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

✍ Scribed by Thomas M. Klapötke; Carles Miró Sabaté; Jan M. Welch

• Publisher: John Wiley and Sons
• Year: 2009
• Tongue: English
• Weight: 381 KB
• Volume: 20
• Category: Article
• ISSN: 1042-7163
• DOI: 10.1002/hc.20509

✦ Synopsis

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 ( 1 H, 13 C, and 14 N) 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 (H 2 O) 2 CH 3 CN (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 P2 1 2 1 2 1 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)