Mimoza Gjikaj

Crown-ether enclosure generated by ionic liquid components—synthesis, crystal structure and Raman spectra of compounds of imidazolium based salts and 18-crown-6

Bis(1,3-dimethylimidazolium methylsulfate) [18-crown-6] (1), ([DMIm]2[CH3SO4]2[18-crown-6], bis(1-butyl-3-methylimidazolium methylsulfate) [18-crown-6] (2), ([BMIm]2[CH3SO4]2[18-crown-6]), bis(1-ethyl-3-methylimidazolium methanesulfonate) [18-crown-6] (3), ([EMIm]2 [CH3SO3]2[18-crown-6]) and bis(1-ethyl-3-methylimidazolium trifluoromethanesulfonate) [18-crown-6] (4), ([EMIm]2[CF3SO3]2[18-crown-6]) were prepared and characterized by single-crystal X-ray diffraction, NMR and Raman spectroscopy. Coulomb interactions between the ionic (liquid) components as well as hydrogen bonding are important. No significant close contacts are observed between the ionic components and the 18-crown-6 molecules. Crystal structures of all compounds consist of alternated layers of crown-ether molecules and respective ionic units compounds. Within the layers of the ionic components (compounds 1, 3 and 4), two cations are linked to each other by C–H⋯π interactions between one methyl carbon and the imidazolium ring of another cation.

Structural and spectroscopic elucidation of imidazolium and pyridinium based hexachloridophosphates and niobates

1-Ethyl-3-methylimidazolium hexachloridophosphate, [EMIm][PCl6] (1), 1-ethyl-3-methylimidazolium hexachloridoniobate, [EMIm][NbCl6] (2), 1-butyl-4-methylpyridinium hexachloridophosphate, [1,4-BMPy][PCl6] (3), 1-butyl-4-methylpyridinium hexachloridoniobate, [1,4-BMPy][NbCl6] (4), and 1-butyl-3-methylpyridinium hexachloridoniobate, [1,3-BMPy] [NbCl6] (5) have been synthesized and characterized by single-crystal X-ray diffraction and Raman spectroscopy. All the saltlike compounds crystallize in the monoclinic space group: [EMIm][PCl6] (1): P21/c (no. 14), a = 7.698(1), b = 12.266(2), c = 15.019(2) A, β = 101.45(1)°, V = 1389.9(3) A3 and Z = 4; [EMIm][NbCl6] (2): P21/n (no. 14), a = 20.186(1), b = 7.084(1), c = 20.549(1) A, β = 98.46(1)°, V = 2906.6(4) A3 and Z = 8; [1,4-BMPy][PCl6] (3): P21/c (no. 14), a = 14.681(2), b = 7.242(1), c = 16.157(2) A, β = 101.55(1)°, V = 1683.0(3) A3 and Z = 4; [1,4-BMPy][NbCl6] (4): P21/c (no. 14), a = 15.163(2), b = 7.323(1), c = 16.205(2) A, β = 101.92(1)°, V = 1760.5(4) A3 and Z = 4; [1,3-BMPy][NbCl6] (5): P21/c (no. 14), a = 10.396(1), b = 23.050(2), c = 14.974(2) A, β = 102.28(1)°, V = 3505.9(6) A3 and Z = 8. Title compounds are built up by the mentioned bulky organic cations and octahedral [PCl6]−respective [NbCl6]− anions. No significant hydrogen bonding is observed between the organic cations and respective inorganic anions. FT-Raman spectra of the title compounds have been recorded and interpreted, especially with respect to the inorganic parts [PCl6]− and [NbCl6]−. NMR spectra and the melting temperatures of 1–5 are given.

Chemistry of polyhalogenated nitrobutadienes, 14: Efficient synthesis of functionalized (Z)-2-allylidenethiazolidin-4-ones

Summary The reaction of mercaptoacetic acid esters with pentachloro-2-nitro-1,3-butadiene (1) provides an appropriate precursor for the synthesis of special thiazolidin-4-ones. Applying different anilines as the second constituent for the requisite cyclization step, a series of (Z)-2-allylidenethiazolidin-4-ones was obtained in yields up to 81%. Some subsequent reactions have been examined too, such as the formation of perfunctionalized 1H-pyrazoles upon treatment with hydrazine. Thiazolidinones are as well known for their physiological activities as for their application in optoelectronics.

Crystal structure of catena-poly[[tetra­aqua­magnesium]-μ-(di­hydrogen hypodiphosphato)-κ2O:O′]

[Mg(H2P2O6)(H2O)4] is the first alkaline earth hypodiphosphate to be structurally determined. It consists of (H2P2O6)2− anions that are bridged by Mg2+ cations into a chain structure. Water molecules complete the octahedral coordination sphere of the metal and built up a three-dimensional hydrogen-bonding network.

Rb2P2S6 - a new alkali thiophosphate : Crystal structure and vibrational spectra of rubidium hexathiodiphosphate(V)

Abstract Single crystals of rubidium hexathiodiphosphate(V), Rb2P2S6, have been obtained and investigated by single crystal X-ray diffraction, and IR/FIR and Raman spectroscopy. The title compound crystallizes isotypically to the potassium, caesium and thallium analogues in the orthorhombic space group Immm (no. 71) with a = 8.485(3), b= 6.953(3), c =9.259(3 Å , and Z = 2, final R1= 0.0579 and wR2 = 0.0987. The crystal structure is characterized by discrete [P2S6]2− anions (edge-sharing double-tetrahedra) with D2h symmetry. Rubidium is coordinated by ten sulfur atoms forming a slightly distorted two-capped tetragonal prism with a coordination number CNRb 10. The FT-Raman and FT-IR/FIR spectra have been recorded and a factor group analysis was carried out.

Crystal structure of bis­[tris­(1,10-phenanthroline-κ2N,N′)cobalt(II)] tetra­nitrate N,N′-(1,4-phenyl­enedicarbon­yl)diglycine solvate octa­hydrate

The complex cation of the title compound includes one CoII atom with a distorted octahedral coordination environment defined by six N atoms from three bidentate phenanthroline ligands. The non-coordinating N,N′-(1,4-phenylenedicarbonyl)diglycine ligand links the cationic building blocks via C—H⋯O contacts and through lone-pair⋯π interactions. Further observed non-covalent interactions contribute to the consolidation of the supramolecular network.

Bis[bis­(2,2′-bi­pyridine-κ2N,N′)(carbon­ato-κ2O,O′)cobalt(III)] 2-{4-[(carboxyl­atometh­yl)carbamo­yl]benz­amido}­acetate hexa­hydrate

The complex cation of the title compound, [Co(CO3)(C10H8N2)2]2(C12H10N2O6)·6H2O, contains a CoIII atom with a distorted octahedral coordination environment formed by four N atoms from two bidentate 2,2′-bipyridine ligands and one bidentate carbonate anion. The asymmetric unit is completed by one-half of the 2-({4-[(carboxylatomethyl)carbamoyl]phenyl}formamido)acetate dianion, which is located on a centre of inversion, and by three water molecules. Two [Co(CO3)(C10H8N2)2]+ cations are connected through C—H⋯O contacts by the uncoordinating anions. The aromatic rings of the 2,2′-bipyridine ligands and diacetate anions are involved in π–π stacking and C—H⋯π interactions. The centroid–centroid distances are in the range 3.4898 (4)–3.6384 (5) Å. The crystal structure is stabilized by further O—H⋯O and N—H⋯O hydrogen bonds, which give rise to a three-dimensional supramolecular network.

Ionic Liquids Based on Hexachloridometalate(V) Anions (Sb, Nb and Ta) and Nitrile-functionalized Pyridinium Cations

Single crystals of 1-(cyanoethyl)-3-methyl-pyridin-1-ium hexachloridoantimonate(V) (1), 1- (cyanomethyl)-3-methyl-pyridin-1-ium hexachloridoniobate(V) (2), 1-(cyanomethyl)-3-methylpyridin- 1-ium hexachloridotantalate(V) (3), 1-(cyanopropyl)-3-methyl-pyridin-1-ium hexachloridoniobate( V) (4), and 1-(cyanopropyl)-3-methyl-pyridin-1-ium hexachloridotantalate(V) (5) have been synthesized and characterized by X-ray diffraction. Compounds 1-3 crystallize in the triclinic space group P1̄ with Z = 2, and compounds 4 and 5 in the monoclinic space group C2/c with Z = 8. FTRaman spectra have been recorded and interpreted, especially with respect to the anions [MCl6]-. In addition, NMR spectra, a study of the melting behavior and elemental analyses complete the characterization. Graphical Abstract Ionic Liquids Based on Hexachloridometalate(V) Anions (Sb, Nb and Ta) and Nitrile-functionalized Pyridinium Cations

Hexa­aqua­nickel(II) di­hydrogen hypodiphosphate

The asymmetric unit of the title compound, [Ni(H2O)6](H2P2O6), contains one-half of the hexaaquanickel(II) cation and one-half of the dihydrogen hypodiphosphate anion. In the complex cation, the Ni2+ atom is located on an inversion center and has an octahedral coordination sphere. The P—P distance in the centrosymmetric anion is 2.1853 (7) Å. In the crystal, discrete [Ni(H2O)6]2+ cations and (H2P2O6)2− anions are stacked in columns parallel to the c axis and are linked into a three-dimensional network by medium-strength O—H⋯O hydrogen bonds.

Ethane-1,2-diaminium 2,2'-[tereph-thal-oyl-bis(aza-nedi-yl)]di-acetate tetrahydrate.

In the title salt hydrate, C2H10N2 2+·C12H10N2O6 2−·4H2O, each of the ions is located about a centre of inversion and the asymmetric unit is completed by two water molecules in general positons. In the crystal, the cations, anions and water molecules are connected by O—H⋯O and N—H⋯O hydrogen bonding into a three-dimensional network.