Raman spectra of sodium sulphamate single crystal

Abstract

Vibrational assignments are proposed for solid NaNH2SO3 on the basis of room temperature polarized Raman spectra of single crystals. Infrared data for the region 4000–50 cm−1 of the polycrystalline sample are also presented. The results indicate that (1) there is no water of crystallization, (2) the hydrogen bonding is extremely weak, and (3) the strength of N—S bond is stronger than in sulphamic acid.

Raman, infrared and 13C NMR studies on betaine–sulfamic acid (2:1) crystal and its hydrogen bonds

“…The lowtemperature spectra were measured using a closed helium cryostat (Displex Model CSW-202 closed-cycle cryogenic refrigeration system and Lakeshore Model 300-11 dualsensor temperature controller). 13 C NMR experiments for the polycrystalline sample were carried out on a Bruker AMX-300 spectrometer using a standard cross-polarization magic angle spinning (CP/MAS) probe and a 7 mm rotor. The operating frequencies were 300.13 and 75.47 MHz for 1 H and 13 C, respectively.…”

“…The operating frequencies were 300.13 and 75.47 MHz for 1 H and 13 C, respectively. 13 C NMR spectra were obtained using CP with 4.5 µs proton 90°p ulse, a contact time of 1 ms and MAS in a standard Bruker double-bearing probe system. Generally a recycle delay for 10 s was used and 200 transients were accumulated.…”

“…Values of the Raman tensor components˛(R) ii (Tables 5 and 6) can be treated as the first derivatives of the molecular Tables 4 and 6 show that Raman tensor components˛0(R) ii , calculated for the C O symmetric stretching vibrations, are linearly related to the carboxylic 13 C shielding components ii if we assume the same local coordinates for both tensors and if we identify 1, 2 and 3 principal directions of the shielding tensor with the y, z and x ones for the Raman tensor, respectively. Figure 5 and Eqn (1) present this relation:…”

“…1 Its infrared and Raman 1 and its 13 C NMR spectra 2 were recorded for polycrystalline samples. In this contribution, we attempt to analyse the spectroscopic properties in relation to different directions of the 2B-HSO 3 NH 2 complex system.…”

“…This method provides much more precise information than 'powder-sample' experiments owing to the close correlation between polarized vibrational spectra and crystal structure. 3 Special attention is paid to (1) relations between shielding and Raman tensors available from 13 C NMR and Raman experiments, respectively, for carboxylic groups engaged in very strong hydrogen bonds and (2) dynamic behaviour of the complex (NH 2 SO 3 moieties engaged in very weak hydrogen bonds.…”