Crystal structure, quantum mechanical investigation, IR and NMR spectroscopy of two new organic perchlorates: (C6H18N3)·(ClO4)3H2O (I) and (C9H11N2)·ClO4(II)
| Autor: | Frédéric Lefebvre, Valeria Ferretti, C. Ben Nasr, Sarra Soudani, I. Bayar, L. Khedhiri |
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| Rok vydání: | 2018 |
| Předmět: |
Infrared spectroscopy
02 engineering and technology Crystal structure Triclinic crystal system DFT calculations 010402 general chemistry Solid-state NMR 01 natural sciences NO Analytical Chemistry Inorganic Chemistry HOMO/LUMO Spectroscopy Chemistry Hirshfeld surface Organic Chemistry Nuclear magnetic resonance spectroscopy 021001 nanoscience & nanotechnology 0104 chemical sciences Crystallography Single crystal X-ray diffraction analysis 0210 nano-technology Hydrate Single crystal Monoclinic crystal system |
| Zdroj: | Journal of Molecular Structure. 1161:486-496 |
| ISSN: | 0022-2860 |
| Popis: | The reaction of perchloric acid with 1-(2-aminoethyl)piperazine or 5,6-dimethyl-benzimidazole results in the formation of 1-(2-amonioethyl)piperazine-1,4-dium triperchlorate hydrate (C6H18N3)·(ClO4)3·H2O (I) or 5,6-dimethyl-benzylimidazolium perchlorate (C9H11N2)·ClO4 (II). Both compounds were fully structurally characterized including single crystal X-ray diffraction analysis. Compound (I) crystallizes in the centrosymmetric triclinic space group P 1 ¯ with the lattice parameters a = 7.455 (2), b = 10.462 (2), c = 10.824 (2) A, α = 80.832 (2), β = 88.243 (2), γ = 88.160 (2) °, Z = 2 and V = 832.77 (3) A3. Compound (II) has been found to belong to the P21/c space group of the monoclinic system, with a = 7.590 (3), b = 9.266 (3), c = 16.503 (6) A, β = 107.38 (2) °, V = 1107.69 (7) A3 and Z = 4. The structures of (I) and (II) consist of slightly distorted [ClO4]- tetrahedra anions and 1-(2-amonioethyl)piperazine-1,4-dium trication (I) or 5,6-dimethyl-benzylimidazolium cations (II) and additionally a lattice water in (I). The crystal structures of (I) and (II) exhibit complex three-dimensional networks of H-bonds connecting all their components. In the atomic arrangement of (I), the ClO4− anions form corrugated chains, while in (II) the atomic arrangement exhibits wide pseudo-hexagonal channels of ClO4 tetrahedra including the organic entities. The lattice water serves as a link between pairs of cations and pairs of anions via several O H⋯O and N-H⋯O interactions in compound (I). The vibrational absorption bands were identified by infrared spectroscopy. These compounds were also investigated by solid-state 13C, 35Cl and 15N NMR spectroscopy. DFT calculations allowed the attribution of the IR and NMR bands. Intermolecular interactions were investigated by Hirshfeld surfaces. Electronic properties such as HOMO and LUMO energies were derived. |
| Databáze: | OpenAIRE |
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