The syntheses and characterization of the bulky terphenyl silanes and chlorosilanes 2,6-Mes(2)C(6)H(3)SiCl(3), 2,6-Trip(2)C(6)H(3)SiCl(3), 2,6-Mes(2)C(6)H(3)SiHCl(2), 2,6-Trip(2)C(6)H(3)SiHCl(2), 2,6-Mes(2)C(6)H(3)SiH(3), 2,6-Trip(2)C(6)H(3)SiH(3) and 2,6-Mes(2)C(6)H(3)SiCl(2)SiCl(3)
Rs. Simons et al., The syntheses and characterization of the bulky terphenyl silanes and chlorosilanes 2,6-Mes(2)C(6)H(3)SiCl(3), 2,6-Trip(2)C(6)H(3)SiCl(3), 2,6-Mes(2)C(6)H(3)SiHCl(2), 2,6-Trip(2)C(6)H(3)SiHCl(2), 2,6-Mes(2)C(6)H(3)SiH(3), 2,6-Trip(2)C(6)H(3)SiH(3) and 2,6-Mes(2)C(6)H(3)SiCl(2)SiCl(3), MAIN GR CHE, 2(4), 1998, pp. 275-283
The synthesis and characterization of the primary terphenyl silanes and chl
orosilanes 2,6-Mes(2)C(6)H(3)SiCl(3) (1a), 2,6-Trip(2)C(6)H(3)SiCl(3) (1b),
2,6-Mes(2)C(6)H(3)SiHCl(2) (2a), 2,6-Trip(2)C(6)H(3)SiHCl(2) (2b), 2,6-Mes
(2)C(6)H(3)SiH(3) (3a), 2,6-Trip(2)C(6)H(3)SiH(3) (3b) and 2,6-Mes(2)C(6)H(
3)SiCl(2)SiCl(3) (4), (where Mes = 2,4,6-Me3C6H2 and Trip = 2,4,6-i-Pr3C6H2
) are described. Compounds (la, Ib), (2a, 2b) and (4) were prepared by the
reaction between SiCl4, SiHCl3 or Si2Cl6, respectively, and the appropriate
aryl lithium reagent (2,6-Mes(2)C(6)H(3)Li or 2,6-Trip(2)C(6)H(3)Li . OEt2
). Compounds (3a) and (3b) were prepared by reduction of (1a) and (1b) with
LiAlH4, respectively. The derivatives (1a)-(3a) were characterized by H-1,
C-13, 29Si NMR and IR spectroscopy. The structures of (1a), (1b) and (4) h
ave been determined. Crystal data with CuK alpha (lambda = 1.54178 Angstrom
) at 130 K: (1a), a = 9.074(2) Angstrom, b = 16.681(3) Angstrom, c = 15.842
(3) Angstrom, beta = 105.20(3)degrees, V = 2313.9(8) Angstrom(3), Z = 4, sp
ace group P2(1)/c, 2772 (I > 2 sigma(I)) data, R = 0.042; (1b), a = 12.197(
2) Angstrom, b = 25.602(5) Angstrom, c = 11.098(2) Angstrom, V = 3465.5(11)
Angstrom(3) Z = 4, space group Pnma, 2131 (I > 2 sigma(I)) data, R = 0.061
; (4), a = 10.799(2) Angstrom, b = 15.355(3) Angstrom, c = 16.724(3) Angstr
om, beta = 106.907(13)degrees, V = 2653.2(8) Angstrom(3), Z = 4, space grou
p P2(1)/n, 2852 (I > 2 sigma(I)) data, R = 0.047.