The Polymorphism of Orlyum White 520T, an Ultraviolet Luminescent Security Ink

The polymorphism of the ultraviolet luminescent security ink Orlyum White 520T (<i>N</i>-(2-(4-oxo-4<i>H</i>-benzo[d][3,1]-oxazin-2-yl)phenyl)naphthalene-2-sulfonamide) is revealed, obtaining two new polymorphic forms with enhanced stability. Beyond the known form (lit. mp. 1...

Full description

Saved in:
Bibliographic Details
Main Authors: János Madarász, Nóra V. May, Petra Bombicz, György Pokol, Richárd Kocsis, Bálint Hegymegi-Barakonyi, Tibor Gizur
Format: Article
Language:English
Published: MDPI AG 2025-04-01
Series:Molecules
Subjects:
Online Access:https://www.mdpi.com/1420-3049/30/8/1671
Tags: Add Tag
No Tags, Be the first to tag this record!
_version_ 1850180064355811328
author János Madarász
Nóra V. May
Petra Bombicz
György Pokol
Richárd Kocsis
Bálint Hegymegi-Barakonyi
Tibor Gizur
author_facet János Madarász
Nóra V. May
Petra Bombicz
György Pokol
Richárd Kocsis
Bálint Hegymegi-Barakonyi
Tibor Gizur
author_sort János Madarász
collection DOAJ
description The polymorphism of the ultraviolet luminescent security ink Orlyum White 520T (<i>N</i>-(2-(4-oxo-4<i>H</i>-benzo[d][3,1]-oxazin-2-yl)phenyl)naphthalene-2-sulfonamide) is revealed, obtaining two new polymorphic forms with enhanced stability. Beyond the known form (lit. mp. 184.8–185.2 °C, Form III, YOCTAO), we succeeded in gaining two new polymorphic forms, Form II and Form I, with higher melting points of 195–196 and 197–198 °C, respectively. Their elemental composition, <sup>1</sup>H and <sup>13</sup>C NMR spectra have been found to be identical, while their powder XRD patterns and FT-IR spectra are significantly different. Based on the single-crystal structure determination of Form II and redetermination of Form III, we uncover the similarities and differences in their packing arrangement and in their secondary interaction systems, all of which affect the molecular conformations in their crystals. In order to explain their significantly distinguishable melting points, Hirshfeld surface analysis and lattice energy calculations have also been carried out. We have made efforts toward revealing the reproducible conditions under which certain polymorphs are formed. It seems that the solvents or other probable organic contaminations are more likely responsible for the formation, nucleation and growth of crystals of various polymorphic forms, traced by thermogravimetric evolved gas analysis (TG/DTA-EGA-MS).
format Article
id doaj-art-820e148bb11d4b6199515d53feff4b31
institution OA Journals
issn 1420-3049
language English
publishDate 2025-04-01
publisher MDPI AG
record_format Article
series Molecules
spelling doaj-art-820e148bb11d4b6199515d53feff4b312025-08-20T02:18:20ZengMDPI AGMolecules1420-30492025-04-01308167110.3390/molecules30081671The Polymorphism of Orlyum White 520T, an Ultraviolet Luminescent Security InkJános Madarász0Nóra V. May1Petra Bombicz2György Pokol3Richárd Kocsis4Bálint Hegymegi-Barakonyi5Tibor Gizur6Department of Inorganic and Analytical Chemistry, Budapest University of Technology and Economics, Műegyetem rkp. 3, HU-1111 Budapest, HungaryCentre for Structural Science, HUN-REN Research Centre for Natural Sciences, Magyar Tudósok Körútja 2, HU-1117 Budapest, HungaryCentre for Structural Science, HUN-REN Research Centre for Natural Sciences, Magyar Tudósok Körútja 2, HU-1117 Budapest, HungaryDepartment of Inorganic and Analytical Chemistry, Budapest University of Technology and Economics, Műegyetem rkp. 3, HU-1111 Budapest, HungaryLuminoChem R&D Ltd., Háros utca 7/A, HU-1222 Budapest, HungaryLuminoChem R&D Ltd., Háros utca 7/A, HU-1222 Budapest, HungaryDepartment of Organic Chemistry and Technology, Budapest University of Technology and Economics, Műegyetem rkp. 3, HU-1111 Budapest, HungaryThe polymorphism of the ultraviolet luminescent security ink Orlyum White 520T (<i>N</i>-(2-(4-oxo-4<i>H</i>-benzo[d][3,1]-oxazin-2-yl)phenyl)naphthalene-2-sulfonamide) is revealed, obtaining two new polymorphic forms with enhanced stability. Beyond the known form (lit. mp. 184.8–185.2 °C, Form III, YOCTAO), we succeeded in gaining two new polymorphic forms, Form II and Form I, with higher melting points of 195–196 and 197–198 °C, respectively. Their elemental composition, <sup>1</sup>H and <sup>13</sup>C NMR spectra have been found to be identical, while their powder XRD patterns and FT-IR spectra are significantly different. Based on the single-crystal structure determination of Form II and redetermination of Form III, we uncover the similarities and differences in their packing arrangement and in their secondary interaction systems, all of which affect the molecular conformations in their crystals. In order to explain their significantly distinguishable melting points, Hirshfeld surface analysis and lattice energy calculations have also been carried out. We have made efforts toward revealing the reproducible conditions under which certain polymorphs are formed. It seems that the solvents or other probable organic contaminations are more likely responsible for the formation, nucleation and growth of crystals of various polymorphic forms, traced by thermogravimetric evolved gas analysis (TG/DTA-EGA-MS).https://www.mdpi.com/1420-3049/30/8/1671structure–property relationshipultraviolet (UV) fluorescencesingle-crystal and powder X-ray diffraction (XRD)FT-IR spectroscopydifferential scanning calorimetry (DSC)TG/DTA-MS
spellingShingle János Madarász
Nóra V. May
Petra Bombicz
György Pokol
Richárd Kocsis
Bálint Hegymegi-Barakonyi
Tibor Gizur
The Polymorphism of Orlyum White 520T, an Ultraviolet Luminescent Security Ink
Molecules
structure–property relationship
ultraviolet (UV) fluorescence
single-crystal and powder X-ray diffraction (XRD)
FT-IR spectroscopy
differential scanning calorimetry (DSC)
TG/DTA-MS
title The Polymorphism of Orlyum White 520T, an Ultraviolet Luminescent Security Ink
title_full The Polymorphism of Orlyum White 520T, an Ultraviolet Luminescent Security Ink
title_fullStr The Polymorphism of Orlyum White 520T, an Ultraviolet Luminescent Security Ink
title_full_unstemmed The Polymorphism of Orlyum White 520T, an Ultraviolet Luminescent Security Ink
title_short The Polymorphism of Orlyum White 520T, an Ultraviolet Luminescent Security Ink
title_sort polymorphism of orlyum white 520t an ultraviolet luminescent security ink
topic structure–property relationship
ultraviolet (UV) fluorescence
single-crystal and powder X-ray diffraction (XRD)
FT-IR spectroscopy
differential scanning calorimetry (DSC)
TG/DTA-MS
url https://www.mdpi.com/1420-3049/30/8/1671
work_keys_str_mv AT janosmadarasz thepolymorphismoforlyumwhite520tanultravioletluminescentsecurityink
AT noravmay thepolymorphismoforlyumwhite520tanultravioletluminescentsecurityink
AT petrabombicz thepolymorphismoforlyumwhite520tanultravioletluminescentsecurityink
AT gyorgypokol thepolymorphismoforlyumwhite520tanultravioletluminescentsecurityink
AT richardkocsis thepolymorphismoforlyumwhite520tanultravioletluminescentsecurityink
AT balinthegymegibarakonyi thepolymorphismoforlyumwhite520tanultravioletluminescentsecurityink
AT tiborgizur thepolymorphismoforlyumwhite520tanultravioletluminescentsecurityink
AT janosmadarasz polymorphismoforlyumwhite520tanultravioletluminescentsecurityink
AT noravmay polymorphismoforlyumwhite520tanultravioletluminescentsecurityink
AT petrabombicz polymorphismoforlyumwhite520tanultravioletluminescentsecurityink
AT gyorgypokol polymorphismoforlyumwhite520tanultravioletluminescentsecurityink
AT richardkocsis polymorphismoforlyumwhite520tanultravioletluminescentsecurityink
AT balinthegymegibarakonyi polymorphismoforlyumwhite520tanultravioletluminescentsecurityink
AT tiborgizur polymorphismoforlyumwhite520tanultravioletluminescentsecurityink