I tried several times a self-assembly reaction between a pyridine (derivatives) base donor linker and Pd salt based acceptor linker in DMSO at very small scale (0.005mmol) but I didn't get crystal of self assembled product. Please suggest me what should I do to get a good crystal.
Dear Khushwant Singh many thanks for your interesting technical question. Growing single-crystals is often more difficult than synthesizing a particular compound. In your case it would first of all be interesting to know if you followed a literature procedure or if this is a new reaction. Normally pyridine ligands would be expected to easily form stable coordination compounds with palladium. Since you are working on a very small scale, I suggest that you should try a vapor diffusion technique to grow crystals of your product. This means that you place your solution in DMSO in a small vial and then place the vial into a larger jar which contains some diethyl ether. Then close the jar tightly and let the diethyl ether diffuse into the DMSO solution. Chances are that crystals will grow after a few days.
There are a few helpful guides available in which the diffusion technique and other methods for growing single crystals are described in detail. Please have a look at the following useful links:
Crystal Growing Tips and Methods
https://cpb-us-w2.wpmucdn.com/web.sas.upenn.edu/dist/f/266/files/2016/11/Crystal-Growing-Tips-and-Methods-xe0crh.pdf
X-RAY STRUCTURE ANALYSIS LAB MANUAL:
A BEGINNER’S INTRODUCTION1 CHAPTER XIV: GROWING SINGLE CRYSTALS
https://www.chem.uni-potsdam.de/groups/rksa/Crystal_Growth.pdf
Growing Quality Crystals
https://web.mit.edu/x-ray/cystallize.html
All three guides can be freely downloaded as public full texts from the internet.
Yet another method which you could try is described in pour paper cited below. It describes a very simple small-scale crystallization technique. In your case you could prepared a solution of your pyridine ligand in a few ml of DMSO in a small vial and add a few mg of your solid Pd salt. Then let the mixture stand undisturbed for a few days and see if crystals grow.
Crystal Structures of Energetic Compounds. I. Safe Small-Scale Preparation and X-Ray Structure Determination of the High-Energy Cobalt(III) Complex [Co(NH3)5N3](N3)2
Article Crystal Structures of Energetic Compounds. I. Safe Small-Sca...
This paper is freely available as public full text on RG. Good luck with your experiments! 👍
Thanks you @Frank T. Edelmann Sir. The links and literatures you suggest are very informative.
Dear Khushwant Singh, just keep in mind that Pd(II) salt in the presence of the DMSO gives stable yellov crystalline complexes like Pd(dmso)2X2 with relatively low solubility.
- Badges
- Science topic
- Similar topics
- Chemistry
- Sulfites
- Inorganic Chemistry
- Inorganic Chemicals
- Salts