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Structural peculiarities of a homologous series of iron(II) cage complexes with ribbed glyoximate, methylglyoximate, and dimethylglyoximate chelate fragments

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Abstract

The crystal and molecular structures of four representatives of the homologous series of iron(ii) clathrochelates FeBd2Gm(BF)2·1.5CHCl3, FeBd2Mm(BF)2·CH2Cl2, FeBd2Dm(BF)2·CH2Cl2, and FeBd2Dm(BF)2·0.5C6H6·0.5iso-C8H18 whose frameworks contain two α-benzyldioximate (Bd) chelate rings and one acyclic α-dioximate fragment (Gm2−, Mm2−, and Dm2− are glyoxime, methylglyoxime, and dimethylglyoxime dianions, respectively) were studied by X-ray diffraction. Two types, A and B, of independent macrobicycles were observed in the unit cell of the crystal FeBd2Gm(BF)2·1.5CHCl3. The geometry of the FeN6 coordination polyhedra of encapsulated iron(ii) ions is intermediate between a trigonal prism (TP) and a trigonal antiprism (TAP). The encapsulated iron(ii) ions occupy centers of the TP-TAP polyhedra. For the macrobicyclic derivatives of dimethylglyoxime, the distortion angles φ(average values 24.0 and 24.7°) are larger than for the glyoximate and methylglyoximate analogs (average values 20.7, 22.6, and 23.2°). The larger trigonal-prismatic distortion of the coordination polyhedron in type-B FeBd2Gm(BF)2 molecules as compared to type-A FeBd2Gm(BF)2 can be explained by a difference in their intermolecular interactions. The carbon-carbon distances in the glyoximate and methylglyoximate ribbed fragments of the clathrochelates FeBd2Gm(BF)2 and FeBd2Mm(BF)2 (average values 1.414 shorter than in the α-benzyldioximate chelate rings (about 1.45 FeBd2Gm(BF)2·1.5CHCl3 and FeBd2Dm(BF)2·CH2Cl2 have laminated structures in which chains of the clathrochelate molecules are differently oriented relative to the axes of the unit cells. The crystals FeBd2Mm(BF)2·CH2Cl2 and FeBd2Dm(BF)2·0.5C6H6·0.5 iso-C8H18 have framework structures and their solvate molecules occupy voids between the dimeric associates and the macrobicyclic molecules, respectively.

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Authors and Affiliations

  1. A. N. Nesmeyanov Institute of Organoelement Compounds, Russian Academy of Sciences, 28 ul. Vavilova, 119991, Moscow, Russian Federation

    Y. Z. Voloshin, A. S. Belov, Z. A. Starikova & A. V. Vologzhanina

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  1. Y. Z. Voloshin
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  2. A. S. Belov
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  3. Z. A. Starikova
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  4. A. V. Vologzhanina
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Correspondence to Y. Z. Voloshin.

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Devoted to the memory of our friend and co-author M. Yu. Antipin (1951–2013).

Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 8, pp. 1858–1865, August, 2013.

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Voloshin, Y.Z., Belov, A.S., Starikova, Z.A. et al. Structural peculiarities of a homologous series of iron(II) cage complexes with ribbed glyoximate, methylglyoximate, and dimethylglyoximate chelate fragments. Russ Chem Bull 62, 1858–1865 (2013). https://doi.org/10.1007/s11172-013-0267-y

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  • DOI: https://doi.org/10.1007/s11172-013-0267-y

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