Generation of nitrosyl сhloride in AgNO2—SOCl2
Russ.Chem.Bull., Int.Ed., Vol. 54, No. 9, September, 2005
2149
C(1), compound 11), 51.7 (CN, compound 12), 51.75 (CN,
compound 11), 64.2 (CCl, compound 12), 66.2 (CCl, comꢀ
pound 11), 169.0 (C=O). IR, ν/cm–1: 3280 (NH bond), 1640
(C=O), 1560 (NH). MS of 11 (EI, 70 eV), m/z (Irel (%)): 190
(1.6), 189 [M + 2]+ (5.0), 188 (4.9), 187 [M]+ (16.9), 86 (45.6),
85 (100), 67 (34.7), 45 (32.6), 44 (96.7). MS of 12 (EI, 70 eV),
m/z (Irel (%)): 190 (0.4), 189 [M + 2]+ (4.9), 188 (2.6), 187 [M]+
(14.5), 152 (15.3), 110 (11.2), 86 (100), 85 (84.8), 67 (53.1), 45
(57.8), 44 (75.9).
Xꢀray diffraction study of 7. Crystals of compound 7 suitable
for Xꢀray diffraction study were grown as colorless prisms of
dimensions 0.85×0.45×0.20 mm by slow evaporation from a
solution in chloroform. Xꢀray diffraction data were collected on
a SyntexꢀP1 diffractometer (MoꢀKα radiation). The structure
was solved by direct methods and refined by the fullꢀmatrix
leastꢀsquares method against F2 with anisotropic displacement
parameters for nonhydrogen atoms. The hydrogen atoms were
located from difference Fourier maps and refined isotropically.
All calculations were carried out using the SHELXL97 program
package.22 The atomic coordinates for the structure of 7 and the
complete tables of the bond lengths and bond angles were deꢀ
posited with the Cambridge Structural Database. Selected bond
lengths and bond angles are given in Table 2. Crystallographic
data, details of Xꢀray data collection, and characteristics of strucꢀ
ture refinement are listed in Table 3.
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This study was financially supported by the Russian
Foundation for Basic Research (Project No. 02ꢀ03ꢀ
33347), the Foundation "Russian Universities" (Grant
05.03.046), and the Russian Academy of Sciences (Proꢀ
gram of the Chemistry and Materials Science Division
"Theoretical and Experimental Studies of the Nature of
Chemical Bonds and Mechanisms of Important Chemiꢀ
cal Reactions and Processes").
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References
22. G. M. Sheldrick, SHELXL97. Program for Crystal Strucꢀ
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and N. V. Zyk, Izv. Akad. Nauk, Ser. Khim., 2005, 2070
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Received May 19, 2005;
in revised form September 21, 2005