Structural phase transition in [NH3(CH2)5NH3]BiCl5: thermal and vibrational studies

Abstract

An x-ray diffraction study carried out on the pentylenediammonium pentachlorobismuthate (III) compound [NH 3 (CH 2 / 5 NH 3 ]BiCl 5 indicated that it is orthorhombic with a P2 1 2 1 2 1 (Z = 4) space group. Differential scanning calorimetry (DSC), differential thermal analysis (DTA) and thermogravimetric analysis (TGA) were also made, which showed that this compound undergoes a unique phase transition at high temperatures. The infrared and Raman spectra recorded at room temperature were interpreted on the basis of data published in the literature. The Raman bands observed below 300 cm −1 are very characteristic of the anions, which are made of isolated (BiCl 5 2− ) n units composed of BiCl 6 3− octahedra. Raman spectra recorded at various temperatures confirmed the contribution to the phase-transition mechanism of both the anion and cation motions.

Synthesis, crystal structure and characterization of two new organic bismuthate(III) compounds: [C6H18O]2Bi2X10·2H2O (X = Br, Cl)

“…3. In comparison with previous research works reported on similar compounds containing [BiCl 5 ] [16,17], the Raman spectrum of [C 6 H 18 N 2 O] 2 Bi 2 Cl 10 Á2H 2 O is found to be similar to that of [NH 3 (CH 2 ) 5 NH 3 ]BiCl 5 [18] registered at 303 K. The highintensity band detected at 266 cm -1 is assigned to the terminal Bi-Cl bonds, and the weak band observed at 220 cm -1 is assigned to the bridging Bi-Cl stretching vibrations. The bands corresponding to the Cl-Bi-Cl deformation mode appear at 167 cm -1 .…”

Crystal structure, vibrational spectroscopy and optical properties of a one-dimensional organic–inorganic hybrid perovskite of [NH3CH2CH(NH3)CH2]BiCl5

“…The anion part of the molecule vibrations are observed in the range 209 to 274 cm À1 and caused by Bi-Cl stretching (Jeghnou et al, 2005;Essid et al, 2014).…”

Butane-1,4-diammonium hexafluorosilicate

“…For similar compounds, see: Jeghnou et al (2005); Rhandour et al (2011);Ouasri et al (2012Ouasri et al ( , 2013aOuasri et al ( ,b, 2014 Table 1 Hydrogen-bond geometry (Å , ). Data collection: APEX2 (Bruker, 2009); cell refinement: SAINT-Plus (Bruker, 2009); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Farrugia, 2012); software used to prepare material for publication: PLATON (Spek, 2009) and publCIF (Westrip, 2010).…”

“…X-ray, thermal and vibrational studies of phase transitions have also been performed for highly related compounds belonging to the alkanediammonium halogenobismuthate salts family as the pentachlorobismuthate one (NH 3 (CH 2 ) n NH 3 )BiCl 5 (Jeghnou et al, 2005;Ouasri et al, 2012;Rhandour et al, 2011;Ouasri et al, 2013a;Ouasri et al, 2013b;Ouasri et al, 2014). The aim of the present paper was to study the recently synthesized butanediammonium hexafluorosilicate (NH 3 (CH 2 ) 4 NH 3 )SiF 6 crystal, by X-ray diffraction at room temperature.…”