Startseite Naturwissenschaften Crystal structure of potassium 1H,1H,2H,2H-perfluorooctanesulfonate, C8H4O3F13SK
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Crystal structure of potassium 1H,1H,2H,2H-perfluorooctanesulfonate, C8H4O3F13SK

  • Zhujun Huang und Ji Li ORCID logo EMAIL logo
Veröffentlicht/Copyright: 23. Oktober 2025

Abstract

C8H4O3F13SK, monoclinic, P21/c (no. 14), a = 27.550(3) Å, b = 16.0932(16) Å, c = 9.9834(10) Å, β = 96.686(4)°, V = 4396.3(8) Å3, Z = 4, T = 100 K, Rgt(F) = 0.0559, wRref(F2) = 0.1609.

CCDC no.: 2480493

The molecular structure is shown in the figure. Table 1 contains the crystallographic data and the list of the atoms including atomic coordinates and displacement parameters can be found in the cif-file attached to this article.

Table 1:

Data collection and handling.

Crystal: Colorless plate
Size: 0.15 × 0.10 × 0.02 mm
Wavelength: Ga Kα radiation (1.34139 Å)
μ: 4.04 mm−1
Diffractometer, scan mode: Bruker D8 venture, φ and ω scans
θmax, completeness: 59.1°, 100 %
N(hkl)measured, N(hkl)unique, Rint: 49875, 9446, 0.063
Criterion for Iobs, N(hkl)gt: Iobs > 2 σ(Iobs), 7480
N(param)refined: 812
Programs: Bruker, 1 SHELX, 2 , 3 , 4 Olex2, 5 Diamond 6

1 Source of materials

All the reagents and solvents were used as obtained without further purification. Potassium 1H,1H,2H,2H-perfluorooctanesulfonate (PFOEKS) was obtained from Aldrich Chemical Reagent Company. A small amount of potassium perfluorohexylethanesulfonate (0.5 g) was dissolved in 10 mL of 95 % methanol and slowly evaporated at room temperature (20 °C). After one week, colorless plate crystals were obtained at the bottom of the vessel. Suitable crystals were selected for the X-ray diffraction experiments. Aiming for a better X-ray data collection, crystals were selected and immersed into perfluoroalkylether, which were then cooled down to −173 °C during the measurement.

2 Experimental details

H atoms were placed at their geometrically idealized positions and constrained to ride on their parent atoms with 0.99 Å and Uiso(H) = 1.2Ueq. Some atoms (C12–C16 and F16–F25) are apparently disordered over two positions. The refinement of their positions, bond distances and thermal factors are refined by using commands PART, SAME and EADP. The final outcome of the occupancies for the major and minor components are 0.63(1):0.37(1), respectively.

3 Comment

Low-dose concentrations of metal Cr(III) ions in drinking water may be oxidized into harmful Cr(VI) ions under the action of a small amount of disinfectants or oxidants. 7 Therefore, removal of these potentially harmful high-valent metal ions is of crucial importance. From a chemical perspective, there are many chelating agents which can remove these metal ions, such as polycarboxylic acids and pyridine-based organic ligands. 8 However, most of the metal complexes formed by these ligands tend to precipitate and are not easily transferred to the organic solvent phase for subsequent separation operations. 9 Organic ligands containing fluorine, such as potassium perfluoroalkyl sulfonates, which have both surfactant and metal-ion-chelating functions, are gradually being applied in water purification treatment. 10 These compounds having high surface activity, can significantly reduce the surface tension of water, and have good water solubility and lipophilicity, which can efficiently transfer harmful metal ions in water that are harmful to the human body to the organic solvent phase, achieving the purpose of water purification and facilitating the subsequent separation and treatment of harmful metals. 11 Due to the presence of multiple fluorine atoms in the molecule, these compounds can also have good chemical stability, thermal stability, and weather resistance. Potassium 1H,1H,2H,2H-perfluorooctanesulfonate (PFOEKS) is a new type of chemical reagent for removing Cr(VI) from water, but the crystal structure of this compound has not been reported yet.

It was found that the compound crystallized in the monoclinic crystal system with the space group P21/c. Its asymmetric unit contained three deprotonated perfluorohexylethanesulfonate anions and three potassium ions. The K1 ion formed a distorted octahedral coordination with six O atoms from six different PFOEKS anions. The K2 ion coordinated with nine O atoms from five different PFOEKS anions, among which both two oxygen atoms of two sulfonate ions chelated to one K2 ion. The K3 ion coordinated with seven O atoms from five different PFOEKS anions and one F27 atom, forming a polyhedral coordination. The K–O coordination bond lengths around the three metal ions ranged from 2.672(2) to 3.036(2) Å, and the only K–F coordination bond length was 2.668(2) Å, which are similar to the coordination bond lengths in the some analogs. 12 , 13 , 14 The distances between K1⋯K2, K2⋯K3 and K1⋯K3 are 2.918(2) Å, 3.901(2) Å and 3.660(2) Å, respectively. All the potassium ions are connected by some μ2- and μ3-O bridges, forming a two-dimensional layered structure parallel to the [100] plane. 15 The two sides of the layer are densely covered with alkyl chains containing a large number of fluorine atoms, while in the center of the layer are sulfonate ions and potassium ions that are more hydrophilic. Such a structure further highlights the hydrophilic and lipophilic properties of the compound.


Corresponding author: Ji Li, School of Biological and Environmental Engineering, Guiyang University, Guiyang, 550005, P.R. China, E-mail:

Acknowledgments

Scientific Research Projects for Higher Education Institutions of Guizhou Provincial Department of Education (Youth Projects), The pollution and the influence of aging process of Microplastic in bottled mineral water, No. [2022] 298.

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Received: 2025-08-15
Accepted: 2025-10-06
Published Online: 2025-10-23
Published in Print: 2025-12-17

© 2025 the author(s), published by De Gruyter, Berlin/Boston

This work is licensed under the Creative Commons Attribution 4.0 International License.

Artikel in diesem Heft

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  2. New Crystal Structures
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  4. Refinement of crystal structure of 2-(2,3-dihydro-3-oxo-1 H -inden-1-ylidene)-1 H -indene-1,3(2 H )-dione C18H10O3
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  25. Crystal structure of (4-(1-phenyl-1H-benzo[d]imidazol-2-yl)phenyl)boronic acid, C19H15BN2O2
  26. The crystal structure of (E)-(2-((pyridin-2-ylmethylene)amino)phenyl)arsonic acid, C12H11AsN2O3
  27. The crystal structure of N(benzyl(phenyl)carbomothioyl)benzamide, C21H18N2OS
  28. The crystal structure of bis(2-picolinium) hexachlorostannate dichloromethane monosolvate, C13H18Cl8N2Sn
  29. Crystal structure of poly[tetraaqua-bis(μ4-3–1-(carboxylatomethyl)-1H-1,2,4-triazole-3-carboxylato)-κ4O:O′,O″,N)zinc(II)], C5H7N3O6Zn
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