I have synthesized Co(III)-hydrazone complex. This complex is soluble in Dimethylformamide(DMF), Dimethylsulphoxide(DMSO) and partially soluble in Methanol. Meanwhile, it is insoluble in Ethers, Acetonitrile, Dichloromethane, Chloroform and others.
I have tried several approaches to grow single crystals but to no avail.
How can I obtain single crystals for SC-XRD measurement.
Hi. As you have said that the complex is soluble in DMF, DMSO therefore the preferred route for purification can be either of the routes listed below.
a) Concentrate the DMF, DMSO layers to saturation/supersaturation and initiate crystallisation at low temperatures.
b) Else concentrate it partially and then initiate antisolvent crystallisation using methanol, ethers or ACN under controlled addition at low temperatures.
Filter the same and dry the crystals to obtain purified crystals
What do you mean by "purify a solution"? If you obtain crystals out of a solution, the obtained material is usually pure (phase pure in a crystallographic sense). The crystals might contain co-crystallised solvent molecules.
If you want to get rid of them, try to crystallise your complex from a different solvent.
But to be honest, I did not get your question, really.
And please refrain from using "pseudo-experts terminology" such as SC-XRD. Its simply: single crystal X-ray diffraction.
you can use mixture solvent
because your complex soluble in DMF and insoluble in methanol
you can mixture ( MDF : Methanol) in different ratio
Solvent mixture is OK. Optimisation necessary. But low temperature + patience!
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