This project has been funded with support from

___________________________________________________ This project has been funded with support from the European Commission. This publication reflects the views only of the authors, and the Commission cannot be held responsible for any use which may be made of the information contained therein.

NETCHEM Remote Access Laboratory Guide Synthesis and characterization of the products of the reaction between K 2[Pt. Cl 4] and primary biomolecules (lab exercise) Prof. Dr Biljana Petrović Faculty of Science, University of Kragujevac 2018 ___________________________________________________ This project has been funded with support from the European Commission. This publication reflects the views only of the authors, and the Commission cannot be held responsible for any use which may be made of the information contained therein.

In this exercise, students will: • • • Synthetize square-planar platinum(II) complexes with different biomolecules Characterize complexes by different experimental methods Record analyze UV-Vis spectra Record analyze Record HPLC chromatograms Record analyze HMR spectra ___________________________________________________ This project has been funded with support from the European Commission. This publication reflects the views only of the authors, and the Commission cannot be held responsible for any use which may be made of the information contained therein.

Background Why Pt(II) complexes? ___________________________________________________ This project has been funded with support from the European Commission. This publication reflects the views only of the authors, and the Commission cannot be held responsible for any use which may be made of the information contained therein.

Why biomolecules? ___________________________________________________ This project has been funded with support from the European Commission. This publication reflects the views only of the authors, and the Commission cannot be held responsible for any use which may be made of the information contained therein.

Synthesis of dichlorido(S-methyl-L-cysteine)platinum(II) complex, [Pt. Cl 2(S-methyl-L-Cys-S, N)] Equation: ___________________________________________________ This project has been funded with support from the European Commission. This publication reflects the views only of the authors, and the Commission cannot be held responsible for any use which may be made of the information contained therein.

Material • • 1. 2. 3. 4. 5. 6. 7. 8. K 2[Pt. Cl 4] HCl S-Methyl-L-Cystene Quartz cuvette KBr for IR measurements Deuterium-oxide, D 2 O NMR tube Other ligands: L-Methionine, L-Cysteine, Glycyl-DL-Methionine, L-Histidine ___________________________________________________ This project has been funded with support from the European Commission. This publication reflects the views only of the authors, and the Commission cannot be held responsible for any use which may be made of the information contained therein.

Procedure: 1. Prepare 50 cm 3 0. 1 M HCl. 2. In separate beakers measure 0. 20 g K 2[Pt. Cl 4] and corresponding amount of S-methyl-L-cysteine. 3. Both substances dissolve in as small quantity of 0, 1 M HCl. 4. Mix the solutions, heat up to 50 -60 o. C with continuous stirring about one hour. 5. Obtained yellow solution put in the fridge over night. 6. Yellow crystals of [Pt. Cl 2(C 4 H 9 NO 2 S)] complex collect by filtration, rinse with water and dry on the air. ___________________________________________________ This project has been funded with support from the European Commission. This publication reflects the views only of the authors, and the Commission cannot be held responsible for any use which may be made of the information contained therein.

Characterization of the product: ___________________________________________________ This project has been funded with support from the European Commission. This publication reflects the views only of the authors, and the Commission cannot be held responsible for any use which may be made of the information contained therein.

UV-VIS - Prepare a water solution of complex - Turn on spectrophotometer - In both quartz cuvettes put bidestilated water - Activate program - Adjust parameters - Record blank solution - Record spectrum of the complex - Analyse spectrum - Use Team. Viewer to record UV-VIS spectra. ___________________________________________________ This project has been funded with support from the European Commission. This publication reflects the views only of the authors, and the Commission cannot be held responsible for any use which may be made of the information contained therein.

IR - Prepare KBr disk Record IR spectrum Analyse IR spectrum - Use Team. Viewer to record IR spectra. ___________________________________________________ This project has been funded with support from the European Commission. This publication reflects the views only of the authors, and the Commission cannot be held responsible for any use which may be made of the information contained therein.

• Additionally, characterization by NMR and HPLC could be performed. NMR - Dissolve complex in 0. 6 cm 3 D 2 O directly in NMR tube. - Use Web Accessed Remote Instrumental Analytical Laboratory (WARIAL) network or Skype to record spectrum - Analyse 1 H NMR spectrum. ___________________________________________________ This project has been funded with support from the European Commission. This publication reflects the views only of the authors, and the Commission cannot be held responsible for any use which may be made of the information contained therein.

Fill the Table ___________________________________________________ This project has been funded with support from the European Commission. This publication reflects the views only of the authors, and the Commission cannot be held responsible for any use which may be made of the information contained therein.

The same procedure can be used for the synthesis of complexes with other biomolecule, such as L-Methionine, L-Cysteine, Glycyl-DL-Methionine, L-Histidine, etc. ___________________________________________________ This project has been funded with support from the European Commission. This publication reflects the views only of the authors, and the Commission cannot be held responsible for any use which may be made of the information contained therein.

___________________________________________________ This project has been funded with support from the European Commission. This publication reflects the views only of the authors, and the Commission cannot be held responsible for any use which may be made of the information contained therein.

Author, Editor and Referee References This remote access laboratory was created thanks to work done primarily at University of Kragujevac. Contributors to this material were: Biljana Petrović Refereeing of this material was done by: ___________ Editing into NETCHEM Format and onto NETCHEM platform was completed by: __________________________________________________________ This project has been funded with support from the European Commission. This publication reflects the views only of the authors, and the Commission cannot be held responsible for any use which may be made of the information contained therein.