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New π ligand N,N,N,N′,N′,N′-hexaallylethylenediaminium (L2+): Synthesis and crystal structures of LBr2 · 2H2O and its cuprocomplexes L[CuII(Br0.45Cl3.55)], L[Cu I4 (Br4.55Cl1.45)], and L[Cu I4 Br6]

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Abstract

The alkylation of ethylenediamine with allyl bromide in the presence of a fourfold (with respect to ethylenediamine) molar amount of NaHCO3 in acetone with an ethanol admixture (15: 1) affords LBr2 · 2H2O (I), where L2+ is the N,N,N,N′,N′,N′-hexaallylethylenediaminium cation. Single crystals of complexes L[CuII(Br0.45Cl3.55)] (II), L[Cu I4 (Br4.55Cl1.45)] (III), and L[Cu I4 Br6] (IV) are prepared by ac electrochemical synthesis from an ethanolic solution of LBr2 · 2H2O, CuCl2 · 2H2O (or CuBr2) at copper wire electrodes. The crystal structures of compounds I–IV are determined by X-ray diffraction analysis. The crystals of complex I are monoclinic: space group P21/n, a = 8.544(3), b = 10.404(3), c = 13.350(4) Å, β = 97.29(3)°, V = 1177.2(6) Å3, Z = 2. The bromine anions in compound I are bonded to the L2+ cations and water molecules through hydrogen contacts (E)H…Br (E = O, C) of 2.57(3)–2.86(3) Å. The crystals of compounds II–IV are triclinic: space group P \( \bar 1 \). For II: a = 8.762(4), b = 9.163(4), c = 16.500(6) Å, α = 95.62(4)°, β = 96.39(4)°, γ = 111.46(4)°, V = 1211.4(9) Å3, Z = 2; for III: a = 9.074(4), b = 9.435(4), c = 9.829(5) Å, α = 116.12(4)°, β = 104.14(4)°, γ = 100.22(4)°, V = 692.3(6) Å3, Z = 1; for IV isostructural III: a = 9.084(4), b = 9.404(4), c = 9.869(4) Å, α = 116.31(3)°, β = 104.00(3)°, γ = 100.37(3)°, V = 692.1(5) Å3, Z = 1. Unlike the isolated tetrahedral CuX 2−4 anion in structure II, an original chain anion (Cu4X 2−6 ) n is observed in the structures of π complexes III and IV.

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Authors and Affiliations

  1. Franko National University, ul. Kirilla i Mefodiya 6, Lviv, 79005, Ukraine

    M. M. Monchak, A. V. Pavlyuk & M. G. Mys’kiv

  2. Wroclaw University, ul. F. Joliot-Curie 14, Wroclaw, Poland

    A. V. Pavlyuk & V. V. Kinzhibalo

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  1. M. M. Monchak
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  2. A. V. Pavlyuk
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  3. V. V. Kinzhibalo
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  4. M. G. Mys’kiv
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Correspondence to M. G. Mys’kiv.

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Original Russian Text © M.M. Monchak, A.V. Pavlyuk, V.V. Kinzhibalo, M.G. Mys’kiv, 2009, published in Koordinatsionnaya Khimiya, 2009, Vol. 35, No. 6, pp. 414–419.

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Monchak, M.M., Pavlyuk, A.V., Kinzhibalo, V.V. et al. New π ligand N,N,N,N′,N′,N′-hexaallylethylenediaminium (L2+): Synthesis and crystal structures of LBr2 · 2H2O and its cuprocomplexes L[CuII(Br0.45Cl3.55)], L[Cu I4 (Br4.55Cl1.45)], and L[Cu I4 Br6]. Russ J Coord Chem 35, 405–410 (2009). https://doi.org/10.1134/S1070328409060037

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  • DOI: https://doi.org/10.1134/S1070328409060037

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