Tris(2-Methoxyphenyl)bismuthine polymorphism characterized by nuclear quadrupole resonance spectroscopy

Hermann Scharfetter*, Roland Fischer, Paul Krassnig, Martin Thonhofer, Felix Theyer, Christian Gösweiner

*Corresponding author for this work

Research output: Contribution to journalArticle

Abstract

Based on the previous identification of metastable polymorphs in crystalline triphenylbismuth by nuclear quadrupole resonance spectroscopy (NQRS), the potential formation of similar phases was studied in Tris(2-Methoxyphenyl)Bismuthine. To this end, commercial samples with known NQRS properties were molten and re-crystallized at different speeds (shock freezing in different coolants versus slow cooling inside of a heater). In all recrystallization products we have identified a new crystal phase which has not been observed after synthesis from a solution. The new crystallographic structure has been confirmed by X-ray diffraction (XRD). The newly isolated polymorph crystallizes in the monoclinic space group P2(1)/c with only one molecule in the asymmetric unit and consequently only one 5/2-7/2 transition is observed at 88.75 MHz at 310 K. In contrast, the two transitions at 89.38 and 89.29 MHz for the well-known trigonal polymorph originate from two crystallographically distinct molecules of Tris(2-methoxy-Phenyl)Bismuthine in the asymmetric unit. Additional relaxometric NQRS shows distinctly different T2 relaxation times for the new polymorph when compared to the original samples. Additional phase transitions could not be observed during temperature sweeps between 153 K and 323 K.

Original languageEnglish
Article number446
JournalCrystals
Volume9
Issue number9
DOIs
Publication statusPublished - 1 Sep 2019

Keywords

  • Melting
  • Nuclear quadrupole resonance spectroscopy
  • Polymorphs
  • Recrystallization
  • Tris(2-Methoxyphenyl)Bismuthine
  • X-ray diffractometry

ASJC Scopus subject areas

  • Chemical Engineering(all)
  • Materials Science(all)
  • Condensed Matter Physics
  • Inorganic Chemistry

Fields of Expertise

  • Human- & Biotechnology

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