Reactions of hydrazine ligands. Part 2. The X-ray structure determination of {7-(3-hydroxypropyl)-16,17-dihydro-15H-dibenzo[f,m][1,11,4,5,7,8]-dithiatetra-azacyclotetradecinato-N6,N9,S14,S18}nickel(II) perchlorate, an unexpected product for a template cyclization in tetrahydrofuran

Abstract

The reactions of 1,3-bis(2,-hydrazinophenylthio)propane with a variety of ketones in tetrahydrofuran solutions of nickel(II) perchlorate have been investigated as part of a programme of study of the reactions of co-ordinated hydrazines. Many of these reactions giveacrystalline by-product in low yield, which is shown to be the perchlorate salt of the macrocyclic monocation : {7-(3-hydroxypropyl)-16,17-dihydro-15H-dibenzo[f,m][1,11,4,5,7,8]dithia-tetra-azacyclotetradecinato-N⁵,N⁹,S¹⁴,S¹⁸}nickel(II) perchlorate. Crystals are monoclinic, space group P2₁/c with a= 9.973(8), b= 14.44(1), c= 17.83(1)Å, β= 124.3(1)°, and Z= 4. Structural refinement based on 2 180 two-circle diffractometer data converged at 0.067.