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Synthesis and structure of catena((μ2-4,4,10,10-tetramethyl-1,3,7,9-tetraazaspiro[5.5]undecane-2,8-dione-O,O′)dichloro-zinc)

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Abstract

The coordination polymer, catena-((μ2-4,4,10,10-tetramethyl-1,3,7,9-tetraazaspiro[5.5]undecane-2,8-dione-O,O′)dichloro-zinc) {[Zn(C11H20N4O2)Cl2]} n (I), is prepared for the first time from zinc chloride and bicyclic bis(urea), 4,4,10,10-tetramethyl-1,3,7,9-tetraazaspiro[5.5]undecane-2,8-dione, and investigated by X-ray diffraction (CIF file CCDC no. 877812). The crystals of I are monoclinic: space group P21, a = 6.2121(17), b = 11.276(3), c = 11.387(3) Å, β = 94.99(3)°, V = 794.6(3) Å3, ρ(calcd.) = 1.574 g/cm3, Z = 2. The singe-phase nature of the powder sample of I is confirmed by Rietveld refinement of the powder X-ray diffraction pattern; at 293 K, a = 6.20369(11), b = 11.23336(18), c = 11.36013(16) Å, β = 95.3001(11)°, V = 788.28(2) Å3. The content of the major phase I in the sample is 100 ± 1%, no impurity lines are found. The zinc coordination polyhedron in the coordination polymer chain is a tetrahedron with vertices being occupied by two chlorine atoms and carbonyl O(1) and O(2) atoms of two TTSU molecules related by the symmetry code (2 − x, 1/2 + y, 2–z). The zinc bond angles are 101.05(12)°–122.13(9)°. The Zn···Zn distance in the polymer is 9.480(2) Å. The chains in the coordination polymers are additionally combined by intermolecular hydrogen bonds, N(2)–H(2)···O(2)i (i 2–x, 1/2 + y, 2 − z) (H···O 2.17 Å, N−H···O 147°) and N(4)–H(4)···Cl(2)ii (ii 1–x, −1/2 + y, 2–z) (H···Cl 2.48 Å, N−H···Cl 159°). The chains are joined into layers along the (0 0 1) plane by intermolecular hydrogen bonds, N(1)−H(1)···Cl(1)iii (iii 1 − x, −1/2 + y, 2–z) (H···Cl 2.78 Å, N−H···Cl 148°).

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Authors and Affiliations

  1. Taurida Academy, Vernadsky Federal University, Simferopol, Russia

    E. E. Netreba

  2. Lobachevsky National Research University, Nizhny Novgorod, Russia

    N. V. Somov

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  1. E. E. Netreba
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  2. N. V. Somov
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Correspondence to E. E. Netreba.

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Original Russian Text © E.E. Netreba, N.V. Somov, 2017, published in Koordinatsionnaya Khimiya, 2017, Vol. 43, No. 7, pp. 416–420.

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Netreba, E.E., Somov, N.V. Synthesis and structure of catena((μ2-4,4,10,10-tetramethyl-1,3,7,9-tetraazaspiro[5.5]undecane-2,8-dione-O,O′)dichloro-zinc). Russ J Coord Chem 43, 441–445 (2017). https://doi.org/10.1134/S1070328417070077

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  • DOI: https://doi.org/10.1134/S1070328417070077

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