676
Russ.Chem.Bull., Int.Ed., Vol. 62, No. 3, March, 2013
Mironov et al.
Scheme 2
C(102a,b)—C(103a,b) bonds point in opposite directions
from the planes of the ligands, whereas the azido groups
are directed toward these planes.
Most of the refined atomic displacement parameters
Uiso are common for such compounds at room temperaꢀ
2
ture and have similar values (0.046(3) Å for the heavy
2
atoms and 0.044(5) Å for the ligand). The exception is
the atomic displacement parameter for the azidoalkyl
2
group (0.106(7) Å ). The high value of the latter parameꢀ
ter suggests that this substituent is disordered over several
positions. However, it was impossible to refine these posiꢀ
tions from the Xꢀray powder diffraction data.
The crystal structure has a molecular packing. The
only relatively short contact between the Cl(1a) atom and
the hydrogen atom H(106a) is 2.81(2) Å.
Reagents: CuCl •2H O, CH Cl /MeOH.
2
2
2
2
Additional crystallographic data on the structure are
available from the Cambridge Crystallographic Data Cenꢀ
tre (CCDC 921946).
the singleꢀcrystal Xꢀray diffraction data for the related
compound (compound 4). The results of the present study
are in rather good agreement with the singleꢀcrystal Xꢀray
data even for pairs of light atoms (C—N bonds), which are
always determined with low accuracy due to the specificiꢀ
ty of the method. The corresponding bond lengths and
bond angles in both compounds are equal within 3. The
S atoms and the first C atoms of the azidoalkyl group
lie nearly in the plane of the fiveꢀmembered ring; the
maximum deviation is observed for the C(102a) atom
†
We thank Yu. D. Seropegin for help in performing the
experiment.
This study was financially supported by the Russian
Foundation for Basic Research (Project Nos 10ꢀ03ꢀ00992a
and 12ꢀ04ꢀ00988a).
References
(
0.31(4) Å), whereas the deviations for the other atoms
1
2
. I. A. Koval, P. Gamez, C. Belle, K. Semeczi, J. Reedijk,
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Structure 3 is typical of such copper coordination comꢀ
pounds. The molecule has a propellerꢀshaped conformaꢀ
tion. Almost planar ligands are rotated with respect to
each other by 53.56(17). The coordination polyhedron of
the copper atom can be described as a distorted tetragonal
pyramid (taking into account the second copper atom). It
should be noted that the chain of atoms N(16a)—Cu(1a)—
Cu(2a)—N(16b) is not linear. It is slightly bent toward
the chlorine atom Cl(1a). The structure is almost symꢀ
metric with respect to a twofold axis passing through the
midpoint of the Cu—Cu bond and the chlorine atom.
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5
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7
8
. E. K. Beloglazkina, S. Z. Vatsadze, A. G. Majouga, N. A.
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2
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Angle
/deg
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2. M. Leoni, Ch. 10: Novye rentgenovskie difraktsionnye metody
analiza mikrostruktury i morfologii nanokristallicheskikh poꢀ
roshkov [New Xꢀray Diffraction Methods of Analysis of the
Microstructure and Morphology of Nanocrystalline Powders],
3
4*
1
1
1
Cu(1a)—Cl(1a)—Cu(2a)
N(16a)—Cu(1a)—S(2)
N(16a)—Cu(1a)—Cu(2a)
N(16a)—Cu(1a)—Cl(1a)
N(15a)—Cu(1a)—Cl(1a)
63.1(6)
97.6(5)
160.3(7)
103.5(7)
109.2(7)
62.68(5)
96.42(15)
164.04(14)
102.58(15)
105.37(14)
*
Singleꢀcrystal Xꢀray diffraction data for the earlier studꢀ
ied compound 4 structurally similar to compound 3
are given.
†
Deceased.