X-ray Crystal Structure of InCl (sub3).2THF, A Neutral Five-Coordinate BIS-Adductof an In(III) Trihalide

摘要

The 2:1 mole ratio reaction of InCl3 and P(SiMe3)3 in a toluene/THF mixture wasinvestigated. Reaction appears to occur in a 1: 1 mole fashion, since the products obtained are unreacted InCl3 (48.5% recovered) as InCl3.2THF and a fine powder which roughly analyzes to be Cl2In3P3(SiMe3)2)n. The latter was characterized by melting point and partial elemental analysis. The X-ray crystal structure of InCl3.2THF is reported. InCl3.2THF crystallizes in the orthorhombic space group Pbcn (D2h14), No.60) with unit cell parameters of a = 10.802(1) A, b = 10.101(1) A, c = 13.083(1) A, v = 1427.5(4) A3, and Dcalcd = 1.700 g cm-3 for Z = 4 R 0.042 (Rw = 0.058) and is an example of a neutral pentacoordinated bis-adduct of an indium(III) trihalide. The crystal structure consists of discrete monomeric units with no abnormally short intermolecular separations. The geometry about the indium atom approximates to trigonal bipyramidal with oxygen atoms of each of the THF molecules occupying axial positions In-0 = 2.257(9) A, 0-In-0 = 178.5(3) deg while the three chlorine atoms (mean In-Cl = 2.321 A) lie in the equatorial plane.