Fortuitous formation of [(LiCl)6{(Me2NCH2C8H5N)3P}2]: an amine-ligated hexameric lithium chloride aggregate

Deprotonation of gramine with nBuLi and subsequent reaction with PCl3 yielded [(LiCl)6{(Me2NCH2C8H5N)3P}2] (2). Compound 2 was characterized by NMR (1H, 13C, 31P) spectroscopy, elemental analysis, and X-ray crystallography. The molecular structure of 2 reveals a novel hexameric lithium chloride aggregate ligated on each of two hexagonal faces by three dimethylamino groups from the intended product, tris{(3-dimethylamino-methyl)indolyl}phosphine. Crystal data for 2 · 3CH2Cl2: C36H45Cl9Li3N6P, monoclinic, P21/n, a = 12.732(4) Å, b = 22.251(6) Å, c = 16.815(5) Å, β = 108.233(5)°, V = 4525(2) Å3, Z = 4, Dcalc = 1.369 g/cm3.