Комплексы меди [CuBr2(DMSO-O)3] и [Cu(DMSO-O)4SF6]. Синтез и строение

V. S. Senchurin; D. P. Shevchenko; V. V. Sharutin

Authors

V. S. Senchurin South Ural State University
D. P. Shevchenko South Ural State University
V. V. Sharutin South Ural State University

Keywords:

copper bromide, copper fluoride, dimethyl sulfoxide, synthesis, structure, X-ray analysis

Abstract

The dissolution of copper (II) bromide and copper (II) fluoride in the presence of hydrofluoric acid in dimethyl sulfoxide, followed by slow evaporation of the solvent, have synthesized copper complexes [CuBr₂(DMSO-O)₃] (1) and [Cu(DMSO-O)₄SF₆] (2). They have been structurally characterized. The X-ray diffraction pattern has been obtained at 293 K on an automatic diffractometer D8 Quest Bruker (MoK_α-radiation, λ = 0.71073 Å, graphite monochromator) of crystals 1 [C₆H₁₈O₃S₃Br₂Cu, M 457,74, the monoclinic syngony, the symmetry group P2₁/c; cell parameters: a 8.812(6), b 15.335(11), c 12.272(8) Å, α = 90.00 degrees, β = 105.82(3) degrees,
γ = 90,00 degrees; V = 1595.5(19)Å³; the crystal size is 0.59 × 0.32 × 0,24 mm; intervals of reflection indexes are –13 ≤ h ≤ 11, –23 ≤ k ≤ 23, –18 ≤ l ≤ 18; total reflections 45529; independent reflections 5832; R_int 0.0971; GOOF 1.001; R₁ = 0.0497, wR₂ = 0.1073; residual electron density 0.77/–1.36 e/Å³] and 2 [C₈H₂₄O₄F₆S₅Cu, M 522.11, the triclinic syngony, the symmetry group
P–1; cell parameters: a 10.325(18), b 10.428(18), c 10.60(2) Å, α = 77.93(11) degrees,
β = 89.49(9) degrees, γ = 68.12(6) degrees; V = 1033(3) Å³; the crystal size is 0.47×0.16×0.13 mm; intervals of reflection indexes are –11 ≤ h ≤ 11, –12 ≤ k ≤ 12, –12 ≤ l ≤ 12; total reflections 9324; independent reflections 3307; R_int 0.0709; GOOF 1.029; R₁ = 0.0555, wR₂ = 0.1309; residual electron density 0.64/–0.82 e/Å³], the copper atoms have a distorted square-pyramidal coordination (the trans-OCuO and trans-OCuBr angles are 165.68(11)° and 143.37(10)° (1); trans-OCuO are 163.8(2), 169.0(2)° (2); the Cu-Br and Cu-O bond lengths are 2.4681(14) Å and 2.5922(14) Å (1), 1.944(3)–2.054(3) Å (1) and 1.940(6)–1.956(5) Å (2) respectively). Fragment SF₆ in 2 (the FSF trans-angles 178.8(2)–179.7(3)°, cis-angles 88.7(2)–91.0(3)°) linked to the central copper atom (the Cu–F bond length 2.208(6) Å). The structural organization of crystals 1 and 2 is controlled by intermolecular bonds O_(DMSO)∙∙∙H–С_(DMSO) (2,57 Å) and Cu–Br∙∙∙H–C_(DMSO) (2.89–3.04 Å) (1), S–F∙∙∙H–C_(DMSO) (2.32–2.60 Å) (2). Complete tables of coordinates of atoms, bond lengths and valence angles for structures 1 and 2 are deposited at the Cambridge Structural Data Bank (no. 1883471, 1898916; deposit@ccdc.cam.ac.uk; https://www.ccdc.cam.ac.uk).

Author Biographies

V. S. Senchurin, South Ural State University

доктор химических наук, профессор, кафедра теоретической и прикладной химии

D. P. Shevchenko, South Ural State University

студент

V. V. Sharutin, South Ural State University

доктор химических наук, профессор, главный научный сотрудник Управления научной и инновационной деятельности

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