Abstract
AbstractTetraphenylphosphonium 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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