Synthesis of LiBC4N4, BC3N3, and related C-N compounds of boron

New precursors to light element ceramics

Darrick Williams, Brett Pleune, John Kouvetakis, M. D. Williams, R. A. Andersen

Research output: Contribution to journalArticle

69 Citations (Scopus)

Abstract

The synthesis of a novel framework cyanide with composition LiBC4N4 (1) is described. X-ray powder diffraction as well as 7Li, 11B, and 13C NMR of 1 reveal an ordered structure which consists of two interpenetrating diamond-like networks of BC4 and LiN4 tetrahedra linked by C-N bonds. The structure is simple cubic, symmetry P43m, a = 5476(3) Å. In solution the presence of the B(CN)4 anion has been established for the first time by spectroscopic methods. Molecular B(CN)3 is isolated for the first time as a Lewis acid-base complex with bases such as NMe3 and SiMe3CN, and a single-crystal X-ray structure of B(CN)3NMe3 (3) has been obtained. The novel solid-state cyanide BC3N3 (2) is prepared from the thermal elimination of NCSiMe3 from B(CN)3NCSiMe3 (4). In route to 4, compounds B(CN)2(SMe)NCSiMe3 (5) and B(CN)2(SMe)-NMe3 (6) have also been isolated. A single-crystal X-ray structure of 6 reveals that the compound crystallizes in the monoclinic space group P21/n. The new crystalline solids 2 and 1 (isoelectronic to C) are promising precursors for high-pressure and high-temperature syntheses of novel phases with structures related to Si3N4, diamond, and graphite.

Original languageEnglish (US)
Pages (from-to)7735-7741
Number of pages7
JournalJournal of the American Chemical Society
Volume122
Issue number32
DOIs
StatePublished - Aug 16 2000

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Boron Compounds
Diamond
Cyanides
Ceramics
Boron
Diamonds
Lewis Bases
X-Rays
Single crystals
Powder Diffraction
Light
X rays
Lewis Acids
Graphite
X-Ray Diffraction
X ray powder diffraction
Anions
Negative ions
Hot Temperature
Nuclear magnetic resonance

ASJC Scopus subject areas

  • Chemistry(all)

Cite this

Synthesis of LiBC4N4, BC3N3, and related C-N compounds of boron : New precursors to light element ceramics. / Williams, Darrick; Pleune, Brett; Kouvetakis, John; Williams, M. D.; Andersen, R. A.

In: Journal of the American Chemical Society, Vol. 122, No. 32, 16.08.2000, p. 7735-7741.

Research output: Contribution to journalArticle

Williams, Darrick ; Pleune, Brett ; Kouvetakis, John ; Williams, M. D. ; Andersen, R. A. / Synthesis of LiBC4N4, BC3N3, and related C-N compounds of boron : New precursors to light element ceramics. In: Journal of the American Chemical Society. 2000 ; Vol. 122, No. 32. pp. 7735-7741.
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abstract = "The synthesis of a novel framework cyanide with composition LiBC4N4 (1) is described. X-ray powder diffraction as well as 7Li, 11B, and 13C NMR of 1 reveal an ordered structure which consists of two interpenetrating diamond-like networks of BC4 and LiN4 tetrahedra linked by C-N bonds. The structure is simple cubic, symmetry P43m, a = 5476(3) {\AA}. In solution the presence of the B(CN)4 anion has been established for the first time by spectroscopic methods. Molecular B(CN)3 is isolated for the first time as a Lewis acid-base complex with bases such as NMe3 and SiMe3CN, and a single-crystal X-ray structure of B(CN)3NMe3 (3) has been obtained. The novel solid-state cyanide BC3N3 (2) is prepared from the thermal elimination of NCSiMe3 from B(CN)3NCSiMe3 (4). In route to 4, compounds B(CN)2(SMe)NCSiMe3 (5) and B(CN)2(SMe)-NMe3 (6) have also been isolated. A single-crystal X-ray structure of 6 reveals that the compound crystallizes in the monoclinic space group P21/n. The new crystalline solids 2 and 1 (isoelectronic to C) are promising precursors for high-pressure and high-temperature syntheses of novel phases with structures related to Si3N4, diamond, and graphite.",
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N2 - The synthesis of a novel framework cyanide with composition LiBC4N4 (1) is described. X-ray powder diffraction as well as 7Li, 11B, and 13C NMR of 1 reveal an ordered structure which consists of two interpenetrating diamond-like networks of BC4 and LiN4 tetrahedra linked by C-N bonds. The structure is simple cubic, symmetry P43m, a = 5476(3) Å. In solution the presence of the B(CN)4 anion has been established for the first time by spectroscopic methods. Molecular B(CN)3 is isolated for the first time as a Lewis acid-base complex with bases such as NMe3 and SiMe3CN, and a single-crystal X-ray structure of B(CN)3NMe3 (3) has been obtained. The novel solid-state cyanide BC3N3 (2) is prepared from the thermal elimination of NCSiMe3 from B(CN)3NCSiMe3 (4). In route to 4, compounds B(CN)2(SMe)NCSiMe3 (5) and B(CN)2(SMe)-NMe3 (6) have also been isolated. A single-crystal X-ray structure of 6 reveals that the compound crystallizes in the monoclinic space group P21/n. The new crystalline solids 2 and 1 (isoelectronic to C) are promising precursors for high-pressure and high-temperature syntheses of novel phases with structures related to Si3N4, diamond, and graphite.

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