Anal. Calc. for C17
C, 69.68; H, 5.15; N, 4.85%. H NMR (CDCl
aryl, 6H), 7.58-7.65 (m, aryl, 5H), 8.19 (m, aryl, 1H). C{ H} NMR (CDCl
C3, PyO), 118.0 (s, C5, PyO), 128.4 (d, J = 17.2 Hz, meta-Ph), 129.6 (s, para-Ph), 130.9 (d, J =
H
14NOP·0.7H
2
O (MW: 291.9), requires: C, 69.95; H, 5.32; N, 4.80. Found:
1
3
, δ ppm): 6.91-6.96 (m, aryl, 2H), 7.34-7.41 (m,
1
3
1
3
, δ ppm): 112.3 (s,
2
1
3.4 Hz, ortho-Ph), 139.1 (s, C4, PyO), 140.7 (d, J = 18.9 Hz, ipso-Ph), 147.6 (s, C6, PyO),
31
1
62.5 (d, J = 6.9 Hz, C2, PyO). P{ H} NMR (CDCl
3
, δ ppm): 100.6 (s).
II
.7. Syntheses of Ru-complexes 2a, 2b, 3a , 3b , 3c and 3c
II
I
II
2
2
a: This compound was synthesized in an analogous manner to 2b from 128 mg (400 µmol) 1a
and 384 mg (400 µmol) [RuCl
yield (256 mg, 243 µmol). Although the single-crystal used for structure analysis revealed a
solvent content of 0.5 Et O, elemental analysis indicates that the bulk of the crystalline product
consists of CHCl /Et O solvates of variable solvent site occupancy. Both CHCl and Et O proton
signals were detected in a H NMR spectrum of 2a recorded in CD
2
(PPh
3
)
3
]. The orange crystalline product was obtained in 61%
2
3
2
3
2
1
2
Cl .
2
Anal. Calc. for C56
H
48Cl
2
NOP
3
Ru·0.2CHCl
3
·0.3Et
2
O (MW: 1062.0), requires: C, 64.92; H, 4.86;
, δ ppm): 2.50 (d, J = 3.72 Hz, -
1
N, 1.32. Found: C, 64.92; H, 4.83; N, 1.38%. H NMR (CDCl
3
CH
3
, 3H), 6.74-6.85 (br. m, meta-PPh
.02 (m, ortho-PPh , 6H), 7.08 (m, para-PPh
.24-7.31 (m, meta-(MeNCOPh), meta-Ph P(MeNCO), 6H), 7.37 (t, J = 7.46 Hz, para-
3
, 12H), 6.89 (d, J = 7.50 Hz, ortho-(MeNCOPh), 2H),
7
7
3
3
, 3H), 7.11-7.21 (m, para-PPh , ortho-PPh , 9H),
3
3
2
1
3
1
(
MeNCOPh), 1H), 7.40-7.47 (m, ortho-Ph
NMR (CDCl , δ ppm): 35.6 (s, -CH ), 126.4 (d, J = 8.3 Hz, meta-PPh
MeNCOPh)), 127.0 (d, J = 9.2 Hz, meta-PPh ), 127.4 (d, J = 8.8 Hz, meta-Ph
27.9 (s, meta-(MeNCOPh)), 128.5 (s, para-PPh ), 128.8 (s, para-PPh ), 129.5 (m, ipso-
P(MeNCO)), 129.8 (s, para-(MeNCOPh)), 130.1 (s, para-Ph P(MeNCO)), 132.5 (d, J = 34.3
Hz, ipso-PPh ), 133.9 (s, ipso-(MeNCOPh)), 134.1 (d, J = 9.7 Hz, ortho-Ph P(MeNCO)), 134.9
d, J = 9.4 Hz, ortho-PPh ), 136.2 (d, J = 8.0 Hz, ortho-PPh ), 136.4 (d, J = 44.0 Hz, ipso-PPh ),
, δ ppm): 108.2 (dd, J = 342 Hz, J = 29 Hz,
, 1P), 19.0 (dd, J = 342 Hz, J = 29 Hz, PPh , 1P).
2
P(MeNCO), para-Ph
2
P(MeNCO), 6H). C{ H}
), 126.9 (s, ortho-
P(MeNCO)),
3
3
3
(
3
2
1
3
3
Ph
2
2
3
2
(
3
3
3
3
1
1
1
83.2 (d, J = 13.8 Hz, NCO). P{ H} NMR (CDCl
3
Ph
2
P(MeNCOPh), 1P), 41.4 (t, J = 29 Hz, PPh
3
3
2
b: 1b (145 mg, 457 µmol) and [RuCl
2
(PPh
3
)
3
] (438 mg, 457 µmol) were dissolved in CHCl
3
(5
mL). The deep red solution was stirred for 3 h and then stored undisturbed at room temperature.
7