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6a-l (General Procedure)
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selenium (1.0 mmol) was stirred at 80–82°C for 4–44
h. After the reaction completion, the crude product
was purified by flash chromatography (neutral alu-
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pure products 6a–l in 88–99% yields.
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X-Ray Crystallography of 6h
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The XRD data were obtained on a Bruker Kappa
Apex II CCD diffractometer using ϕ, ω scans of
narrow (0.5°) frames with Mo Kα radiation (λ =
˚
0.71073 A) and a graphite monochromator. The
structures were solved by direct methods and refined
by the full-matrix least-squares method against all
F2 in anisotropic approximation using the SHELX-
97 programs set [37]. The H atoms positions were
calculated with the riding model. Absorption cor-
rections were applied empirically using SADABS
programs. Compound 6h is triclinic, space group
P-1, a = 7.6775(7), b = 18.006(2), c = 18.281(2)
˚
A, α = 63.802(4), β = 89.779(4), γ = 82.341(4)°,
3
˚
V = 2243.0(4) A , Z = 4, C24H27PSSe, Dc = 1.355
g/cm3, μ = 1.845 mm−1, F(0 0 0) = 944, crystal
size 0.8 × 0.60 × 0.04 mm3, independent reflections
8050, wR2 = 0.1860, S = 1.02 for all reflections (R
= 0.0754 for 4859 F > 4σ). Tables listing detailed
crystallographic data, atomic positional parameters,
and bond lengths and angles are available as CCDC
1404950 from the Cambridge Crystallographic Data
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ACKNOWLEDGMENTS
This work was supported by the President of the Rus-
sian Federation (program for the support of leading
scientific schools, grant NSh-156.2014.3). The spec-
tral data were obtained using instrumental park of
Baikal Analytical Center SB RAS.
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Heteroatom Chemistry DOI 10.1002/hc