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High-Pressure Synthesis and Crystal Structures of β-MNCl (M=Zr and Hf)

✍ Scribed by Xuean Chen; Takeshi Koiwasaki; Shoji Yamanaka

Publisher
Elsevier Science
Year
2001
Tongue
English
Weight
532 KB
Volume
159
Category
Article
ISSN
0022-4596

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✦ Synopsis

The single crystals of two kinds of metal nitride halides, -ZrNCl and -HfNCl, have been grown for the 5rst time in the presence of NH 4 Cl under a high pressure of 3 GPa at 9003C and 12003C, respectively. Their crystal structures have been re5ned on the basis of X-ray four-circle di4ractometer data. -ZrNCl crystallizes in the rhombohedral space group R-3m; a ‫؍‬ 3.6046(4) A s , c ‫؍‬ 27.672(4) A > , and Z ‫؍‬ 6; R1/wR2 ‫؍‬ 0.0270/0.0751 for 447 observed re6ections and 11 variables. For the isostructural compound -HfNCl, a ‫؍‬ 3.5767(8) A s , c ‫؍‬ 27.711(7) A > ; R1/wR2 ‫؍‬ 0.0372/0.0979 for 454 observed re-6ections. The compounds are isotypic with SmSI and composed of structural slabs [Cl+M +N+N+M+Cl] (M ‫؍‬ Zr, Hf ) with close-packed anion layers. Three of those slabs are stacked rhombohedrally in the unit cell along the c-axis and held together by Cl 2 Cl van der Waals interactions. The metal atoms (M) are placed in the octahedral sites between the Cl and N layers, leading to the overall layer sequence of Cl

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