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Issue 18, 2012
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Investigation of a new organic/inorganic hybrid crystal tri(p-chloro-anilium) pentabromocadmate(II) by in situPXRD and FTIR methods: Thermal stability and the route to suppress its decomposition

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Abstract

A new organic/inorganic hybrid crystal tri(p-chloro-anilium) pentabromocadmate(II) ((p-Cl-C6H4-NH3)3CdBr5) was grown by a programmed cooling method, and its structure was determined using an X-ray diffraction method. This hybrid crystal crystallizes in the monoclinic space group P21/c with unit cell parameters a = 15.033(2) Å, b = 8.0189(12) Å, c = 23.103(4) Å, β = 99.649(8)°, V = 2745.6(7) Å3, Z = 4, R[F2 > 2σ(F2)] = 0.0538, wR(F2) = 0.0833. The heating processes of the hybrid crystals were investigated by TGA-DTA, in situ X-ray diffraction (XRD) and Fourier transform infrared (FTIR) measurements. The results revealed that the crystal decomposed in two stages. First, p-chlorobenzenamine hydrobromide (p-Cl-C6H4-NH2HBr) was produced from the crystal when subjected to temperatures above 170 °C, the gas products of p-Cl-C6H4-NH2HBr then followed as the temperature increased continuously. Furthermore, the in situ FTIR spectra collected at high pressure demonstrated that its dissociation temperature increased by ∼22 °C in a nitrogen atmosphere of 4.0 MPa.

Graphical abstract: Investigation of a new organic/inorganic hybrid crystal tri(p-chloro-anilium) pentabromocadmate(II) by in situ PXRD and FTIR methods: Thermal stability and the route to suppress its decomposition

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Supplementary files

Article information


Submitted
16 Apr 2012
Accepted
21 May 2012
First published
30 May 2012

CrystEngComm, 2012,14, 5795-5800
Article type
Paper

Investigation of a new organic/inorganic hybrid crystal tri(p-chloro-anilium) pentabromocadmate(II) by in situ PXRD and FTIR methods: Thermal stability and the route to suppress its decomposition

L. Cao, Z. Liu, T. Wang, H. Dai, L. Zhang, X. Tao and D. Cui, CrystEngComm, 2012, 14, 5795
DOI: 10.1039/C2CE25571E

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