Characterisation of temperature-dependent phase transitions in 2,2-trimethylenedioxy- 4,4,6,6-tetrachlorocyclotriphosphazene, N3P3Cl4[O(CH2)3O]

Powder X-ray diffraction patterns were collected on a PANalytical X'Pert PRO diffractometer in Bragg-Brentano geometry using an X'Celerator detector and Cu radiation source with a Ni filter. Samples were spun during data collection. For variable temperature PXRD studies, samples were ground to a fine powder with a mortar and pestle and sealed in a 0.3 mm glass capillary. The capillary spinner configuration (with focusing mirror) of the instrument was used along with an Oxford Cryosystems cryostat for accurate temperature

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A Series of Polymorphs of Hexakis(4-fluorophenoxy)cyclotriphosphazene

Wahl

Haynes

Roex

2012

Crystal Growth & Design

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Enantiotropic conformational polymorphism in 2,2,4,4-bis-(2′,2′-dimethylpropane-1′,3′-dioxy)-6,6-dichlorocyclotriphosphazene

et al. 2011

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Conformational polymorphism has previously been observed in 2,2-dichloro-4,4:6,6-bis(2,2'-dimethlypropane-1,3-dioxy)-cyclotriphosphazene and the crystal structures of two forms were reported. In that study the melting points of both forms (alpha and beta) were reported as 211-212 degrees C and no investigation was made on the stability of, or the thermodynamic relationships between the polymorphs. In the present work the two forms were characterized by various analytical techniques, such as single-crystal X-ray diffraction, differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), thermomicroscopy (TM) and variable temperature single crystal and powder X-ray diffraction. Thermal analysis suggests that the polymorphs are enantiotropically related and it is found that the solid-solid transformation of the beta to alpha form may start with defects of alpha form inside the beta form followed by a nucleation and growth type mechanism involving at least three main molecular centred events; conformational change, rotation and tilting

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Characterisation of temperature-dependent phase transitions in 2,2-trimethylenedioxy- 4,4,6,6-tetrachlorocyclotriphosphazene, N3P3Cl4[O(CH2)3O]

Cited by 2 publications

References 11 publications

A Series of Polymorphs of Hexakis(4-fluorophenoxy)cyclotriphosphazene

A Series of Polymorphs of Hexakis(4-fluorophenoxy)cyclotriphosphazene

Enantiotropic conformational polymorphism in 2,2,4,4-bis-(2′,2′-dimethylpropane-1′,3′-dioxy)-6,6-dichlorocyclotriphosphazene

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