TETRA(N-BUTYL)AMMONIUM PHTHALOCYANINATO(2 -)LITHATE TETRAHYDROFURANE AND BIS(TETRA(N-BUTYL)AMMONIUM) PHTHALOCYANINATO(2-)LITHATE FLUORIDE HYDRATE - SYNTHESIS AND CRYSTAL-STRUCTURE

Dilithiumphthalocyaninate(2-) reacts with excess tetra(n-butyl)ammoniu m fluoride trihydrate to yield a mixture of blue tetra(n-butyl)ammoniu m phthalocyaninato(2-)lithate tetrahydrofurane and bis(tetra(n-butyl)a mmonium) phthalocyaninato(2-)lithate fluoride hydrate. The latter crys tallizes triclinic with crystal data: a = 8.6480(1) Angstrom; b = 12.6 20(2) Angstrom; c = 14.866(5) Angstrom; alpha = 82.44(2)degrees; beta = 87.01(2)degrees; gamma = 75.02 degrees; space group P (1) over bar; Z = 1. Fluoride is not coordinated to lithium. On the contrary, a doub le-salt is formed, which consists of alternating layers of cations and anions. This arrangement opens a cavity in the centre of the unit cel l which shares statistically a fluoride and a disordered fluoride hydr ate. Pure tetra(n-butyl)ammonium phthalocyaninato(2-)lithate is obtain ed as a tetrahydrofurane solvate by the reaction of dilithiumphthalocy aninate(2-) with tetra(n-butyl)ammonium bromide in tetrahydrofurane. T he solvate crystallizes monoclinic with crystal data: a = 12.455(5) An gstrom; b = 23.396(5) Angstrom; c = 16.120(5) Angstrom; beta = 94.986( 5)degrees; space group P2/c1; Z = 4.