Preparation and crystal structures of two salts with the 5-nitrotetrazolate anion

Authors

  • Thomas M. Klapötke,

    Corresponding author
    1. Department of Chemistry and Biochemistry, Energetic Materials Research, Ludwig-Maximilian University, Butenandtstr. 5-13 (D), 81377 Munich, Germany
    • Department of Chemistry and Biochemistry, Energetic Materials Research, Ludwig-Maximilian University, Butenandtstr. 5-13 (D), 81377 Munich, Germany
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  • Carles Miró Sabaté,

    1. Department of Chemistry and Biochemistry, Energetic Materials Research, Ludwig-Maximilian University, Butenandtstr. 5-13 (D), 81377 Munich, Germany
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  • Jan M. Welch

    1. Department of Chemistry and Biochemistry, Energetic Materials Research, Ludwig-Maximilian University, Butenandtstr. 5-13 (D), 81377 Munich, Germany
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Abstract

Tetraphenylphosphonium 5-nitrotetrazolate (2) was prepared by metathesis of sodium 5-nitrotetrazolate dihydrate (1; NaNT) with tetraphenylphosphonium chloride in acetone. The new compound was fully characterized by vibrational (IR, Raman) and NMR (1H, 13C, and 14N) spectroscopies, elemental analysis, and mass spectrometry. Attempted synthesis of 2-methyl-5-nitrotetrazole (2-MeNT) by methylation of 1 with dimethylsulfate at reflux from acetonitrile failed, and crystals of an explosive compound with the formula (NaNT)2(H2O)2CH3CN (3), NT = 5-nitrotetrazolate, formed. X-ray diffraction techniques were used to determine the crystal structure of 2 and 3. Compound 2 crystallizes in the orthorhombic space group P212121 with four molecules in the unit cell and unit cell parameters a = 7.7413(4) Å, b = 13.624(1) Å, c = 21.252(1) Å, and V = 2241.5(2) Å3, whereas 3 crystallizes in the orthorhombic space group Ama2 with four formula unit in the unit cell and unit cell parameters a = 14.805(6) Å, b = 9.908(4) Å, c = 8.940(3) Å, and V = 1311.4(1) Å3. © 2009 Wiley Periodicals, Inc. Heteroatom Chem 20:35–44, 2009; Published online in Wiley InterScience (www.interscience.wiley.com). DOI 10.1002/hc.20509

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