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Figure 2 Molecular structure of 2a (p = 50%). The disordering of the CF3
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C(11)
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and C(3) atoms is not shown.
to rotation around a single bond. The (CH2)4 moiety in 2c
demonstrates conformational rigidity: the C(2) and C(3) atoms
are disordered over two positions (see Online Supplementary
Materials).
This work was supported by the Russian Foundation for Basic
Research (grant no. 19-33-50086). Crystal structure determination
was performed at the Department of Structural Studies of
N. D. Zelinsky Institute of Organic Chemistry, Moscow.
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Online Supplementary Materials
Supplementary data associated with this article can be found
in the online version at doi: 10.1016/j.mencom.2020.09.027.
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Crystal data for 2a. C12H11F3N2, M = 240.23, triclinic, space group
¯
P1, a = 6.2608(2), b = 8.2336(3) and c = 10.2971(4) Å, a = 85.4144(10)°,
b = 89.7475(10)°, g = 79.8077(10)°, V = 520.73(3) Å3, Z = 2, dcalc
=
= 1.532 g cm–3, F(000) = 248, μ(MoKa) = 0.130 mm–1, qmin = 1.98°,
qmax = 32.03°, 22692 reflections measured, 3618 independent reflections
(Rint = 0.0392), R1 = 0.0467, wR2 = 0.1071 for 2939 reflections with
I > 2s(I); R1 = 0.0618, wR2 = 0.1183 for all data, 181 parameters and
84 restraints, GOF = 1.040, rmax / rmin = 0.431 / –0.353 e Å–3.
Crystal data for 2c. C12H11N3, M = 197.24, orthorhombic, space
group Pbca, a = 7.1674(2), b = 11.8345(4) and c = 22.7718(8) Å, V =
= 1931.56(11) Å3, Z = 8, dcalc = 1.356 g cm–3, F(000) = 832,
μ(MoKa) = 0.084 mm-1, qmin = 3.36°, qmax = 31.25°, 49378 reflections
measured, 3144 independent reflections (Rint = 0.0672), R1 = 0.0467,
wR2 = 0.1096 for 2504 reflections with I > 2s(I); R1 = 0.0640, wR2 =
= 0.1234 for all data, 155 parameters and 3 restraints, GOF = 1.033,
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V. P. Gul’tyai, Mendeleev Commun., 2009, 19, 96.
37 Bruker APEX3, Bruker AXS, Madison, WI, USA, 2018.
38 L. Krause, R. Herbst-Irmer, G. M. Sheldrick and D. Stalke, J. Appl.
Crystallogr., 2015, 48, 3.
r
max / rmin = 0.336 / –0.242 e Å–3.
CCDC 1991687 and 1991688 contain the supplementary
39 G. M. Sheldrick, Acta Crystallogr., 2015, A71, 3.
40 G. M. Sheldrick, Acta Crystallogr., 2015, C71, 3.
crystallographic data for this paper. These data can be obtained free of
charge from The Cambridge Crystallographic Data Centre via http://
See Online Supplementary Materials for geometric parameters and
refinement details.
Received: 24th March 2020; Com. 20/6177
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