Crystalline Forms of 4,4'-Methylenediantipyrine: Crystallographic Unit Cell for the Anhydrous Form, from Laboratory Powder XRD Pattern by DASH Program Package

Authors

  • Dorottya Fruzsina Bánhegyi
    Affiliation
    Department of Organic Chemistry and Technology, Faculty of Chemical Technology and Biotechnology, Budapest University of Technology and Economics, Műegyetem rkp. 3, H-1111 Budapest, Hungary
  • János Madarász
    Affiliation
    Department of Inorganic and Analytical Chemistry, Faculty of Chemical Technology and Biotechnology, Budapest University of Technology and Economics, Műegyetem rkp. 3, H-1111 Budapest, Hungary
  • Elemér Fogassy
    Affiliation
    Department of Organic Chemistry and Technology, Faculty of Chemical Technology and Biotechnology, Budapest University of Technology and Economics, Műegyetem rkp. 3, H-1111 Budapest, Hungary
  • Emese Pálovics
    Affiliation
    Department of Organic Chemistry and Technology, Faculty of Chemical Technology and Biotechnology, Budapest University of Technology and Economics, Műegyetem rkp. 3, H-1111 Budapest, Hungary
  • György Pokol
    Affiliation
    Department of Inorganic and Analytical Chemistry, Faculty of Chemical Technology and Biotechnology, Budapest University of Technology and Economics, Műegyetem rkp. 3, H-1111 Budapest, Hungary
https://doi.org/10.3311/PPch.22950

Abstract

Crystalline unit cell structure of anhydrous title compound, diantipyrinylmethane (CAS Registry No. 1251-85-0), a substance usually obtained as a by-product in Mannich type reactions of antipyrine, has been modelled by the help of powder X-ray diffraction, applying the DASH software package and crystal coordinates coming from former single crystal X-ray structure determinations (CSD codes FADDIY and FADDIY01) of its monohydrate. The unit cell of the anhydrate compound belongs to the monoclinic space group P21/a, with unit cell parameters of a = 14.604, b = 9.858, c = 14.509 Å, β = 95.56 °, V = 2078.9 Å3, Z = 4, Z ' = 1. Comparisons of FT-IR spectrum and thermal behavior of the anhydrous and monohydrated forms confirm differences in degree of hydration and solid state structure, while those of 1H- and 13C NMR-spectra show their molecular identity.

Keywords:

anhydrous form of diantipyrinylmethane, monohydrate form of diantipyrinylmethane, crystallographic unit cell indexing from powder XRD by DASH, crystal structure modelling by simulated annealing, FT-IR spectra, Differential Scanning Calorimetry (DSC), Thermogravimetry (TG)

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Published Online

2023-10-16

How to Cite

Bánhegyi, D. F., Madarász, J., Fogassy, E., Pálovics, E., Pokol, G. “Crystalline Forms of 4,4’-Methylenediantipyrine: Crystallographic Unit Cell for the Anhydrous Form, from Laboratory Powder XRD Pattern by DASH Program Package”, Periodica Polytechnica Chemical Engineering, 67(4), pp. 557–564, 2023. https://doi.org/10.3311/PPch.22950

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