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

A new complex of iodophthalocyaninato(2-) indate(III) has been synthesized in crystalline form by the reaction of indium powder with 1;2-dicyanobenzen e under a stream of iodine at about 200 degrees C. It crystallizes in the m onoclinic system, space group P2(t)/n,ln with Z=4 in a unit cell of dimensi ons a= 12.797(3), b = 10.776(2), c = 19.475 Angstrom and B = 98.05(3)degree s (V = 2659.1 Angstrom(3)). The structure was solved-by Patterson and Fouri er difference methods and refined by full-matrix least-Squares techniques t o R = 0.0380, wR (on F-2) =0.0702 and S=1.058 for 3303 independent reflecti ons and 379 refined parameters. The indium atom coprdinates four Ni,, atoms of the saucer-shaped phthalocyaninato(2-) ligand and apically on iodine at om in a tetragonal pyramidal arrangement. The indium atom is located out of the plane towards the iodine-atom by 0;737(3) A. The In-I distance is 2.67 2(1) A,:the In-N-iso,SO distances range from 2.124(6):to 2.133(7) A. The ph thalocyaninato ligand is severely distorted from planarity (convex distorti on). The characteristic frequencies observed in IR and Raman spectroscopy h ave been assigned and discussed in relation to other metallophthalocyanines . (C) 1999 Elsevier Science S.A. All rights reserved.