Molecular structures of two copper complexes with the pharmaceuticals norfloxacin and tinidazole, when powder X-ray diffraction assists multi-domain single-crystal X-ray diffraction

Acta Crystallogr B Struct Sci Cryst Eng Mater. 2022 Jun 1;78(Pt 3 Pt 2):490-498. doi: 10.1107/S2052520622003766. Epub 2022 May 20.

Abstract

The crystal structures of bis[1-ethyl-6-fluoro-4-oxo-7-(piperazin-1-ium-4-yl)-1,4-dihydroquinoline-3-carboxylato]copper(II) sulfate heptahydrate, [Cu(C16H18FN3O3)2]SO4·7H2O or [Cu(nor)2]SO4·7H2O (nor is norfloxacin), and bis{1-[2-(ethylsulfonyl)ethyl]-2-methyl-5-nitroimide}dinitratocopper(II), [Cu(NO3)2(C8H13N3O4S)2] or [Cu(NO3)2(tnz)2] (tnz is tinidazole), were solved by X-ray diffraction. Both complexes crystallize in the space group P21/c, with Z = 4 (for nor) and Z = 2 (for ntz) molecules per unit cell. In [Cu(nor)2]SO4·7H2O, the CuII ion is at the centre of a square-planar environment, trans coordinated to two independent norfloxacin molecules in the zwitterionic form acting as bidentate ligands through one of the carboxyl (cbx) and the carbonyl (cb) O atoms. The solid is further stabilized by an extensive network of N-H...O(sulfate), N-H...O(cbx), N-H...OW, OW-H...O(sulfate) and OW-H...OW hydrogen bonds. The [Cu(NO3)2(tnz)2] complex is centrosymmetric, with the CuII ion in a square planar environment, coordinated to a tinidazole molecule acting as a monodentate ligand through its imidazole N atom and to one nitrate O atom. The vibrational FT-IR absorption spectra and thermal behaviour of the complexes were also studied and are briefly discussed based on the crystal structures.

Keywords: PXRD-assisted SCXRD; X-ray crystal structures; copper(II) complexes of norfloxacin and tinidazole; thermal decomposition; vibrational IR spectra.

MeSH terms

  • Copper* / chemistry
  • Crystallography, X-Ray
  • Ligands
  • Molecular Structure
  • Norfloxacin
  • Powders
  • Spectroscopy, Fourier Transform Infrared
  • Sulfates
  • Tinidazole*
  • X-Ray Diffraction

Substances

  • Ligands
  • Powders
  • Sulfates
  • Tinidazole
  • Copper
  • Norfloxacin