Abstract
The structures oftrans-1NH,8NH- (I) andcis-1NH,8NH-(II)-2,5,7,10,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradeca-4,11-dienenickel(II) diperchlorates have been investigated by X-ray diffractometric methods. CompoundI crystallizes in a monoclinic system, space groupP21,Z=4,a=11.225(1),b=13.710(1),c=15.898(2) Å,β=109.22(1)°. CompoundII crystallizes in an orthorhombic system, space groupP212121,Z=4,a=15.529(2),b=14.129(2),c=10.621(1) Å. The structures were solved by the heavy-atom method followed by a series of Fourier syntheses, and refined by full-matrix least squares to give forI andII R=0.051 (for 3787 independent reflections) andR=0.048 (for 1494 reflections), respectively. Conformational analysis of chelate rings and of the macrocyclic ring was performed forI andII, and the results were compared with those of some known 1,4,8,11-tetraazacyclotetradeca-4,11-dienenickel (II) complexes. A novel conformation of the macrocycle was found in cationI. Conformations of the methyl groups are forI andII 2(a),7(e),10(a),14(e) and 2(a),7(e),10(a),14(a), respectively, with a 1,3-syn-axial interaction of the 2,14-methyl groups inII. The absolute configuration of cationI is 1N(S), 2(R), 7(R), 8N(S), 10(R), 14(S), and differs from that of cationII by 1N(R) exclusively (1N-epimeric compounds).
Similar content being viewed by others
References
Bucourt, R. (1974)Top. Stereochem. 8, 159–224.
Cremer, D., and Pople, J. A. (1975)J. Amer. Chem. Soc. 97, 1354–1358.
Curtis, N. F. (1968)Coord. Chem. Rev. 3, 3–47.
Curtis, N. F. (1979) InCoordination Chemistry of Macrocyclic Compounds, Melson, G. A., ed. (Plenum Press, New York), pp. 219–344.
Duax, W. L., Weeks, C. M., and Roher, D. C. (1976)Top. Stereochem. 9, 271–383.
Gluziński, P. (1986)Isom, Program for Estimation of Isomorphism of Two Crystallographically Determined Molecules or Their Fragments (Institute of Organic Chemistry, Polish Academy of Sciences, Warsaw, Poland).
Gusiev, A. I., Krajewski, J. W., and Urbańczyk, Z. (1974)Bull. Acad. Polon. Sci. Ser. Sci. Chim. 22, 387–392.
International Tables for X-Ray Crystallography (1976) Vol. IV (Kynoch Press, Birmingham, England).
IUPAC Nomenclature of Inorganic Chemistry, Definitive Rules 1970. Rules 7.83 and 7.88 (1971)Pure Appl. Chem. 28, 1–110.
Koliński, R. A., and Korybut-Daszkiewicz, B. (1975)Inorg. Chim. Acta 14, 237–245.
Koliński, R. A., Kubaj, Z., and Kasprzyk, St. P. (1988a)Inorg. Chim. Acta (in press).
Koliński, R. A., Kubaj, Z., Kasprzyk, St. P., and Korybut-Daszkiewicz, B. (1988b)Inorg. Chim. Acta. (in press).
Krajewski, J. W., Urbańczyk-Lipkowska, Z., and Gluziński, P. (1974)Bull. Acad. Polon. Sci. Ser. Sci. Chim. 22, 955–958.
Krajewski, J. W., Urbańczyk-Lipkowska, Z., and Gluziński, P. (1977)Roczniki Chem. 51, 2385–2393.
Párkányi, L. (1979)Ring, Program for conformational analysis (Central Research Institute for Chemistry, Hungarian Academy of Sciences, Budapest, Hungary).
Sheldrick, G. M. (1976).Shelx 76, Program for crystal structure determination and refinement (University of Cambridge, England).
Stewart, J. M., Kundell, F. A., and Baldwin, J. C. (1976) X-Ray 76 System (Computer Science Center, University of Maryland, College Park, Maryland).
Urbańczyk-Lipkowska, Z., Krajewski, J. W., Gluziński, P., and Párkányi, L. (1983)Polish J. Chem. 57, 85–92.
Walker, N., and Stuart, D. (1983)Acta Crystallogr. A39, 158–166.
Warner, L. G., Rose, N. J., and Busch, D. H. (1968)J. Amer. Chem. Soc. 90, 6938–6946.
Author information
Authors and Affiliations
Rights and permissions
About this article
Cite this article
Gluziński, P., Koliński, R.A., Krajewski, J.W. et al. X-ray structural investigation of two optically active 1N-epimers of 2,5,7,10,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradeca-4,11-dienenickel(II) diperchlorate. A novel conformation of the macrocyclic ligand. Journal of Crystallographic and Spectroscopic Research 19, 51–70 (1989). https://doi.org/10.1007/BF01160843
Received:
Issue Date:
DOI: https://doi.org/10.1007/BF01160843