Indate(III) phthalocyanines: synthesis, spectroscopy and crystal structure of iodophthalocyaninato(2-) indate(III)

Abstract

A new complex of iodophthalocyaninato(2-) indate(III) has been synthesized in crystalline form by the reaction of indium powder with 1,2-dicyanobenzene under a stream of iodine at about 200°C. It crystallizes in the monoclinic system, space group P2 1/ n with Z=4 in a unit cell of dimensions a=12.797(3), b=10.776(2), c=19.475 Å and β=98.05(3)° ( V=2659.1 Å 3). The structure was solved by Patterson and Fourier difference methods and refined by full-matrix least-squares techniques to R=0.0380, wR (on F 2)=0.0702 and S=1.058 for 3303 independent reflections and 379 refined parameters. The indium atom coordinates four N iso atoms of the saucer-shaped phthalocyaninato(2-) ligand and apically on iodine atom in a tetragonal pyramidal arrangement. The indium atom is located out of the plane towards the iodine atom by 0.737(3) Å. The In–I distance is 2.672(1) Å, the In–N iso distances range from 2.124(6) to 2.133(7) Å. The phthalocyaninato ligand is severely distorted from planarity (convex distortion). The characteristic frequencies observed in IR and Raman spectroscopy have been assigned and discussed in relation to other metallophthalocyanines.