the hydrogen and
carbon atoms of one of the phenyl groups come close
to chlorine atoms inspite of the developing steric
hindrances [3]. An analogous contact is observed in
tri(m-tolyl)antimony dichloride, where the distance
between the equatorial carbon atom of one of the
phenyl groups and the chlorine atom (3.188 , [4]) is
also shorter than the sum of the van der Waals radii
C1
C2
Cl1
C3
C4
of C and Cl (3.25
[5]).
C5
To find out the reasons for nonbonded C Cl inter-
actions in compounds of this type, we have studied
the structure of tri(p-tolyl)antimony dichloride (I).
Earlier for this compound crystal lattice parameters
were only reported [6]. The general view of the mo-
lecule is presented in the figure. The coordinates of
non-hydrogen atoms are listed in Table 1, and the
principal interatomic distances and bond angles, in
Table 2.
General view of the molecule of compound I.
gonal-bipyramidal coordination. The corresponding
interatomic distances are 2.4617, 2.4793, and 2.101,
2.112, and 2.116
.
Hence, para-methyl substituents in the aryl rings
favor increased molecular symmetry of triarylanti-
mony dichloride. Because of the molecular symmetry
According to X-ray diffraction data, the antimony
atom in compound I has trigonal-bipyramidal coordi-
Table 1. Atomic coordinates ( 10 4 ) and equivalent
isotropic thermal parameters (B 10 , ) in the molecule
3
2
nation with axial tolyl groups and axial chlorine atoms. of compound I
The molecular symmetry is D . Contrary to tri(m-
3
tolyl)antimony dichloride, where the Cl Sb Cl angle
is 177.2 , in tri(p-tolyl)antimony dichloride the loca-
tion of these atoms is linear (the corresponding angle
is 180 ). The antimony atom lies strictly in the equa-
torial plane. All the phenyl ring planes form the same
angles with the equatorial plane (37.9 ) and with each
other (64.2 ). The Sb Cl distances are equal to each
other [2.476(2) ], and the same is true of the Sb C
distances [2.104(7) ]. Note that the antimony atom
in tri(m-tolyl)antimony dichloride has a distorted tri-
Atom
x
y
z
B
Sb
1250
127(1)
1250
1250
127(1)
61(1)
83(1)
62(2)
79(1)
81(2)
67(2)
95(3)
1
Cl
C
C
C
C
C
127(1)
1250
324(4)
336(4)
1250
1250
1
81(4)
346(5)
1098(5)
1476(4)
2297(5)
2419(4)
2774(5)
3552(5)
3976(4)
4797(5)
2
3
4
5
1
070-3632/02/7203-0392$27.00 2002 MAIK Nauka/Interperiodica
Sharutin
