Paper
Dalton Transactions
[(µ-H)2Ru3(μ3-S)(CO)7(µ-1,2-1c)] 7, yield 27 mg (32%); (Rf = 2003(vs), 1992(s), 1983(m), 1976(w), 1945(m), 1938(w); 1H NMR
0.5); IR (ν(CO)/cm−1, cyclohexane) 2057(s), 2038(vs), 1995(vs), (500 MHz, CDCl3) δ −18.14 (ddd, J = 13.8, 4.5, 2.5 Hz, 1H),
1984(s), 1965(m), 1932(m); 1H NMR (500 MHz, CDCl3) δ −18.31 (‘m’, ddd, J = not resolved 1H, cf. ESI†); 31P NMR
−18.51 (ddd, J = 11.0, 9.7, 3.0 Hz, 1H), −18.64 (dt, J = 11.8, 3.0 (202 MHz, CDCl3) δ 52.62 (m), 49.49 (dd, J = 11.1, 1.3 Hz). ES+
Hz, 1H); 31P NMR (202 MHz, CDCl3) δ 56.47 (dd, J = 9.6, 5.0 MS (m/z): 1502 [M + Na]+.
Hz), 37.16 (t, J = 9.7 Hz). ES+ MS (m/z): 1228 [M + Na]+.
[(µ-H)2Ru3(μ3-S)(CO)7(µ-1,2-1f)] 14, yield 45 mg (43%); (Rf =
[(µ-H)2Ru3(μ3-S)(CO)7(µ-1,2-1c)] 8, yield 33 mg (39%); (Rf = 0.6); IR (ν(CO)/cm−1, cyclohexane) 2064(vs), 2047(s), 2037(m),
0.4); IR (ν(CO)/cm−1, cyclohexane) 2057(s), 2034(vs), 1998(vs), 2003(vs), 1992(m), 1977(w), 1946(w), 1939(w); 1H NMR
1985(s), 1969(m), 1942(m); 1H NMR (500 MHz, CDCl3) δ (500 MHz, CDCl3) δ −18.17 (ddd, J = 11.9, 7.0, 3.6 Hz, 1H),
−18.08 (ddd, J = 10.3, 9.0, 3.0 Hz, 1H), −19.02 (‘m’, ddd, J = −18.83 (ddd, J = 4.8, 3.6 Hz, 1H); 31P NMR (202 MHz, CDCl3) δ
not resolved 1H, cf. ESI†); 31P NMR (202 MHz, CDCl3) δ 59.08 48.49 (dd, J = 11.3, 6.5 Hz), 34.37 (d, J = 8.4 Hz). ES+ MS (m/z):
(dd, J = 9.6, 6.2 Hz), 35.24 (dd, J = 8.6, 2.7 Hz); ES+ MS (m/z): 1479 [M]+.
1228 [M + Na]+.
[(µ-H)2Ru3(µ3-S)(CO)7(µ-1,2-1g)], 15 and 16
[(µ-H)2Ru3(µ3-S)(CO)7(µ-1,2-1d)], 9 and 10
A
total of 55 mg (71 μmol) of 1g was reacted with
A
total of 74 mg (71 μmol) of 1d was reacted with [(μ-H)2Ru3(μ3-S)(CO)9] to give two diastereomers with the
[(μ-H)2Ru3(μ3-S)(CO)9] to give two diastereomers with the general formula [(µ-H)2Ru3(μ3-S)(CO)7(µ-1,2-1g)].
general formula [(µ-H)2Ru3(μ3-S)(CO)7(µ-1,2-1d)].
[(µ-H)2Ru3(μ3-S)(CO)7(µ-1,2-1g)] 15, yield 36 mg (39%); (Rf =
[(µ-H)2Ru3(μ3-S)((CO)7(µ-1,2-1d)] 9, yield 26 mg (23%); (Rf = 0.6); IR (ν(CO)/cm−1, cyclohexane) 2059(s), 2042(vs), 1999(vs),
0.5); IR (ν(CO)/cm−1, cyclohexane) 2063(s), 2044(vs), 2008(vs), 1983(s), 1970(m), 1938(m); 1H NMR (500 MHz, CDCl3) δ
1993(s), 1976(m), 1951(m); 1H NMR (500 MHz, CDCl3) δ −17.69 (td, J = 9.7, 3.0 Hz, 1H), −18.25 (dt, J = 6.4, 3.0 Hz, 1H);
−18.09 (dt, J = 9.6, 2.8 Hz, 1H), −18.39 (ddd, J = 12.8, 10.2, 2.9 31P NMR (202 MHz, CDCl3) δ 44.05 (dd, J = 9.5, 6.4 Hz), 36.51
1H); 31P NMR (202 MHz, CDCl3) δ 48.89 (d, J = 11.8 Hz), 35.65 (dd, J = 8.8, 2.6 Hz). ES+ MS (m/z): 1327 [M + Na]+.
(t, J = 9.6 Hz). ES+ MS (m/z): 1580 [M]+.
[(µ-H)2Ru3(μ3-S)(CO)7(µ-1,2-1g)] 16, yield 48 mg (52%); (Rf =
[(µ-H)2Ru3(μ3-S)(CO)7(µ-1,2-1d)] 10, yield 37 mg (33%); (Rf = 0.5); IR (ν(CO)/cm−1, cyclohexane) 2057(s), 2039(s), 2003(s),
0.4); IR (ν(CO)/cm−1, cyclohexane) 2064(s), 2047(vs), 2006(vs), 2003(vs), 1984(s), 1967(m), 1940(w); 1H NMR (500 MHz, CDCl3)
1992(s), 1980(m), 1949(m); 1H NMR (500 MHz, CDCl3) δ δ −18.16 (m, 2H); (500 MHz, acetone-d6, 253 K) δ −18.12 (dt,
−17.82 (ddd, J = 12.2, 8.8, 3.4 Hz, 1H), −18.63 (ddd, J = 7.3, J = 11.0, 3.0 Hz, 1H), −18.19 (‘m’, ddd, J = not resolved 1H, cf.
5.0, 3.4 Hz 1H); 31P NMR (202 MHz, CDCl3) δ 48.49 (dd, J = ESI†); 31P NMR (202 MHz, CDCl3) δ 49.32 (dd, J = 7.1, 5.1 Hz),
11.3, 6.5 Hz), 34.37 (d, J = 8.4 Hz). ES+ MS (m/z): 1603 38.10 (t, J = 9.6 Hz). ES+ MS (m/z): 1305 [M + H]+.
[M + Na]+.
[(µ-H)2Ru3(µ3-S)(CO)7(µ-1,2-1h)], 17
[(µ-H)2Ru3(µ3-S)(CO)7(µ-1,2-1e)], 11 and 12
A
total of 47 mg (71 μmol) of 1h was reacted with
A total of 51 mg (71 μmol) of 1e was reacted with [(μ-H)2Ru3(μ3- [(μ-H)2Ru3(μ3-S)(CO)9] to give [(µ-H)2Ru3(μ3-S)(CO)7(µ-1,2-1h)]
S)(CO)9] to give two diastereomers with the general formula 17.
[(µ-H)2Ru3(μ3-S)(CO)7(µ-1,2-1e)].
[(µ-H)2Ru3(μ3-S)(CO)7(µ-1,2-1h)] 17, yield 36 mg (42%); (Rf =
[(µ-H)2Ru3(μ3-S)((CO)7(µ-1,2-1e)] 11, yield 29 mg (33%); (Rf = 0.5); IR (ν(CO)/cm−1, cyclohexane) 2060(s), 2043(vs), 2001(vs),
0.6); IR (ν(CO)/cm−1, cyclohexane) 2059(s), 2042(vs), 2000(vs), 1986(s), 1972(m), 1941(m); 1H NMR (500 MHz, CDCl3) δ
1985(m), 1970(w), 1939(w); 1H NMR (500 MHz, CDCl3) δ −17.75 (ddd, J = 10.1, 9.1, 3 Hz, 1H), −18.47 (dt, J = 6.1, 3.0 Hz,
−17.61 (td, J = 9.8, 3.0 Hz, 1H), −18.17 (‘m’, ddd, J = not 1H); 31P NMR (202 MHz, CDCl3) δ 44.95 (dd, J = 9.9, 5.7 Hz),
resolved 1H, cf. ESI†); 31P NMR (202 MHz, CDCl3) δ 43.88 (dd, 35.39 (dd, J = 9.1, 1.8 Hz). ES+ MS (m/z): 1191 [M]+.
J = 9.5, 6.2 Hz), 35.63 (dd, J = 8.9, 2.4 Hz). ES+ MS (m/z): 1248
[(µ-H)2Ru3(µ3-S)(CO)7(µ-1,2-2a)], 18 and 19
[M]+.
[(µ-H)2Ru3(μ3-S)(CO)7(µ-1,2-1e)] 12, yield 38 mg (43%); (Rf = A total of 62 mg (71 μmol) of 2e was reacted with [(μ-H)2Ru3(μ3-
0.5); IR (ν(CO)/cm−1, cyclohexane) 2059(s), 2042(vs), 2000(vs), S)(CO)9] to give two diastereomers with the general formula
1985(m), 1970(w), 1939(w); 1H NMR (500 MHz, CDCl3) δ [(µ-H)2Ru3(μ3-S)(CO)7(µ-1,2-2a)].
−17.61 (ddd, J = 10.0, 3.0 Hz, 1H), −18.16 (‘m’, ddd, J = not
[(µ-H)2Ru3(μ3-S)(CO)7(µ-1,2-2a)] 18, yield 14 mg (14%); (Rf =
resolved 1H, cf. ESI†); 31P NMR (202 MHz, CDCl3 49.09 (dd, J = 0.6): IR (ν(CO)/cm−1, cyclohexane) 2066(vs), 2036(s), 2005(vs),
10.2, 1.7 Hz), 36.60 (t, J = 9.5 Hz). ES+ MS (m/z): 1248 [M]+.
1996(s), 1987(m), 1951(m); 1H NMR (500 MHz, CDCl3) δ
−18.29 (dt, J = 36.5, 2.5 Hz, 1H), −19.46 (ddd, J = 13.3, 7.1, 2.5
Hz, 1H); 31P NMR (202 MHz, CDCl3) δ 56.94 (dd, J = 34.7, 5.9
[(µ-H)2Ru3(µ3-S)(CO)7(µ-1,2-1f)], 13 and 14
A
total of 70 mg (71 μmol) of 1f was reacted with Hz), 25.71 (d, J = 11.8 Hz). ES+ MS (m/z): 1400 [M]+.
[(μ-H)2Ru3(μ3-S)(CO)9] to give two diastereomers with the
general formula [(µ-H)2Ru3(μ3-S)(CO)7(µ-1,2-1f)].
[(µ-H)2Ru3(μ3-S)(CO)7(µ-1,2-2a)] 19, yield 25 mg (25%); (Rf =
0.5): IR (ν(CO)/cm−1, cyclohexane) 2064(vs), 2039(ms, 2032(w),
[(µ-H)2Ru3(μ3-S)(CO)7(µ-1,2-1f)] 13, yield 33 mg (31%); (Rf = 2007(vs), 1993(m), 1980(m), 1967(w), 1951(w); 1H NMR
0.6); IR (ν(CO)/cm−1, cyclohexane) 2064(vs), 2047(m), 2038(s), (500 MHz, CDCl3) δ −17.84 (ddd, J = 12.7, 9.0, 3.6 Hz, 1H),
Dalton Trans.
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