Journal of the American Chemical Society, volume 135, issue 44, pages 16668-16679
High-Pressure Synthesis and Characterization of Li2Ca3[N2]3—An Uncommon Metallic Diazenide with [N2]2– Ions
Sebastian B Schneider
1
,
Markus Seibald
1
,
Ralf P. Stoffel
,
Rainer Frankovsky
1
,
Gina M Friederichs
1
,
Henryk Laqua
2
,
Viola Duppel
3
,
Gunnar Jeschke
2
,
Wolfgang Schnick
1
2
Publication type: Journal Article
Publication date: 2013-10-28
Quartile SCImago
Q1
Quartile WOS
Q1
Impact factor: 15
ISSN: 00027863, 15205126
General Chemistry
Catalysis
Biochemistry
Colloid and Surface Chemistry
Abstract
Dinitrogen (N2) ligation is a common and well-characterized structural motif in bioinorganic synthesis. In solid-state chemistry, on the other hand, homonuclear dinitrogen entities as structural building units proved existence only very recently. High-pressure/high-temperature (HP/HT) syntheses have afforded a number of binary diazenides and pernitrides with [N2](2–) and [N2](4–) ions, respectively. Here, we report on the HP/HT synthesis of the first ternary diazenide. Li2Ca3[N2]3 (space group Pmma, no. 51, a = 4.7747(1), b = 13.9792(4), c = 8.0718(4) Å, Z = 4, wRp = 0.08109) was synthesized by controlled thermal decomposition of a stoichiometric mixture of lithium azide and calcium azide in a multianvil device under a pressure of 9 GPa at 1023 K. Powder X-ray diffraction analysis reveals strongly elongated N–N bond lengths of dNN = 1.34(2)–1.35(3) Å exceeding those of previously known, binary diazenides. In fact, the refined N–N distances in Li2Ca3[N2]3 would rather suggest the presence of [N2](3·–) radical ions. Also, characteristic features of the N–N stretching vibration occur at lower wavenumbers (1260–1020 cm(–1)) than in the binary phases, and these assignments are supported by first-principles phonon calculations. Ultimately, the true character of the N2 entity in Li2Ca3[N2]3 is probed by a variety of complementary techniques, including electron diffraction, electron spin resonance spectroscopy (ESR), magnetic and electric conductivity measurements, as well as density-functional theory calculations (DFT). Unequivocally, the title compound is shown to be metallic containing diazenide [N2](2–) units according to the formula (Li(+))2(Ca(2+))3([N2](2–))3·(e(–))2.
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Schneider S. B. et al. High-Pressure Synthesis and Characterization of Li2Ca3[N2]3—An Uncommon Metallic Diazenide with [N2]2– Ions // Journal of the American Chemical Society. 2013. Vol. 135. No. 44. pp. 16668-16679.
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Schneider S. B., Seibald M., Deringer V. L., Stoffel R. P., Frankovsky R., Friederichs G. M., Laqua H., Duppel V., Jeschke G., Dronskowski R., Schnick W. High-Pressure Synthesis and Characterization of Li2Ca3[N2]3—An Uncommon Metallic Diazenide with [N2]2– Ions // Journal of the American Chemical Society. 2013. Vol. 135. No. 44. pp. 16668-16679.
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TY - JOUR
DO - 10.1021/ja408816t
UR - https://doi.org/10.1021/ja408816t
TI - High-Pressure Synthesis and Characterization of Li2Ca3[N2]3—An Uncommon Metallic Diazenide with [N2]2– Ions
T2 - Journal of the American Chemical Society
AU - Schneider, Sebastian B
AU - Stoffel, Ralf P.
AU - Frankovsky, Rainer
AU - Friederichs, Gina M
AU - Laqua, Henryk
AU - Duppel, Viola
AU - Seibald, Markus
AU - Deringer, Volker L.
AU - Jeschke, Gunnar
AU - Dronskowski, Richard
AU - Schnick, Wolfgang
PY - 2013
DA - 2013/10/28 00:00:00
PB - American Chemical Society (ACS)
SP - 16668-16679
IS - 44
VL - 135
SN - 0002-7863
SN - 1520-5126
ER -
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@article{2013_Schneider,
author = {Sebastian B Schneider and Ralf P. Stoffel and Rainer Frankovsky and Gina M Friederichs and Henryk Laqua and Viola Duppel and Markus Seibald and Volker L. Deringer and Gunnar Jeschke and Richard Dronskowski and Wolfgang Schnick},
title = {High-Pressure Synthesis and Characterization of Li2Ca3[N2]3—An Uncommon Metallic Diazenide with [N2]2– Ions},
journal = {Journal of the American Chemical Society},
year = {2013},
volume = {135},
publisher = {American Chemical Society (ACS)},
month = {oct},
url = {https://doi.org/10.1021/ja408816t},
number = {44},
pages = {16668--16679},
doi = {10.1021/ja408816t}
}
Cite this
MLA
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Schneider, Sebastian B., et al. “High-Pressure Synthesis and Characterization of Li2Ca3[N2]3—An Uncommon Metallic Diazenide with [N2]2– Ions.” Journal of the American Chemical Society, vol. 135, no. 44, Oct. 2013, pp. 16668-16679. https://doi.org/10.1021/ja408816t.