Abstract
The structure of molecular compoundI (2IA·IB·2H2O), whereIA is a square-planar 2(e),5,9(a),12-tetramethyl-1,8-cis-1,4,8,11-tetraazacyclotetradeca-4,11-dienenickel(II) diperchlorate andIB is an octahedraltrans-diaquo-2(e),5,9(e),12-tetramethyl-1,8-trans-1,4,8,11-tetraazacyclotetradeca-4,11-dienenickel(II) diperchlorate has been investigated by X-ray diffractometric methods. Compound I crystallizes in an orthorhombic system, space groupPbca, Z=12,a=26.321(3),b=19.919(2),c=13.306(1) Å. The structure was solved by the heavy-atom method followed by a series of Fourier syntheses and refined by full-matrix least-squares to giveR=0.060 (for 3757 independent reflections).
Conformations were ascribed to chelate rings and to the macrocyclic rings ofIA andIB, and the results were compared with those of some known 1,4,8,11-tetraazacyclotetradeca-4,11-dienenickel(II) complexes. The relative configurations were found 1RS,2SR,8RS,9RS (a racemate) forIA and 1R,2S,8S,9R (ameso-form) forIB. They differ each from the other by configuration on one nitrogen centre (N-epimeric compounds).
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Gluziński, P., Koliński, R.A., Krajewski, J.W. et al. X-ray structural investigation of paramagnetic molecular compound of 2,5,9,12-tetramethyl-1,8-cis-1,4,8,11-tetraazacyclotetradeca-4,11-dienenickel(II) diperchlorate,trans-diaquo-2,5,9,12-eramehyl-1,8-trans-1,4,8,11-tetraazacyclotetradeca-4,11-dienenickel(II) diperchlorate, and water 2[cis-C14H28N4Ni](ClO4)2·[trans-C14H28N4Ni· 2H2O](ClO4)2·2H2O. Journal of Crystallographic and Spectroscopic Research 20, 271–278 (1990). https://doi.org/10.1007/BF01187253
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DOI: https://doi.org/10.1007/BF01187253