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Title: The synthesis and structural characterization of the new ternary nitrides: Ca{sub 4}TiN{sub 4} and Ca{sub 5}NbN{sub 5}

Abstract

The ternary nitrides, Ca{sub 4}TiN{sub 4} and Ca{sub 5}NbN{sub 5}, were synthesized in sealed niobium tubes using lithium nitride as a flux at 900 and 1050 deg. C, respectively. The structures of both compounds were solved from single-crystal X-ray diffraction data. Ca{sub 4}TiN{sub 4} is the first example of a calcium group IV nitride; it crystallizes in the triclinic space group P1-bar (No. 2) with cell parameters a=5.9757(5) A, b=6.0129(5) A, c=6.0116(12) A, {alpha}=71.565(4){sup o}, {beta}=79.471(4){sup o}, {gamma}=68.258(4){sup o} and Z=2. Ca{sub 4}TiN{sub 4} is isostructural with Na{sub 4}TiO{sub 4} and contains tetrahedral TiN{sub 4} units connected through edges and corners to CaN{sub 4} tetrahedra and CaN{sub 5} square pyramids. Ca{sub 5}NbN{sub 5} crystallizes in the monoclinic space group C2/m (No. 12) with cell parameters a=11.922(7) A, b=6.878(5) A, c=8.936(7) A, {beta}=101.22(3){sup o} and Z=4. Ca{sub 5}NbN{sub 5} is isostructural with Ba{sub 5}NbN{sub 5}; the structure contains NbN{sub 4} tetrahedra that share vertices with CaN{sub 5} trigonal bipyramids.

Authors:
 [1];  [2];  [2];  [2];  [2]
  1. Department of Chemistry, Cornell University, Ithaca, NY 14853 (United States), E-mail: jhunting@fandm.edu
  2. Department of Chemistry, Cornell University, Ithaca, NY 14853 (United States)
Publication Date:
OSTI Identifier:
21015615
Resource Type:
Journal Article
Resource Relation:
Journal Name: Journal of Solid State Chemistry; Journal Volume: 180; Journal Issue: 1; Other Information: DOI: 10.1016/j.jssc.2006.09.018; PII: S0022-4596(06)00528-7; Copyright (c) 2006 Elsevier Science B.V., Amsterdam, The Netherlands, All rights reserved; Country of input: International Atomic Energy Agency (IAEA)
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY; CALCIUM NITRIDES; LITHIUM NITRIDES; MONOCLINIC LATTICES; MONOCRYSTALS; NIOBIUM NITRIDES; SPACE GROUPS; SYNTHESIS; TITANIUM NITRIDES; X-RAY DIFFRACTION

Citation Formats

Hunting, Janet L., Szymanski, Marta M., Johnson, Philip E., Brenhin Kellar, C., and DiSalvo, Francis J.. The synthesis and structural characterization of the new ternary nitrides: Ca{sub 4}TiN{sub 4} and Ca{sub 5}NbN{sub 5}. United States: N. p., 2007. Web. doi:10.1016/j.jssc.2006.09.018.
Hunting, Janet L., Szymanski, Marta M., Johnson, Philip E., Brenhin Kellar, C., & DiSalvo, Francis J.. The synthesis and structural characterization of the new ternary nitrides: Ca{sub 4}TiN{sub 4} and Ca{sub 5}NbN{sub 5}. United States. doi:10.1016/j.jssc.2006.09.018.
Hunting, Janet L., Szymanski, Marta M., Johnson, Philip E., Brenhin Kellar, C., and DiSalvo, Francis J.. Mon . "The synthesis and structural characterization of the new ternary nitrides: Ca{sub 4}TiN{sub 4} and Ca{sub 5}NbN{sub 5}". United States. doi:10.1016/j.jssc.2006.09.018.
@article{osti_21015615,
title = {The synthesis and structural characterization of the new ternary nitrides: Ca{sub 4}TiN{sub 4} and Ca{sub 5}NbN{sub 5}},
author = {Hunting, Janet L. and Szymanski, Marta M. and Johnson, Philip E. and Brenhin Kellar, C. and DiSalvo, Francis J.},
abstractNote = {The ternary nitrides, Ca{sub 4}TiN{sub 4} and Ca{sub 5}NbN{sub 5}, were synthesized in sealed niobium tubes using lithium nitride as a flux at 900 and 1050 deg. C, respectively. The structures of both compounds were solved from single-crystal X-ray diffraction data. Ca{sub 4}TiN{sub 4} is the first example of a calcium group IV nitride; it crystallizes in the triclinic space group P1-bar (No. 2) with cell parameters a=5.9757(5) A, b=6.0129(5) A, c=6.0116(12) A, {alpha}=71.565(4){sup o}, {beta}=79.471(4){sup o}, {gamma}=68.258(4){sup o} and Z=2. Ca{sub 4}TiN{sub 4} is isostructural with Na{sub 4}TiO{sub 4} and contains tetrahedral TiN{sub 4} units connected through edges and corners to CaN{sub 4} tetrahedra and CaN{sub 5} square pyramids. Ca{sub 5}NbN{sub 5} crystallizes in the monoclinic space group C2/m (No. 12) with cell parameters a=11.922(7) A, b=6.878(5) A, c=8.936(7) A, {beta}=101.22(3){sup o} and Z=4. Ca{sub 5}NbN{sub 5} is isostructural with Ba{sub 5}NbN{sub 5}; the structure contains NbN{sub 4} tetrahedra that share vertices with CaN{sub 5} trigonal bipyramids.},
doi = {10.1016/j.jssc.2006.09.018},
journal = {Journal of Solid State Chemistry},
number = 1,
volume = 180,
place = {United States},
year = {Mon Jan 15 00:00:00 EST 2007},
month = {Mon Jan 15 00:00:00 EST 2007}
}