Molecules 2021, 26, 4154
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THF), 1.29 (d, 6H, CH(CH3)2), 3.31 (br s, 2H, CH(CH3)2), 3.59 (m, 4H, THF), 6.43–7.39 (m,
◦
11H, Ph-H), 8.00 (s, 1H, CH = NAr). 13C NMR (125 MHz, C6D6, 128 ppm, 25 C): 3.22, 25.6,
29.0, 45.9, 68.5, 114.9, 118.7, 119.5, 120.5, 121.8, 124.4, 126.5, 135.2, 136.2, 138.4, 141.5, 146.6,
151.8, 157.3, 159.1, 170.4. Anal. Calcd for C40H64FN2OScSi2 (%): C, 67.75; H, 9.10; N, 3.95.
Found: C, 67.53; H, 8.90; N, 4.20.
3.2.4. Synthesis of L1Lu(CH2SiMe3)2(THF) (1b)
1
The preparation method of complex 1b is similar to that of complex 1a (67%). H NMR
(500 MHz, C6D6, 7.16 ppm, 25 ◦C): δ −0.77 (s, 4H, CH2SiMe3), 0.08 (s, 18H, CH2SiMe3),
0.92 (d, 6H, CH(CH3)2), 1.23 (m, 4H, THF), 1.34 (d, 6H, CH(CH3)2), 3.21 (m, 2H, CH(CH3)2),
3.85 (m, 4H, THF), 6.36–7.48 (m, 11H, Ph-H), 7.96 (s, 1H, CH = NAr). 13C NMR (125 MHz,
C6D6, 128 ppm, 25 ◦C): 4.28, 25.0, 25.4, 28.9, 41.2, 70.3, 114.4, 115, 116, 120.5, 124.1, 125.6,
126.1, 127.2, 133.4, 134.8, 140.6, 141.5, 147.9, 149.2, 156.2, 158.1, 168.6. Anal. Calcd for
C40H64FLuN2OSi2 (%): C, 57.26; H, 7.69; N, 3.34. Found: C, 57.56; H, 7.90; N, 3.08.
3.2.5. Synthesis of L1Y(CH2SiMe3)2(THF) (1c)
The preparation method of complex 1c is similar to that of complex 1a (65%). Single
◦
crystal suitable for X-ray analysis was obtained from hexane at
−
30 C. 1H NMR (500 MHz,
C6D6, 7.16 ppm, 25 ◦C): δ −0.51 (s, 4H, CH2SiMe3), 0.11 (s, 18H, CH2SiMe3), 0.94 (d, 6H,
CH(CH3)2), 1.22 (m, 4H, THF), 1.36 (d, 6H, CH(CH3)2), 3.21 (m, 2H, CH(CH3)2), 3.84 (m,
4H, THF), 6.◦38–7.49 (m, 11H, Ph-H), 7.98 (s, 1H, CH = NAr). 13C NMR (125 MHz, C6D6,
128 ppm, 25 C): 4.13, 25.33, 28.95, 35.30, 70.30, 114.22, 115.45, 120.66, 124.15, 125.90, 126.07,
127.13, 133.29, 134.88, 140.45, 141.33, 147.73, 148.53, 156.32, 158.12, 168.18. Anal. Calcd for
C40H64FN2OSi2Y (%): C, 63.80; H, 8.57; N, 3.72. Found: C, 63.59; H, 8.81; N, 3.95.
3.2.6. Synthesis of L2Sc(CH2SiMe3)2 (2a)
The hexane solution (4 mL) of Sc(CH2SiMe3)3(THF)2 (0.22 g, 0.5 mmol) was added
dropwise to the ligand L2 solution (0.193 g, 0.5 mmol in 4 mL hexane) at 0 °C. The mixture
was stirred for 1 h and then cooling to
−
30 ◦C for 1 day afforded crystalline solids, which
dried in vacuo to give orange solids of 2a (0.22 g, 73%). 1H NMR (500 MHz, C6D6,
7.16 ppm, 25 ◦C): δ −0.05 (s, 4H, CH2SiMe3), 0.00 (s, 18H, CH2SiMe3), 1.01–1.33 (m, 12H,
CH(CH3)2), 3.37 (m, 2H, CH(CH3)2), 3.90 (s, 3H, OCH3), 6.48–7.45 (m, 11H, Ph-H), 8.07
(s, 1H, CH = NAr). 13C NMR (125 MHz, C6D6, 128 ppm, 25 ◦C): 3.25, 26.07, 58.54, 111.28,
117.43, 118.51, 120.46, 120.99, 121.24, 124.14, 124.44, 135.15, 136.36, 139.96, 141.81, 147.12,
149.88, 153.11, 170.63. Anal. Calcd for C37H60N2OScSi2 (%): C, 68.37; H, 9.30; N, 4.31.
Found: C, 68.72; H, 9.04; N, 4.58.
3.2.7. Synthesis of L2Lu(CH2SiMe3)2(THF) (2b)
The preparation method of complex 2b is similar to that of complex 2a (70%). 1H
◦
NMR (500 MHz, C6D6, 7.16 ppm, 25 C): δ −0.59,
−
0.84 (4H, CH2SiMe3), 0.00 (s, 18H,
CH2SiMe3), 0.96–1.24 (m, 12H, CH(CH3)2), 1.37 (m, 4H, THF), 3.22 (m, 2H, CH(CH3)2),
3.55 (m, 4H, THF), 3.75 (s, 3H, OCH3), 6.44–7.45 (m, 11H, Ph-H), 7.94 (s, 1H, CH=NAr).
13C NMR (125 MHz, C6D6, 128 ppm, 25 ◦C): 3.88, 25.71, 29.06, 58.01, 67.99, 111.60, 117.28,
120.12, 120.45, 120.62, 121.47, 124.43, 135.06, 136.57, 140.90, 141.64, 145.97, 149.98, 154.17,
171.05. Anal. Calcd for C41H67LuN2O2Si2 (%): C, 57.86; H, 7.93; N, 3.29. Found: C, 57.63;
H, 8.14; N, 3.53.
3.2.8. Synthesis of L2Y(CH2SiMe3)2(THF) (2c)
The preparation method of complex 2c is similar to that of complex 2a (74%). Sin-
gle crystals suitable for X-ray analysis were obtained from hexane at
−
30 ◦C. 1H NMR
◦
(500 MHz, C6D6, 7.16 ppm, 25 C): δ −0.46,
−
0.68 (4H, CH2SiMe3), 0.06 (s, 18H, CH2SiMe3),
1.00–1.33 (m, 12H, CH(CH3)2), 1.37 (m, 4H, THF), 3.19 (m, 2H, CH(CH3)2), 3.61 (m, 4H,
THF), 3.78 (s, 3H, OCH3), 6.52–7.63 (m, 11H, Ph-H), 7.94 (s, 1H, CH = NAr). 13C NMR
(125 MHz, C6D6, 128 ppm, 25 ◦C): 4.21, 25.38, 29.00, 31.97, 34.57, 34.88, 57.66, 69.37, 110.62,