An unusual hydrated complex of 1,4,7,10,13-pentaoxacyclohexadecane-14,16-dione (L) with calcium thiocyanate, C26H48Ca2N4O20S4 (I), was synthesized and studied by X-ray diffraction analysis (CAD4 automated diffractometer, λMoK α radiation). The unit cell parameters are as follows: a = 31.293 Å, b = 9.756 Å, c = 14.253 Å, space group Pca21, Z = 4. Structure I was solved by the direct method and refined by the full-matrix least-squares method in the anisotropic approximation (final R = 0.075 for all 5187 measured independent reflections). In crystal form, complex I is composed of oppositely charged complex ions [CaL2(H2O)4]2+ (I 1) and [Ca(NCS)4(H2O)2]2– (I 2) united by an infinite three-dimensional net of hydrogen bonds. The coordination polyhedron of Ca2+ in ion I 1 (CN = 7) is a distorted octahedron with a bifurcate vertex. This Ca2+ cation is not located in the cavities of either of the crown ligands L and is not coordinated by any of the ether O atoms. The coordination polyhedron of Ca2+ in ion I 2 (CN = 6) is a distorted octahedron with two cis-arranged water molecules. This Ca2+ cation is also coordinated by the nitrogen atoms of four SCN– anions.
Russian Journal of Coordination Chemistry – Springer Journals
Published: Oct 13, 2004
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