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(C
2
F
x
Br
0.01
·
y
CH
3
CN)
n
intercalation compounds, with (C
2
F
x
Br
0.01
)
n
(0.5 <
x
< 1.0) as a host and CH
3
CN as a guest (
x
and
y
are stoichiometric coefficients), have been synthesized. The influence of fluorine content on the spectroscopic characteristics of the intercalation compounds with acetonitrile has been studied by Raman, IR, and X-ray photoelectron spectroscopies. The macroscopic properties of the intercalation compounds are shown to correlate with their spectroscopic characteristics. The data for the compounds stored in air for about a year indicate that their surface and interior differ in structure.