Single crystals of 2,3,5-triphenyltetrazolium hexachloroantimonate(V), [TPT][SbCl 6 ] (1) and of 1-ethyl-3-methyl-4-chloroimidazolium hexachloroantimonate(V), [Cl-EMIm][SbCl 6 ] (2) could be obtained and their crystal structures determined. Compound 1 crystallizes in the monoclinic space group P2 1 /c (C 2h 5 ) with a ϭ 1328.7(2), b ϭ 1085.2(1), c ϭ 1752.4(3) pm, β ϭ 111.51(1)°, and Z ϭ 4, whereas compound 2 crystallizes in the same monoclinic space group P2 1 /c (C 2h 5 ) with a ϭ 716.9(1), b ϭ
1‐Butyl‐4‐methylpyridinium hexachloridotantalate(V), [BMPy][TaCl6] (1), tetrakis(1‐butyl‐4‐methylpyridinium) bis(hexachloridotantalate(V) (μ‐oxido)‐decachloridotantalate(V), [BMPy]4[(TaCl6)2(Ta2OCl10)] (2), and bis(1‐ethyl‐3‐methylimidazolium)‐(μ‐oxido)‐decachloridoditantalate(V), [EMIm]2[Ta2OCl10] (3) were synthesized and characterized by single‐crystal X‐ray diffraction and vibrational spectroscopy. Compounds 1 and 3 crystallize in the monoclinic space group P21/c (no. 14), whereas compound 2 crystallizes in the triclinic space group P$\bar{1}$ (no. 2). All compounds are built up by the mentioned bulky organic cations and octahedral [TaCl6]– respective linear [Ta2OCl10]2– anions. Coulomb interactions are dominant between the ionic species. FT‐IR and FT‐Raman spectra were recorded and interpreted, especially with respect to the inorganic species [TaCl6]– (Oh) and [Ta2OCl10]2– (Ci symmetry, approximately D4h). The melting temperatures of compounds 1–3 are given.
Single crystals of 2,3,5-triphenyltetrazolium hexachloridoniobate(V) [TPT][NbCl 6 ] (1) and of 2,3,5-triphenyltetrazolium oxidotetrachloridoniobate(V) [TPT][NbOCl 4 (CH 3 CN)] (2) could be obtained and their crystal structures were determined. The structure of 1 is isotypic to that of the recently characterized [TPT][SbCl 6 ] and built up by [TPT] + and octahedral [NbCl 6 ]ions. The ionic compound 2 contains [TPT] + and [NbOCl 4 (CH 3 CN)]ions. The nitrogen atom of the 2273 acetonitrile solvate molecule is coordinated to the niobium ion in the trans-position to the oxido ligand. The Nb-O bond length of 169.6 pm corresponds to a double bond. The [TPT][NbOCl 4 (CH 3 CN)] formation obviously proceeds via NbOCl 3 with the hydrate [TPT]Cl·H 2 O. The FT-Raman and FT-IR/FIR spectra of both compounds were recorded and interpreted, especially with respect to the inorganic structure parts. The melting temperatures of 1 and 2 are given.
4), and 1-butyl-3-methylpyridinium hexachloridoniobate, [1,3-BMPy] [NbCl 6 ] (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]
2,3,5-Triphenyltetrazolium hexachlorophosphate, [C 19 in dry acetonitrile, and their crystal structures were determined by single-crystal X-ray diffraction analysis. In the title compounds, the [TPT] + cations show a face-to-face stacked orientation between the phenyl rings of neighboring molecules, which is caused by intermolecular π ···π interactions. The crystal structure of compound 1 consists of layers of 2,3,5-triphenyltetrazolium cations and hexachlorophosphate anions. In compound 2 the tetrahedral [PO 2 Cl 2 ] − anions exhibit approximate C 2v symmetry with P-O bond lengths from 1.454 to 1.463Å and P-Cl bond lengths from 2.038 to 2.050Å. The Raman spectrum of compound 1 was recorded, and the assignment of the [PCl 6 ] − Raman modes is proposed.
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