PREPARATION AND CHARACTERIZATION OF ARSINE DERIVATIVES - X-RAY CRYSTAL-STRUCTURES OF AS(SI(T)BUME(2))(3), AS(SIME(3))(2)(SIPH(3)), ET(3)GA-CENTER-DOT-AS(SIME(3))(2)(SIPH(3)), AND AS(SEPH)(3)
Ra. Baldwin et al., PREPARATION AND CHARACTERIZATION OF ARSINE DERIVATIVES - X-RAY CRYSTAL-STRUCTURES OF AS(SI(T)BUME(2))(3), AS(SIME(3))(2)(SIPH(3)), ET(3)GA-CENTER-DOT-AS(SIME(3))(2)(SIPH(3)), AND AS(SEPH)(3), Heteroatom chemistry, 7(6), 1996, pp. 409-416
As(Si(t)BuMe(2))(3) (1) was prepared by the salt-elimination reaction
between (Na/K)(3)As and (t)BuMe(2)SiCl. Mixing LiAs(SiMe(3))(2) with P
h(3)SiCl (1:1) yielded As(SiMe(3))(2)(SiPh(3)) (2) in a good crystalli
ne yield. Reaction of 2 (1:1) with Et(3)Ga gave the expected Lewis aci
d-base adduct Et(3)Ga . As(SiMe(3))(2)(SiPh(3)) (3). The 1:1 mole rati
o reaction of In(SePh)(3) with As(SiMe(3))(3) resulted in a ligand red
istribution around the indium and arsenic centers to afford As(SePh)(3
) (4) in a low yield. The solid-state structures of 1-4 have been esta
blished by single-crystal X-ray analysis. Crystal data for 1, monoclin
ic space group P 2(1)/c, with a = 11.112(2), b = 17.453(2), c = 14.199
(2) Angstrom, beta = 114.89 degrees for Z = 4; 2, orthorhombic space g
roup P c2(1)n, with a = 9.236(1), b = 16.612(2), c = 16.803(4) Angstro
m for Z = 4; 3, monoclinic space group P 2(1)/c, with a = 16.799(1), b
= 11.199(2), c = 19.413(3) Angstrom, beta = 112.22(1) for Z = 4; 4, t
rigonal space group R (3) over bar, with a = 12.863(5), c = 18.96(1) A
ngstrom for Z = 6. (C) 1996 John Wiley & Sons, Inc.