Zirconium tetrachloride revisited
Abstract
We present that zirconium tetrachloride, ZrCl 4, is a strategic material with wide-ranging applications. Until now, only one crystallographic study on ZrCl 4has been reported [Krebs (1970).Z. Anorg. Allg. Chem.378, 263–272] and that was more than 40 years ago. The compound used for the previous determination was prepared from ZrO 2 and Cl 2–CCl 4, and single-crystal X-ray diffraction (SCXRD) studies on ZrCl 4 obtained from Zr metal have not yet been reported. In this context, we prepared ZrCl 4 from the reaction of Zr metal and Cl 2 gas in a sealed tube and investigated its structure at 100, 150, 200, 250, and 300 K. At 300 K, the SCXRD analysis indicates that ZrCl 4 crystallizes in the orthorhombic space group Pca2 1 [a= 6.262 (9),b= 7.402 (11),c= 12.039 (17) Å, andV= 558.0 (14) Å 3] and consists of infinite zigzag chains of edge-sharing ZrCl 6 octahedra. This chain motif is similar to that observed previously in ZrCl 4, but the structural parameters and space group differ. Finally, in the temperature range 100–300 K, no phase transformation was identified, while elongation of intra-chain Zr...Zr [3.950 (1) Å at 100 K and 3.968 (5) Å at 300 K] and inter-chainmore »
- Authors:
-
[2];
- Univ. of Nevada, Las Vegas, NV (United States). Department of Chemistry and Biochemistry
- Univ. of Nevada, Las Vegas, NV (United States). Department of Physics and Astronomy
- Sandia National Lab. (SNL-NM), Albuquerque, NM (United States)
- Publication Date:
- Research Org.:
- Sandia National Lab. (SNL-NM), Albuquerque, NM (United States)
- Sponsoring Org.:
- USDOE Office of Nuclear Energy (NE), Fuel Cycle Technologies (NE-5); USDOE National Nuclear Security Administration (NNSA)
- OSTI Identifier:
- 1429669
- Report Number(s):
- SAND-2017-11627J
Journal ID: ISSN 2053-2296; ACSCGG; 658195
- Grant/Contract Number:
- AC04-94AL85000; NE0008449; NA0003525
- Resource Type:
- Accepted Manuscript
- Journal Name:
- Acta Crystallographica. Section C, Structural Chemistry (Online)
- Additional Journal Information:
- Journal Name: Acta Crystallographica. Section C, Structural Chemistry (Online); Journal Volume: 74; Journal Issue: 3; Journal ID: ISSN 2053-2296
- Publisher:
- International Union of Crystallography
- Country of Publication:
- United States
- Language:
- English
- Subject:
- 36 MATERIALS SCIENCE; 37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY; zirconium tetrachloride; crystal structure; chain motif; temperature study
Citation Formats
Borjas Nevarez, Rosendo, Balasekaran, Samundeeswari Mariappan, Kim, Eunja, Weck, Philippe, and Poineau, Frederic. Zirconium tetrachloride revisited. United States: N. p., 2018.
Web. doi:10.1107/S205322961800219X.
Borjas Nevarez, Rosendo, Balasekaran, Samundeeswari Mariappan, Kim, Eunja, Weck, Philippe, & Poineau, Frederic. Zirconium tetrachloride revisited. United States. doi:10.1107/S205322961800219X.
Borjas Nevarez, Rosendo, Balasekaran, Samundeeswari Mariappan, Kim, Eunja, Weck, Philippe, and Poineau, Frederic. Mon .
"Zirconium tetrachloride revisited". United States. doi:10.1107/S205322961800219X. https://www.osti.gov/servlets/purl/1429669.
@article{osti_1429669,
title = {Zirconium tetrachloride revisited},
author = {Borjas Nevarez, Rosendo and Balasekaran, Samundeeswari Mariappan and Kim, Eunja and Weck, Philippe and Poineau, Frederic},
abstractNote = {We present that zirconium tetrachloride, ZrCl4, is a strategic material with wide-ranging applications. Until now, only one crystallographic study on ZrCl4has been reported [Krebs (1970).Z. Anorg. Allg. Chem.378, 263–272] and that was more than 40 years ago. The compound used for the previous determination was prepared from ZrO2 and Cl2–CCl4, and single-crystal X-ray diffraction (SCXRD) studies on ZrCl4 obtained from Zr metal have not yet been reported. In this context, we prepared ZrCl4 from the reaction of Zr metal and Cl2 gas in a sealed tube and investigated its structure at 100, 150, 200, 250, and 300 K. At 300 K, the SCXRD analysis indicates that ZrCl4 crystallizes in the orthorhombic space group Pca21 [a= 6.262 (9),b= 7.402 (11),c= 12.039 (17) Å, andV= 558.0 (14) Å3] and consists of infinite zigzag chains of edge-sharing ZrCl6 octahedra. This chain motif is similar to that observed previously in ZrCl4, but the structural parameters and space group differ. Finally, in the temperature range 100–300 K, no phase transformation was identified, while elongation of intra-chain Zr...Zr [3.950 (1) Å at 100 K and 3.968 (5) Å at 300 K] and inter-chain Cl...Cl [3.630 (3) Å at 100 K and 3.687 (9) Å at 300 K] distances occurred.},
doi = {10.1107/S205322961800219X},
journal = {Acta Crystallographica. Section C, Structural Chemistry (Online)},
number = 3,
volume = 74,
place = {United States},
year = {2018},
month = {2}
}
Search WorldCat to find libraries that may hold this journalFigures / Tables:
Table 1: Crystal data and refinement quality factors for ZrCl4
Works referencing / citing this record:
CCDC 1822235: Experimental Crystal Structure Determination: REWBED : Non-CSD Structure
dataset, February 2018
- Nevarez, R.; Balasekaran, S.; Kim, E.
- Cambridge Structural Database (CSD)
CCDC 1822236: Experimental Crystal Structure Determination: REWBIH : Non-CSD Structure
dataset, February 2018
- Nevarez, R. Borjas; Balasekaran, S. M.; Kim, E.
- Cambridge Structural Database (CSD)
CCDC 1822237: Experimental Crystal Structure Determination: REWBON : Non-CSD Structure
dataset, February 2018
- Nevarez, R. Borjas; Balasekaran, S. M.; Kim, E.
- Cambridge Structural Database (CSD)
CCDC 1822238: Experimental Crystal Structure Determination: REWBUT : Non-CSD Structure
Space Group: P c a 21 (29), Cell: a 6.253(5)Å b 7.383(6)Å c 12.017(9)Å, α 90° β 90° γ 90°
dataset, February 2018
- Borjas Nevarez, R.; Balasekaran, S. M.; Kim, E.
- The Cambridge Crystallographic Data Centre, vp
CCDC 1822239: Experimental Crystal Structure Determination: REWCAA : Non-CSD Structure
dataset, February 2018
- Nevarez, R. Borjas; Balasekaran, S. M.; Kim, E.
- Cambridge Structural Database (CSD)
Figures / Tables found in this record: