Tris(2-Methoxyphenyl)Bismuthine Polymorphism Characterized by Nuclear Quadrupole Resonance Spectroscopy
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...
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MDPI AG
2019-08-01
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| Series: | Crystals |
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| Online Access: | https://www.mdpi.com/2073-4352/9/9/446 |
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| author | Hermann Scharfetter Roland Fischer Paul Krassnig Martin Thonhofer Felix Theyer Christian Gösweiner |
| author_facet | Hermann Scharfetter Roland Fischer Paul Krassnig Martin Thonhofer Felix Theyer Christian Gösweiner |
| author_sort | Hermann Scharfetter |
| collection | DOAJ |
| description | 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 T<sub>2</sub> 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. |
| first_indexed | 2024-04-11T21:53:18Z |
| format | Article |
| id | doaj.art-903d6db6140a47759f5e6ef173496169 |
| institution | Directory Open Access Journal |
| issn | 2073-4352 |
| language | English |
| last_indexed | 2024-04-11T21:53:18Z |
| publishDate | 2019-08-01 |
| publisher | MDPI AG |
| record_format | Article |
| series | Crystals |
| spelling | doaj.art-903d6db6140a47759f5e6ef1734961692022-12-22T04:01:11ZengMDPI AGCrystals2073-43522019-08-019944610.3390/cryst9090446cryst9090446Tris(2-Methoxyphenyl)Bismuthine Polymorphism Characterized by Nuclear Quadrupole Resonance SpectroscopyHermann Scharfetter0Roland Fischer1Paul Krassnig2Martin Thonhofer3Felix Theyer4Christian Gösweiner5Institute of Medical Engineering, Graz University of Technology, Stremayrgasse 16, 8010 Graz, AustriaInstitute of Inorganic Chemistry, Graz University of Technology, Stremayrgasse 9, 8010 Graz, AustriaInstitute of Medical Engineering, Graz University of Technology, Stremayrgasse 16, 8010 Graz, AustriaInstitute of Organic Chemistry, Graz University of Technology, Stremayrgasse 9, 8010 Graz, AustriaInstitute of Medical Engineering, Graz University of Technology, Stremayrgasse 16, 8010 Graz, AustriaInstitute of Medical Engineering, Graz University of Technology, Stremayrgasse 16, 8010 Graz, AustriaBased 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 T<sub>2</sub> 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.https://www.mdpi.com/2073-4352/9/9/446nuclear quadrupole resonance spectroscopyTris(2-Methoxyphenyl)Bismuthinepolymorphsrecrystallizationmeltingx-ray diffractometry |
| spellingShingle | Hermann Scharfetter Roland Fischer Paul Krassnig Martin Thonhofer Felix Theyer Christian Gösweiner Tris(2-Methoxyphenyl)Bismuthine Polymorphism Characterized by Nuclear Quadrupole Resonance Spectroscopy Crystals nuclear quadrupole resonance spectroscopy Tris(2-Methoxyphenyl)Bismuthine polymorphs recrystallization melting x-ray diffractometry |
| title | Tris(2-Methoxyphenyl)Bismuthine Polymorphism Characterized by Nuclear Quadrupole Resonance Spectroscopy |
| title_full | Tris(2-Methoxyphenyl)Bismuthine Polymorphism Characterized by Nuclear Quadrupole Resonance Spectroscopy |
| title_fullStr | Tris(2-Methoxyphenyl)Bismuthine Polymorphism Characterized by Nuclear Quadrupole Resonance Spectroscopy |
| title_full_unstemmed | Tris(2-Methoxyphenyl)Bismuthine Polymorphism Characterized by Nuclear Quadrupole Resonance Spectroscopy |
| title_short | Tris(2-Methoxyphenyl)Bismuthine Polymorphism Characterized by Nuclear Quadrupole Resonance Spectroscopy |
| title_sort | tris 2 methoxyphenyl bismuthine polymorphism characterized by nuclear quadrupole resonance spectroscopy |
| topic | nuclear quadrupole resonance spectroscopy Tris(2-Methoxyphenyl)Bismuthine polymorphs recrystallization melting x-ray diffractometry |
| url | https://www.mdpi.com/2073-4352/9/9/446 |
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