Chemistry - A European Journal
10.1002/chem.201702207
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ethylenediamine (en) and 5.0 mL H
2
O. The mixture was transferred into a
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teflon-lined stainless steel autoclave (50 mL) and heated at 145 °C for
36 hours. After the mixture was slowly cooled to room temperature,
1
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black block crystals suitable for X-ray structure determination were
obtained. The attempts to obtain compound 1 using other copper sources
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(
3 2 2 2 2
such as Cu(CH COOH) ·H O and CuCl ·2H O) were not successful
under the same conditions up to the present. The crystals were washed
with deionized water, purified ultrasonically, and air-dried to give a yield
of ca. 62% (based on CuO).
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[
Single-crystal X-ray diffraction: The crystal data (0.24 × 0.20 × 0.18 mm)
were collected on a Bruker APEX-II CCD diffractometer (Mo-Kα, λ = 0.71073
Å) at 293(2) K. A total of 14098 reflections were collected, of which 9907
1
1
reflections were unique (Rint = 0.0311). The structure was solved by the direct
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[
1536420): C20
120 5 20 80 r
H B20Cu N O V12, M = 3066.32, triclinic, space group P-1
(no. 2), a = 13.888(7) Å, b = 14.464(7) Å, c = 14.851(8) Å, α = 74.470(8)°, β =
3
= 1.964 g· cm−3, μ =
= 0.0541 and wR = 0.1259 (I >
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2
2
8.072(10)°, γ = 63.880(8)°, V = 2568(2) Å , Z = 1, D
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159-163.
1
2
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σ(I)).
Acknowledgements
This work was financially supported by the National Natural
Science Foundation of China (no. 21601095, 21571109), the
Youth Project of Nanyang Normal University (no. QN2017065)
and the Opening Laboratory Project of Nanyang Normal
University (no. SYKF2016075).
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Keywords: open-framework borovanadate • benzylic C–H bond
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