ISSN 0036ꢀ0236, Russian Journal of Inorganic Chemistry, 2014, Vol. 59, No. 10, pp. 1119–1122. © Pleiades Publishing, Ltd., 2014.
Original Russian Text © V.V. Sharutin, O.K. Sharutina, 2014, published in Zhurnal Neorganicheskoi Khimii, 2014, Vol. 59, No. 10, pp. 1356–1359.
COORDINATION COMPOUNDS
Phenylbismuth Bis(2,5ꢀdimethylbenzenesulfonate):
Structure and Properties
V. V. Sharutin and O. K. Sharutina
National South Ural State Research University, pr. Lenina 76, Chelyabinsk, 454080 Russia
eꢀmail: vvsharutin@rambler.ru
Received February 17, 2014
Abstract—Phenylbismuth bis(2,5ꢀdimethylbenzenesulfonate) (I), a coordination polymer in which a bisꢀ
muth atom has a distorted square pyramidal coordination to an axial carbon atom (Bi–C, 2.247(5) Å) and
basal oxygen atoms (Bi–O, 2.390(9)–2.403(10) Å), has been synthesized by the reaction between triphenylꢀ
bismuth and 2,5ꢀdimethylbenzenesulfonic acid (1 : 2 mol/mol) in toluene and structurally characterized.
Pentaphenylbismuth and pentaphenylantimony phenylate compound I to triphenylbismuth.
DOI: 10.1134/S0036023614100179
Molecules of tricoordinated bismuth derivatives
(bismuth in s2p3 electron configuration) have a pyraꢀ
midal arrangement of three bonds with the lone pair
Reaction between compound I and pentaphenylbisꢀ
muth. A mixture of compound (0.100 g, 0.15 mmol)
I
and pentaphenylbismuth (0.180 g, 0.30 mmol) in tolꢀ
uene (5 mL) was stirred for 1 h at 20°C. The solvent
was removed, and the residue was dissolved in hot
water (20 mL) and filtered out, to obtain, after evapoꢀ
ration of water, 0.204 g (93%) of tetraphenylbismuth
2,5ꢀdimethylbenzenesulfonate crystal hydrate with
on the bismuth atom. The involvement of d orbitals in
bonding increases the coordination number of the bisꢀ
muth atom and gives rise to the polymorphism of bisꢀ
muth(III) compounds, which tend to the formation of
dimers and polymers. Most of the described structures
of dimers and polymers do not contain Bi–C bonds
[1–5], and only some of them are organoelemental
compounds [6–8].
Tm = 177°C. A sample of the latter in a mixture with
tetraphenylbismuth 2,5ꢀdimethylbenzenesulfonate
crystal hydrate [9] melted without depression. Tripheꢀ
nylbismuth (0.06 g, 90%) was separated out from the
waterꢀinsoluble residue by extraction with benzene
The objective of this work was to synthesize pheꢀ
nylbismuth bis(2,5ꢀdimethylbenzenesulfonate) (I)
and to highlight features of its structural and chemiꢀ
cal behavior.
(2
×
10 mL).
The reaction between compound
I
and pentapheꢀ
nylantimony was performed in a similar fashion.
EXPERIMENTAL
IR spectrum was recorded on a Bruker Tensor 27 IR
Synthesis of phenylbismuth bis(2,5ꢀdimethylbenzeꢀ
nesulfonate) (I). A mixture of triphenylbismuth (0.200 g,
0.45 mmol) and 2.5ꢀdimethylbenzenesulfonic acid
(0.170 g, 0.90 mmol) in toluene (5 mL) was allowed to
spectrometer as KBr pellets.
Xꢀray diffraction analysis of a crystal of compound
was performed on a Bruker D8 QUEST diffractometer
Mo radiation, = 0.71073 Å, graphite monochroꢀ
I
(
K
λ
stand for 1 h at 90
°
С and cooled, thereupon the
α
mator). The collection and edition of data, the refineꢀ
ment of unit cell parameters, and the application of
absorption corrections were performed by the
SMART and SAINTꢀPlus software [10]. All calculaꢀ
tions in the solution and refinement of the structure
were performed by the SHELXL/PC software [11].
formed crystals were filtered out and dried. Colorless
crystals of compound
219°C were obtained.
I (0.280 g, 94%) with Tdec =
IR spectrum (
, cm–1): 3448, 3048, 2981, 2921,
ν
1494, 1476, 1430, 1383, 1329, 1282, 1232, 1178, 1101,
1076, 1003, 816, 728, 704, 690, 618, 591, 555, 516,
451, 439.
The structure of compound
I was solved by direct
methods and refined by the leastꢀsquare technique in
the anisotropic approximation for nonꢀhydrogen
atoms. Selected crystallographic data and refinement
For C22H23O6S2Bi, anal. calcd. (%): C 40.24; H,
3.50.
Found (%): C, 39.98; H, 3.64.
details for the structure of compound I are listed in
1119
Sharutin
