2
12
VORONKOV et al.
+
+
+
EXPERIMENTAL
Cl) , 144 (8) (M 2Cl) , 109 (44) (M 3Cl) ], di-
methyl disulfide [mass spectrum, m/e (I, %): 94 (100)
1
+
+
The IR spectra (4000 400 cm ) of liquid DMSO
M , 79 (60) (M Me) , 64 (12), 61 (15), 45 (65)],
dimethyl sulfoxide [mass spectrum, m/e (I, %): 78
(74) M , 63 (100) (M Me) , 45 (35)], and chloro-
methyl methyl sulfide [mass spectrum, m/e (I, %): 96
(62) M , 81 (3) (M Me) , 61 (100) (M Cl) , 47
(12) (M CH Cl) , 45 (50)].
and GeCl (in thin films) and crystalline GeCl4
DMSO (in KBr pellets and Nujol) were recorded on
4
+
+
2
a Specord IR-75 spectrometer using KBr glasses. The
1
+
+
+
low-frequency spectra (600 200 cm ) were measured
on a Specord M-82 spectrometer using CI glasses and
polyethylene plates (for liquid samples and Nujol
mulls).
+
2
The solid residue [found, %: C 36.88; H 7.80; S
2.29] contained polyoxymethylene [ (COC) 920,
(COC) 1080 cm ] and dimethyl sulfone [ (SO )
1150,
1
s
1
Gas chromatography was performed on a Tsvet-
00 chromatograph using a 1000 0.5-mm column
as
s
2
1
5
(SO ) 1320 cm ] [11].
as
2
packed with SE-30 (5%) on Chromaton. The rate of
carrier gas (He) was 12 cm /min. The injector tempera-
3
REFERENCES
ture was 260 C, and the detector (katharometer) tem-
perature was 240 C. The column temperature was
linearly programmed from 50 to 220 C at a rate of
1
. Basenko, S.V., Gebel’, I.A., Voronkov, M.G., Kly-
ba, L.V., and Mirskov, R.G., Zh. Obshch. Khim., 1998,
vol. 68, no. 2, pp. 341 342.
1
0 C/min.
2
3
4
5
. Langer, H.G. and Blut, A.H., J. Organomet. Chem.,
Gas chromatography mass spectrometry was per-
1
966, vol. 5, no. 3, pp. 288 291.
formed on an LKB-2091 GC MS system (ionizing
voltage 60 V) using a 38-m SB-5 capillary column.
The column temperature was programmed at a rate of
. Horrocks, W.D., Jr., and Cotton, F.A., Spectrochim.
Acta, 1961, vol. 17, no. 2, pp. 134 147.
. Cotton, F.A., Francis, R., and Horrocks, W.D., Jr.,
J. Phys. Chem., 1960, vol. 64, no. 10, pp. 1534 1536.
1
6 C/min to 270 C. Accelerating voltage 2.33 kV.
Injector temperature 280 C.
. Nakamoto, K., Infra-Red and Raman Spectra of In-
organic and Coordination Compounds, New York:
Wiley, 1986.
Complex of tetrachlorogermane with dimethyl
sulfoxide 2(Me SO) GeCl (I). Tetrachlorogermane,
2
4
2
1.4 g, was added dropwise with stirring over the
course of 10 min to 15.6 g of dimethyl sulfoxide in
00 ml of methylene chloride. A precipitate formed
6
7
. Gur’yanova, E.N., Gol’dshtein, I.P., and Romm, I.P.,
Donorno-aktseptornaya
svyaz’
(Donor-Acceptor
1
Bond), Moscow: Khimiya, 1973.
and was filtered off and dried in a vacuum (10 mm) to
obtain 36.9 g (99%) of complex I, mp 136 C. Found,
. Beattie, I.R., Gilson, T.R., and Ozin, G.A., J. Chem.
Soc. A, 1968, no. 11, pp. 2772 2778.
%
: C 12.88; H 3.18; Cl 38.12; Ge 19.41; S 17.19.
C H Cl GeO S . Calculated, %: C 12.96; H 3.26; Cl
8. Beattie, I.R. and Ozin, G.A., J. Chem. Soc. A, 1970,
4
12
4
2 2
3
8.26; Ge 19.58; S 17.30.
no. 3, pp. 370 377.
9
. Goldstein, M. and Unsworth, W.D., Spectrochim.
Acta, Part A, 1972, vol. 28, no. 7, pp. 1297 1304.
Thermolysis of complex I. Complex I, 3.7 g, was
slowly heated at atmospheric pressure under dry argon.
At the bottoms temperature 165 210 C, a fraction
distilled (1.3 g) with bp 80 175 , which, according to
GC MS data, contained tetrachlorogermane [mass
1
0. Raotz, R.F.W. and Sweeting, O.J., J. Org. Chem.,
963, vol. 28, no. 6, pp. 1612 1616.
1
11. Smit, A., Applied Infared Spectroscopy, New York:
+
spectrum, m/e (I, %): 214 (22) M , 179 (100) (M
Wiley, 1979.
RUSSIAN JOURNAL OF GENERAL CHEMISTRY Vol. 71 No. 2 2001