Dalton Transactions
Paper
4.3. Preparation of I·2H2O
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Glutaric acid (13.3 mg, 0.1 mmol) and Zn(NO3)2·6H2O (30.4 mg,
0.1 mmol) were dissolved in 4 mL H2O and carefully layered by
a 4 mL acetonitrile solution of 1,2-bis(4-pyridyl)ethylene ligand
(37.6 mg, 0.2 mmol). Suitable crystals of I·2H2O for X-ray ana-
lysis were obtained in two weeks. The yield was 28.7 mg (69%)
for I·2H2O. IR (KBr): ν(cm−1) = 3629(brs), 2971(m), 1613(w),
1568(s), 1435(m), 1390(s), 1336(w), 1027(w), 985(m), 825(m),
548(w). Anal. Calcd for C17H20N2O6Zn (413.74): C, 49.35; H,
4.87; N, 6.77. Found: C, 49.85; H, 4.91; N, 6.83.
4.4. X-ray crystallography
C17H16N2O6Zn, M = 409.69, monoclinic, P2/n, a = 8.0460(16) Å,
b = 5.7930(12) Å, c = 19.177(4) Å, β = 97.46(3)°, V = 886.3(3) Å3,
Z = 2, μ(MoKα) = 1.422 mm−1, 4697 reflections measured, 1741
unique (Rint = 0.0226) which were used in all calculations, final
R = 0.0321 (wR = 0.0963) with reflections having intensities
greater than 2σ, GOF(F2) = 1.123. The X-ray diffraction
data of I·2H2O were collected using a Bruker SMART APEX
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diffractometer equipped with
a monochromater in the
MoKα (λ = 0.71073 Å) incident beam. A single crystal was
mounted on a glass fiber. The CCD data were integrated and
scaled using the Bruker-SAINT software package, and the struc-
ture was solved and refined using SHEXTL V6.12. All hydrogen
atoms were placed in the calculated positions. The bond dis-
tances and angles are listed in Table S1.† Structural infor-
mation was deposited at the Cambridge Crystallographic Data
Centre (CCDC reference number 911186).
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4.5. Catalytic reaction conditions
Phenyl acetate (0.05 mmol) was dissolved in methanol (1 mL),
and I·2H2O (5.0 mg) was added and shaken at 50 °C (450 rpm).
Reaction conversion was monitored by GC/mass analysis of
20 μL aliquots withdrawn periodically from the reaction
mixture. All reactions were run at least three times and the
average conversion yields are presented. Yields were based on
the formation of the product methyl acetate.
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Acknowledgements
The Basic Science Research Program of the National Research
Foundation of Korea (NRF) funded by the Ministry of Edu-
cation, Science and Technology (2012008875, 2012001725,
20110008018, 2013R1A1A2006914) and RP-Grant 2013 of Ewha
Womans University are gratefully acknowledged.
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and S. Huh, Eur. J. Inorg. Chem., 2013, 4228.
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and S. J. Lee, Chem. Commun., 2012, 48, 5512.
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Notes and references
1 K. Sumida, D. L. Rogow, J. A. Mason, T. M. McDonald,
E. D. Bloch, Z. R. Herm, T.-H. Bae and J. R. Long, Chem.
Rev., 2012, 112, 724.
This journal is © The Royal Society of Chemistry 2013
Dalton Trans., 2013, 42, 15645–15649 | 15649