Russian Journal of Coordination Chemistry, Vol. 28, No. 11, 2002, pp. 753–757. Translated from Koordinatsionnaya Khimiya, Vol. 28, No. 11, 2002, pp. 803–808.
Original Russian Text Copyright © 2002 by Sharutin, Pakusina, Platonova, Egorova, Sharutina, A. Gerasimenko, Sergienko, E. Gerasimenko.
Synthesis and Structure of Tetraphenylantimony 2-Furoinate
and Benzoate
V. V. Sharutin, A. P. Pakusina, T. P. Platonova, I. V. Egorova, O. K. Sharutina,
A. V. Gerasimenko, A. S. Sergienko, and E. A. Gerasimenko
Blagoveshchensk State Pedagogical University, ul. Lenina 104, Blagoveshchensk, 675000 Russia
Institute of Chemistry, Far East Division, Russian Academy of Sciences,
pr. Stoletiya Vladivostoka 159, Vladivostok, 690022 Russia
Received May 25, 2001
Abstract—Tetraphenylantimony 2-furoinate Ph4SbOC(O)C4H3O is synthesized by the reaction of pentaphenyl-
antimony with triphenylantimony bis(2-furoinate). The structure of the compound is determined by X-ray dif-
fraction analysis. The Sb atom in the compound has a distorted trigonal-bipyramidal coordination with the phe-
nyl and 2-furoinate groups in the axial positions. The Sb(1)–C(Ph)eq distances lie in the 2.119(1)–2.121(1) Å
interval; the Sb–O(1) and Sb–C(Ph)ax bond lengths are equal to 2.273(1) and 2.161(1) Å, respectively; and the
Sb(1)···é(2) intramolecular contact is 3.234(1) Å.
INTRODUCTION
Tetraphenylantimony benzoate was synthesized
similarly.
In the majority of antimony compounds with the
general formula Ar4Sbï (X is an organic or inorganic
X-ray diffraction analysis of crystals I and II was
ligand), the Sb atom has the trigonal bipyramid config- performed on a SMART-1000 CCD automated diffrac-
uration with coordination number (CN) 5 [1]. However, tometer (Bruker). The data for compound I were col-
when the ligands contain potential coordination sites, lected in sets of 606, 435, and 230 frames at the angle
they can additionally interact with the Sb atom. As a ϕ = 0°, 90°, and 180°, respectively (ω scan mode with an
result, a coordination environment of the Sb atom with increment of 0.3° and exposure of 10 s per frame for
CN 6 can be realized. For example, most tetraarylanti- compound I and 20 s per frame for compound II).
mony acylates [2–8] exhibit shortened Sb···O distances
The structures were determined by the direct
as compared to the sum of van der Waals radii, thus
method and refined by the least-squares method in the
indicating an additional coordination of the Sb atom in
anisotropic approximation for all non-hydrogen atoms.
these compounds.
The positions of hydrogen atoms were calculated geo-
In continuation of our studies on the structures of
tetraphenylantimony acylates [2–8], we examined the
molecular and crystal structures of tetraphenylanti-
mony 2-furoinate (I) and tetraphenylantimony ben-
zoate (II), which are antimony derivatives that differ
only in the nature of the arene ring of the carboxylic
acid. The structure of compound II determined with
lower accuracy than in the present work, was reported
in [8].
metrically and included in the refinement by the “rider”
model.
The data collection and editing and the refinement
of the unit cell parameters were performed using the
SMART and SAINT-Plus program packages [9]. All
calculations for determination and refinement of the
structures were performed using the SHELXTL/PC
program package [10].
The main crystallographic data and results of refine-
ment of the structures are presented in Table 1. The
1
EXPERIMENTAL
atomic coordinates are presented in Table 2, and the
bond lengths and angles are given in Table 3.
Synthesis of tetraphenylantimony 2-furoinate was
carried out in an evacuated glass tube as follows. Pen-
taphenylantimony (1.00 g, 1.97 mmol) and triphenylan-
timony bis(2-furoinate) (1.13 g, 1.96 mmol) in toluene
(10 ml) were heated at 90°ë for 1 h. The solvent was
removed, and the residue was recrystallized from a ben-
zene–heptane (3 : 1) mixture. The complex was
obtained in 96% yield (2.05 g), mp 166°C.
RESULTS AND DISCUSSION
Compounds I and II were synthesized by the dispro-
portionation of pentaphenylantimony and triphenylan-
timony diacylates in toluene at 90°ë. The reaction was
IR (ν, cm–1): 1630 vs, 1395 vs, 1180 vs, 1125 s,
1060 vs.
1
The coordinates of hydrogen atoms and their thermal isotropic
parameters can be made available by the authors.
1070-3284/02/2811-0753$27.00 © 2002 åÄIä “Nauka /Interperiodica”
Sharutin
