The preparation of good quality single crystals by diffusion in aqueous silicate gels is a well established technique. Non aqueous gels are not widely used for growing crystals of organic compounds. A mixture of 3:1 toluene and methanol used is too good a solvent to allow crystallization of the metal complexes and organic electron donor acceptor complexes, which are of interest in crystallography. Using this technique single crystals suitable for x-ray measurements (size range 0.2 - 5.0 mm) have been obtained from a number of systems.