7
.25 (td, 1H, Hpy), 7.43 (d, 1H, Hpy), 7.92 (d, 1H, Hpy), 8.09 (td, 1H, Hpy), 8.54 (s, 1H,
13
CH=N). C-NMR (75.47 MHz, CD
2 2
Cl ): 18.39, 125.35, 126.83, 128.13, 129.24, 129.91,
3
1
1
41.66, 143.05, 145.46, 149.74, 167.31 (C=N). P-NMR (121.48 MHz, CD Cl ): -144.37
2 2
-
(
sept, PF
6
). µeff (Evans’ NMR method) = 1.3 µ .
B
3
.3.2. Synthesis of complex C2
The analogous complex C2 was prepared from CoCl
0.58 g, 2.6 mmol) and salt (0.43 g, 1.26 mmol) following the method described above. Yield:
2
.6H O (0.3 g, 1.26 mmol), ligand L2
2
(
0
.58 g (67%). Anal. Calc. for C30
H32ClCoF
6
N
4
P (687.95): C, 52.38; H, 4.69; N, 8.14. Found:
-
1
1
C, 51.42; H, 4.77; N, 8.17. IR (cm ): 1629; 1595. H NMR (CD
2
Cl
2
): δ (ppm) 1.39 (s, 3H,
CH
3
-C=N), 2.24 (s, 3H, o-CH
3
), 2.31 (s, 3H, o-CH ), 6.70 (d, 1H, J = 7.5 Hz, Har), 7.06 (t, 1H,
3
J = 7.5 Hz, Har), 7.18 (t, 1H, J = 5.1 Hz, Hpy), 7.23 (d, 1H, J = 7.8 Hz, Har), 7.45 (d, 1H, J = 5.2
1
3
Hz, Hpy), 8.03 (t, 1H, J = 7.8 Hz, Hpy), 8.11 (d, 1H, J = 7.8 Hz, Hpy). C-NMR (75.47 MHz,
CD Cl ): 17.51, 17.89, 18.56, 126.09, 127.72, 128.60, 129.33, 129.81, 141.56, 143.85,
46.66, 149.18, 172.98 (C=N). P-NMR (121.48 MHz, CD
Evans’ NMR method) = 1.4 µ
2
2
3
1
-
6
1
2
Cl
2
): -144.45 (sept, PF
). µeff
(
B
.
3.3.3. Synthesis of complex C3
Analogously to the synthesis of complex C1, complex C3 was prepared from CoCl
2 2
.6H O
(
(
0.6 g, 2.52 mmol), ligand L3 (1.46 g, 5.21 mmol) and salt (0.85 g, 2.52 mmol). Yield: 1.48 g
73%). Anal. Calc. for C38
H48ClCoF
6
N
4
P (800.16): C, 57.04; H, 6.05; N, 7.00. Found: C,
-
1
1
5
6
7.83; H, 6.78; N, 6.82. IR (cm ): 1629; 1595. H NMR (CD
2
Cl
2
): δ (ppm) 1.03 (d, 12H, J =
-C=N), 2.88 (m, 2H,
.9 Hz, CH
3
-iPr), 1.30 (d, 12H, J = 6.9 Hz, CH
3
-iPr), 2.39 (s, 3H, CH
3
CH-iPr), 7.32 (m, 3H, Har), 7.93 (t, 1H, J = 5.1 Hz, Hpy), 8.22 (d, 1H, J = 8.1 Hz, Hpy), 8.32 (t,
1
3
1
2
1
H, J = 7.8 Hz, Hpy), 8.85 (d, 1H, J = 5.1 Hz, Hpy). C-NMR (75.47 MHz, CD
2 2
Cl ): 18.61,
4.53, 24.85, 28.75, 125.01, 126.26, 128.21, 129.98, 139.82, 140.08, 142.41, 147.75, 149.72,
3
1
-
2 2 6
71.63 (C=N). P-NMR (121.48 MHz, CD Cl ): -144.44 (sept, PF ). µeff (Evans’ NMR
method) = 1.4 µ
B
.
3.4. Solid state structure determination
X-ray quality crystals of C1 were grown from a mixture of CH
standing at ambient temperature. Intensity data were collected at ambient temperature on a
Nonius Kappa-CCD diffractometer equipped with graphite monochromated MoK radiation.
2 2
Cl /n-hexane solution upon
α
1
0