m/z exact mass [Ag3D16·2·Cl]3+ 894.12, C130H109N10O19ClS6Ag3
requires 894.11, [Ag3D16·2·(OTf)·(CH3SO3)·(H2O)2]2+ 1460.14,
C133H119N10O27F3S8Ag3 requires 1460.15, [Ag3D16·2·(OTf)2·
(H2O)]2+ 1481.11, C133H114N10O26F6S8Ag3 requires 1481.14.
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Single ball bearing Ag36·10·(CH3SO3)3. To a solution of 10
(1.59 mg, 2.62 mmol, 1.0 equiv) and 6 (1.80 mg, 2.62 mmol,
1.0 equiv) in CD3OD (450 mL, 5.8 mM) was added a solution
of AgCH3SO3 (7.8 mmol, 3.0 equiv) in a mixture of CD3OD and
D2O (CD3OD/D2O = 4 : 1, 39 mL, 0.20 M) at room temperature.
The reaction mixture was allowed to stand at room temperature
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1
for a few minutes; H NMR (500 MHz, CD3OD, 293 K) d 2.14
(s, 6H, OAc), 2.69 (s, 9H, CH3SO3), 3.70 (t, J = 9.5 Hz, 4H,
NCH2CH2O), 3.70 (t, J = 9.5 Hz, 2H, NCH2CH2O), 4.06 (t, J =
9.5 Hz, 4H, NCH2CH2O), 4.07 (t, J = 9.5 Hz, 2H, NCH2CH2O),
4.69 (s, 2H, SCCH2OH), 4.72 (s, 2H, C6H4CH2OH), 5.21 (s, 4H,
C6H4CH2OAc), 7.19 (d, J = 8.0 Hz, 2H, C6H4CH2OAc), 7.24 (d,
J = 8.0 Hz, 1H, C6H4CH2OH), 7.29 (dd, J = 1.5, 8.0 Hz, 1H,
C6H4CH2OH), 7.34 (dd, J = 1.5, 8.0 Hz, 2H, C6H4CH2OAc),
7.54 (d, J = 8.0 Hz, 1H, C6H4CH2OH), 7.57 (d, J = 8.0 Hz, 2H,
C6H4CH2OAc), 7.61 (s, 1H, NCHCCH2), 7.77 (d, J = 3.3 Hz, 1H,
SCH), 7.78 (d, J = 3.3 Hz, 2H, SCH), 7.79 (d, J = 3.3 Hz, 2H,
SCH), 7.85 (dd, J = 1.5, 8.0 Hz, 1H, C6H4CH2OH), 7.87 (dd, J =
1.5, 8.0 Hz, 2H, C6H4CH2OAc), 7.92 (d, J = 3.3 Hz, 2H, NCH),
7.93 (d, J = 3.3 Hz, 1H, NCH), 7.94 (d, J = 3.3 Hz, 2H, NCH).
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Acknowledgements
This work was supported by Grants-in Aid from MEXT of Japan
and the Global COE Program for Chemistry Innovation. E.O.
thanks JSPS Research Fellowship for Young Scientists from the
Japan Society for the Promotion of Science.
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4116 | Dalton Trans., 2010, 39, 4107–4116
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