
%0 Journal Article
%A Curtis, NF 
%A Gainsford, GJ 
%T Studies of Some Tetraazacyclopentadecadiene Complexes of Nickel(II). The Crystal and Molecular-Structure of (1RS,8SR)-(5,7,7,13,15,15-Hexamethyl-1,4,8,12-Tetraazacyclopentadeca-4,1 2-Diene)Nickel(II) Perchlorate Hydrate
%J Australian Journal of Chemistry
%D 1986/10/01
%V 39
%N 10
%P 1509-1523
%K 
%R https://doi.org/10.1071/CH9861509
%U https://www.publish.csiro.au/paper/CH9861509 
%X The crystal and molecular structure has been determined by X-ray diffractometry for the singlet ground state nickel(II) compound of a fifteen- membered  tetraaza  macrocyclic  ligand , formed by reaction of a mixture of tris ( ethanediamine )nickel(II) and tris (propane-1,3- diamine )nickel(II) perchlorates with acetone. The compound, (1RS,8SR)- 5,7,7,13,15,15-hexamethyl-1,4,8,12-tetraazacyclopentadeca-4,12- diene )nickel(II) perchlorate hydrate, [Ni( hmpd )](ClO4)2.H2O, is monoclinic, space group P21/C, a 1158.76(14), b 1319.53(22), c 1630.35(21) pm, &#946; 96.209(10)&#176;, R 0.046, Rw 0.062 for 2798 reflections. The nickel(II) ion is in tetrahedrally distorted square-planar coordination [mean Ni-N distances 188.9 pm ( imine ), 191.9 pm (amine), displacements of nitrogens c. ±20 pm from mean coordination plane]. Triplet ground state compounds [Ni( hmpd )( acac )]ClO4 and [{Ni( hmpd )}2C2O4](ClO4)2, with the macrocycle in folded coordination, were prepared and converted into an isomeric form of [Ni( hmpd )](ClO4)2. The 3,5,7,7,13,15,15-heptamethyl homologue of [Ni( hmpd )]2+ was prepared by reaction of tris (propane-1,2-diamine)- and tris (propane-1,3-diamine)- nickel(II) perchlorates with acetone. The electronic (d-d), 1H N.M.R. and 13C N.M.R . spectra of compounds of these macrocyclic  cations, and of (5,5,7,13,15,15-hexamethyl-1,4,8,12-tetraazacyclopentadeca-7,12-diene) nickel(II) are reported. 
