Synthesis and crystal structure of (2.2.2-cryptand)potassium perchlorate

Synthesis and crystal structure of (2.2.2-cryptand)potassium perchlorate A new complex (2.2.2-cryptand)potassium perchlorate [K(Crypt-222)]ClO4 is synthesized, and its structure is studied by X-ray diffraction analysis (space group R32, a = 8.441 Å, c = 30.475 Å, Z = 3). The structure is solved by the direct method and refined by the full-matrix least-squares method in the anisotropic approximation to R = 0.032 for 1222 independent (with allowance for anomalous dispersion) reflections (CAD4 automated diffractometer, λMoK α radiation). The centers of the ClO 4 − anion and [K(Crypt-222)]+ complex cation are in the positions (0,0,0) and (0,0,1/2), respectively, with the point symmetry 32. The ClO 4 − anion is randomly disordered. The complex cation (with the high symmetry D 3) is of the host-guest type and is somewhat disordered and exists as two different conformations with probabilities of 87 and 13%. The coordination polyhedron of the K+ cation (coordination number 8) is a two-base-centered trigonal prism distorted toward antiprism. http://www.deepdyve.com/assets/images/DeepDyve-Logo-lg.png Russian Journal of Coordination Chemistry Springer Journals

Synthesis and crystal structure of (2.2.2-cryptand)potassium perchlorate

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Publisher
Springer Journals
Copyright
Copyright © 2006 by Pleiades Publishing, Inc.
Subject
Chemistry; Inorganic Chemistry; Physical Chemistry
ISSN
1070-3284
eISSN
1608-3318
D.O.I.
10.1134/S1070328406110042
Publisher site
See Article on Publisher Site

Abstract

A new complex (2.2.2-cryptand)potassium perchlorate [K(Crypt-222)]ClO4 is synthesized, and its structure is studied by X-ray diffraction analysis (space group R32, a = 8.441 Å, c = 30.475 Å, Z = 3). The structure is solved by the direct method and refined by the full-matrix least-squares method in the anisotropic approximation to R = 0.032 for 1222 independent (with allowance for anomalous dispersion) reflections (CAD4 automated diffractometer, λMoK α radiation). The centers of the ClO 4 − anion and [K(Crypt-222)]+ complex cation are in the positions (0,0,0) and (0,0,1/2), respectively, with the point symmetry 32. The ClO 4 − anion is randomly disordered. The complex cation (with the high symmetry D 3) is of the host-guest type and is somewhat disordered and exists as two different conformations with probabilities of 87 and 13%. The coordination polyhedron of the K+ cation (coordination number 8) is a two-base-centered trigonal prism distorted toward antiprism.

Journal

Russian Journal of Coordination ChemistrySpringer Journals

Published: Nov 6, 2006

References

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