Inorganic Chemistry
Article
(m, 4H, CH2, partially behind the H2O peak), 1.61−1.54 (m, 4H,
CH2), 1.46−1.38 (m, 8H, CH2), 0.96 (t, J = 6.8 Hz, 6H, CH3).
ESI-MS: m/z calcd for [Cu21BF4(CH3CN)]+: 1268.36; found:
1268.44.
ACKNOWLEDGMENTS
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This study was supported by Grants-in-Aids from MEXT of
Japan and Global COE Program for Chemistry Innovation
through Cooperation of Science and Engineering.
Preparation of [CuZn1(X)4]n+ (4a) (X = CF3CO2 or solvent). To
a solution of 1 in CDCl3/CD3CN = 10:1 (300 μM, 300 μL, 0.090
μmol, 1.0 equiv) was added a solution of Cu(CH3CN)4BF4 in CD3CN
(26 mM, 3.4 μL, 0.090 μmol, 1.0 equiv) and a solution of
Zn(CF3CO2)2 in CD3CN (26 mM, 3.4 μL, 0.090 μmol, 1.0 equiv).
CDCl3 was added to keep the solvent ratio (CDCl3/CD3CN = 10:1)
constant. p-Dimethoxybenzene (100 μM) was used as an internal
standard.
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ESI-MS: m/z calcd for [CuZn1(CF3CO2)2(CH3CN)]+: 1408.33;
found: 1408.05.
Preparation of [CuZn1(X)4]n+ (4b) (X = Cl or solvent). To a
solution of 1 in CDCl3/CD3CN = 10:1 (240 μM, 340 μL, 0.081 μmol,
1.0 equiv) was added a solution of Cu(CH3CN)4BF4 in CD3CN (20
mM, 4.0 μL, 0.080 μmol, 1.0 equiv) and a solution of ZnCl2 in
CD3CN (23 mM, 3.5 μL, 0.081 μmol, 1.0 equiv). CDCl3 was added to
keep the solvent ratio (CDCl3/CD3CN = 10:1) constant. p-
Dimethoxybenzene (100 μM) was used as an internal standard.
1H NMR (500 MHz, CDCl3/CD3CN = 10:1, 293 K): δ 8.82 (d, J =
8.5 Hz, 2H, ArH), 8.69 (d, J = 8.3 Hz, 2H, ArH), 8.45 (d, J = 8.1 Hz,
4H, ArH), 8.33−8.28 (m, 8H, ArH), 8.20 (s, 2H, ArH), 8.10 (s, 2H,
ArH), 7.93−7.90 (m, 8H, ArH), 7.60 (s, 2H, ArH), 7.26 (s, 2H, ArH),
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1H NMR (500 MHz, CDCl3/CD3CN = 10:1, 293 K): δ 8.87 (d, J =
8.5 Hz, 2H, ArH), 8.69 (d, J = 8.1 Hz, 2H, ArH), 8.32 (d, J = 8.2 Hz,
2H, ArH), 8.29 (d, J = 8.3 Hz, 2H, ArH), 8.25−8.23 (m, 6H, ArH),
8.11 (s, 2H, ArH), 8.02 (d, J = 7.9 Hz, 4H, ArH), 7.95 (d, J = 7.9 Hz,
4H, ArH), 7.86 (d, J = 8.1 Hz, 4H, ArH), 7.41 (s, 2H, ArH), 7.28 (s,
2H, ArH), 7.22 (s, 2H, ArH), 4.17 (t, J = 6.4 Hz, 4H, CH2), 1.90−1.80
(m, 4H, CH2, behind the H2O peak), 1.62−1.54 (m, 4H, CH2), 1.46−
1.39 (m, 8H, CH2), 0.95 (t, J = 6.6 Hz, 6H, CH3).
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ASSOCIATED CONTENT
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S
* Supporting Information
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Synthetic procedure of 1, ESI-TOF mass and NMR spectra of 1
and its metal complexes, UV−vis spectra of 2a, 2b, and 3, and
X-ray crystallographic data of 1 and 2a in cif format. This
material is available free of charge via the Internet at http://
AUTHOR INFORMATION
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Corresponding Author
(7) (a) Hiraoka, S.; Goda, M.; Shionoya, M. J. Am. Chem. Soc. 2009,
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131, 4592−4593. (b) Gagne, R. R.; Spiro, C. L.; Smith, T. J.; Hamann,
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dx.doi.org/10.1021/ic201803c | Inorg. Chem. 2012, 51, 1508−1515