Figueroa et al.
1
powder (2.54 g, 84%). H NMR (CDCl3): δ 7.40 [m, 6H, Ph],
to stir for 18 h and then filtered. The volatile components were
removed from the filtrate in vacuo, and the resulting residue was
extracted with CH2Cl2 (3 mL). The solution was placed at
-35 °C, thereby depositing [κ2-(mimPh)2]CoCl2 as blue crystals over
a period of 2 days, which were isolated and dried in vacuo (0.198
7.22 [s, 2H, Im], 7.14 [m, 6H, Ph and Im]. IR (KBr, cm-1): 3132-
(m), 3115(m), 1716(w), 1652(w), 1595(m), 1558(w), 1539(vw),
1500(vs), 1487(s), 1455(m), 1426(vs), 1338(w), 1307(m), 1299-
(s), 1263(w), 1173(w), 1159(m), 1123(s), 1092(m), 1085(m), 1074-
(m), 1030(w), 1003(w), 980(w), 908(m), 870(w), 831(w), 782(s),
771(vs), 764(vs), 756(vs), 693(vs), 668(m), 639(w), 561(m), 493-
(s), 482(m). Crystals suitable for X-ray diffraction were obtained
from CH2Cl2.
1
g, 72%). H NMR (CDCl3): δ 63.7 [s, 2H, Im], 45.7 [s, 2H, Im],
8.11 [s, 4H, Ph], 6.18 [s, 2H, Ph], 5.95 [s, 4H, Ph]. Anal. Calcd
for [κ2-(mimPh)2]CoCl2‚CH2Cl2: C, 40.4; H, 2.9; N, 9.9. Found:
C, 39.9; H, 2.4; N, 9.7. Crystals suitable for X-ray diffraction were
obtained from CH2Cl2.
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Synthesis of [κ2-(mimBu )2]FeCl2. A solution of (mimBu )2 (0.600
g, 1.93 mmol) in CH2Cl2 (5 mL) was added to a slurry of FeCl2
(0.275 g, 2.17 mmol) in CH2Cl2 (1 mL). The mixture was allowed
to stir for 18 h and then filtered. The volatile components were
removed from the filtrate in vacuo, and the resulting residue was
extracted with CH2Cl2 (3 mL). The solution was placed at -35
Synthesis of [κ2-(mimPh)2]ZnCl2. A solution of (mimPh)2 (0.300
g, 0.85 mmol) in CH2Cl2 (3 mL) was added to a slurry of ZnCl2
(0.127 g, 0.94 mmol) in CH2Cl2 (1 mL). The mixture was allowed
to stir for 18 h and then filtered. The volatile components were
removed from the filtrate in vacuo, and the resulting residue was
extracted with CH2Cl2 (2 mL). The solution was placed at
-35 °C, thereby depositing [κ2-(mimPh)2]ZnCl2 as pale-yellow
crystals over a period of 6 days, which were isolated and dried in
vacuo (0.089 g, 22%). 1H NMR (CDCl3): δ 7.72 [s, 2H, Ph], 7.54
[s, 6H, Im and Ph], 7.35 [s, 2H, Im], 7.31 [s, 4H, Ph]. Anal. Calcd
for [κ2-(mimPh)2]ZnCl2‚CH2Cl2: C, 39.9; H, 2.8; N, 9.8. Found:
C, 38.7; H, 2.8; N, 9.3.
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°C, thereby depositing [κ2-(mimBu )2]FeCl2 as orange crystals over
a period of 3 days, which were isolated and dried in vacuo (0.264
g, 31%). 1H NMR (CDCl3, 300 MHz, 25 °C): δ 64.0 [s, 2H, Im],
47.5 [s, 2H, Im], 1.51 [s, 18H, But]. µeff (Evans method): 5.2 µB.
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Anal. Calcd for [κ2-(mimBu )2]FeCl2: C, 38.5; H, 5.1; N, 12.8.
Found: C, 38.2; H, 4.9; N, 12.6. Crystals suitable for X-ray
diffraction were obtained from CH2Cl2.
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Synthesis of [κ2-(mimBu )2]CoCl2. A solution of (mimBu )2 (0.500
g, 1.61 mmol) in CH2Cl2 (5 mL) was added to a slurry of CoCl2
(0.234 g, 1.80 mmol) in CH2Cl2 (1 mL). The mixture was allowed
to stir for 18 h and then filtered. The volatile components were
removed from the filtrate in vacuo, and the resulting residue was
extracted with CH2Cl2 (3 mL). The solution was placed at
Synthesis of [κ2-(seimMes)2]FeCl2. A solution of (seimMes)2 (0.200
g, 0.38 mmol) in CH2Cl2 (5 mL) was added to a slurry of FeCl2
(0.048 g, 0.38 mmol) in CH2Cl2 (1 mL). The mixture was allowed
to stir for 18 h and then filtered. The volatile components were
removed from the filtrate in vacuo, and the resulting residue was
extracted with CH2Cl2 (2 mL). The solution was placed at
-35 °C, thereby depositing [κ2-(seimMes)2]FeCl2 as orange crystals
over a period of 2 days, which were isolated and dried in vacuo
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-35 °C, thereby depositing [κ2-(mimBu )2]CoCl2 as blue crystals
over a period of 3 days, which were isolated and dried in vacuo
1
1
(0.313 g, 44%). H NMR (CDCl3): δ 71.9 [s, 2H, Im], 49.6 [s,
(0.153 g, 62%). H NMR (CDCl3): δ 65.9 [s, 2H, Im], 42.9 [s,
2H, Im], 2.92 [s, 18H, But]. µeff (Evans method): 4.4 µB. Anal.
2H, Im], 7.37 [s, 4H, m-Mes], 2.10 [s, 12H, p-CH3Mes], 1.12 [s,
6H, o-CH3Mes]. Anal. Calcd for [κ2-(seimMes)2]FeCl2: C, 44.0; H,
4.0; N, 8.6. Found: C, 43.0; H, 3.8; N, 8.3. MS: m/z 621.0 {M -
Cl}+. Crystals suitable for X-ray diffraction were obtained from
CH2Cl2.
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Calcd for [κ2-(mimBu )2]CoCl2: C, 38.2; H, 5.0; N, 12.7. Found:
C, 38.1; H, 5.0; N, 12.7. Crystals suitable for X-ray diffraction
were obtained from CH2Cl2.
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Synthesis of [κ2-(mimBu )2]NiCl2. A solution of (mimBu )2 (0.250
g, 0.80 mmol) in CH2Cl2 (3 mL) was added to a slurry of NiCl2
(0.156 g, 1.20 mmol) in CH2Cl2 (1 mL). The mixture was allowed
to stir for 18 h and then filtered. The volatile components were
removed from the filtrate in vacuo, and the resulting residue was
extracted with CH2Cl2 (1.5 mL). The solution was placed at
Synthesis of [κ2-(seimMes)2]CoCl2. A solution of (seimMes
)
2
(0.085 g, 0.16 mmol) in CH2Cl2 (3 mL) was added to a slurry of
CoCl2 (0.031 g, 0.24 mmol) in CH2Cl2 (1 mL). The mixture was
allowed to stir for 18 h and then filtered. The volatile components
were removed from the filtrate in vacuo, and the resulting residue
was extracted with CH2Cl2 (2 mL). The solution was placed at
-35 °C, thereby depositing [κ2-(seimMes)2]CoCl2 as green crystals
over a period of 2 days, which were isolated and dried in vacuo
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-35 °C, thereby depositing [κ2-(mimBu )2]NiCl2 as a purple
precipitate over a period of 1 day, which was isolated and dried in
vacuo (0.108 g, 31%). 1H NMR (CDCl3): δ 99.3 [s, 2H, Im], 61.7
[s, 2H, Im], 6.17 [s, 18H, But]. µeff (Evans method): 2.9 µB. MS:
m/z 403.15 {M - Cl}+. Crystals suitable for X-ray diffraction were
obtained from CH2Cl2.
1
(0.049 g, 47%). H NMR (CDCl3): δ 69.8 [s, 2H, Im], 44.6 [s,
2H, Im], 7.83 [s, 4H, m-Mes], 2.72 [s, 6H, p-CH3Mes], 1.26 [br s,
12H, o-CH3Mes]. MS: m/z 622.2 {M - Cl}+. Crystals suitable
for X-ray diffraction were obtained from CH2Cl2.
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Synthesis of [κ2-(mimBu )2]ZnCl2. A solution of (mimBu )2 (0.300
g, 0.97 mmol) in CH2Cl2 (3 mL) was added to a slurry of ZnCl2
(0.144 g, 1.06 mmol) in CH2Cl2 (1 mL). The mixture was allowed
to stir for 18 h and then filtered. The volatile components were
removed from the filtrate in vacuo, and the resulting residue was
extracted with CH2Cl2 (2 mL). The solution was placed at
Synthesis of [κ2-(seimMes)2]NiCl2. A solution of (seimMes)2 (0.090
g, 0.17 mmol) in CH2Cl2 (5 mL) was added to a slurry of NiCl2
(0.029 g, 0.22 mmol) in CH2Cl2 (1 mL). The mixture was allowed
to stir for 30 h and then filtered. The volatile components were
removed from the filtrate in vacuo, and the resulting residue was
extracted with CH2Cl2 (2 mL). The solution was placed at
-35 °C, thereby depositing [κ2-(seimMes)2]NiCl2 as green crystals
over a period of 2 days, which were isolated and dried in vacuo
t
-35 °C, thereby depositing [κ2-(mimBu )2]ZnCl2 as pale-yellow
crystals over a period of 3 days, which were isolated and dried in
1
vacuo (0.086 g, 20%). H NMR (CDCl3): δ 7.55 [d, 2H, J ) 1.5
Hz, Im], 7.27 [d, 2H, J ) 1.5 Hz, Im], 1.72 [s, 18H, But]. Anal.
(0.033 g, 30%). H NMR (CDCl3): δ 88.2 [s, 2H, Im], 54.4 [s,
1
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Calcd for [κ2-(mimBu )2]ZnCl2: C, 37.6; H, 5.0; N, 12.5. Found:
2H, Im], 8.66 [s, 4H, m-Mes], 3.60 [s, 6H, p-CH3Mes], 3.47 [s,
12H, o-CH3Mes]. MS: m/z 623.1 {M - Cl}+. Crystals suitable
for X-ray diffraction were obtained from CHCl3.
C, 37.7; H, 4.7; N, 12.4. Crystals suitable for X-ray diffraction
were obtained from CH2Cl2.
Synthesis of [κ2-(mimPh)2]CoCl2. A solution of (mimPh)2 (0.200
g, 0.57 mmol) in CH2Cl2 (3 mL) was added to a slurry of CoCl2
(0.081 g, 0.62 mmol) in CH2Cl2 (1 mL). The mixture was allowed
t
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Synthesis of [κ2-(mimBu )2]CuCl. A solution of (mimBu )2 (0.300
g, 0.96 mmol) in CH2Cl2 (3 mL) was added to a slurry of CuCl
(0.100 g, 1.01 mmol) in CH2Cl2 (1 mL). The mixture was allowed
9242 Inorganic Chemistry, Vol. 46, No. 22, 2007