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ItalianChemist
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[*] posted on 24-11-2023 at 04:42
New Europium complex?


New Europium complex?


Hello everybody, lately I've been experimenting with metals complexes, especially Europium.
I have prepared this complex that I couldn't find any information about unfortunately.
My proposed structure is [Eu(DBM)3(2,2'-bipy)] (similar to the TEA complex). Unfortunately I have no means to verify that!

The complex was prepared mixing the stechiometric amount of Europium chloride hydrate, Dybenzoylmethame and 2,2'bipyridyl in a 1:1 Water:EtOH solution.
This solution becomes immediately very cloudy and shows very low fluorescent under UV light.
The mix was left for 48h. After that intensely fluorescent yellow crystals had formed.
The complex was recovered and washed with distilled water and ethanol. It seems to be insoluble in both solvents.

It shows an intense red fluorescence under UV light, but it doesn't show any triboluminescence (At least with naked eye).
I am sure someone prepared this complex before, but I couldn't find any information about it online.


IMG_5264 copia.JPG - 2.3MB IMG_5270 copia.JPG - 833kB

[Edited on 24-11-2023 by ItalianChemist]
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[*] posted on 26-11-2023 at 06:51


Quote: Originally posted by kmno4  
Your boring complex
Oh come on, why do you feel the need to be an ass about it? That attitude only discourages people from sharing their experiments.



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Bedlasky
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[*] posted on 26-11-2023 at 07:48


I don't think that this complex is boring. I find it very interesting. Good work ItalianChemist!
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[*] posted on 26-11-2023 at 09:48


Quote: Originally posted by Bedlasky  
I don't think that this complex is boring. I find it very interesting. Good work ItalianChemist!

Thank you!
I like Eu complexes because they have pretty unique luminescent properties. Some day I will try to make bigger crystals of it!
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[*] posted on 2-12-2023 at 17:31


Nice! Please post what you find out about its solubility- I have a number of lanthanides, some bipy and some DBM. I'd love to be able to grow some crystals of such complexes.



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[*] posted on 4-12-2023 at 01:09


It seems to be very slightly soluble in the EtOH/H2O mix. The solution isn't fluorescent, but it leaves a very nice pink fluorescent mark when left to dry.
It can be used for hot recrystallization, but I don't think it will be suitable to make bigger crystals.
One way could be to let slowly cool down the solution using a thermal insulator or an oven!
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[*] posted on 4-12-2023 at 05:57


I don't know if it's "new" or not, but it reminded me of my last year as a student making hexadecylpridinuim tetrakis dibenzoylmethanato europiate (III)
That can be made into fluorescent molecular monolayers.
While I had all the components I made the triboluminescent amine salt.

The stuff has an unusually long fluorescence half life of about a millisecond.

[Edited on 4-12-23 by unionised]
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[*] posted on 4-12-2023 at 12:08


Quote: Originally posted by unionised  
I don't know if it's "new" or not, but it reminded me of my last year as a student making hexadecylpridinuim tetrakis dibenzoylmethanato europiate (III)

How stable is that anion? Could it be crystallized with a much smaller cation? Or could it slowly decompose in solution to give crystals of the Eu(DBM)3 compound?




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[*] posted on 4-12-2023 at 12:41


The stuff was stable enough to prepare Langmuir Blodget films of it by floating it on the surface of water.

Here's my notes (and I'm amused to note that this is the most useful they have been since 1988)

The compound was prepared by dissolving 2 mMol of EuCl3 ; 8 mMol of dibenzoylmethane and 2 mMol of cetylypridinium chloride in 70 ml of hot ethanol and adding 4 ml of 2M NaOH.
The complex precipitated as an off- white powder .
This was filtered off and dried. It was then further purified by recrystallisation from acetone / butanone (1:1 by volume). About 100 ml of solvent was required to dissolve the material.
2.68 g were obtained (approximately 90% yield).

Looking back, I'm pretty sure the NaOH solution was aqueous.
The synthesis was pretty trivial.

I also made the corresponding triethylammonium salt via the same method (unofficially) because I thought the idea of a triboluminescent material was cool. The easy way to test is to evaporate a solution of the candidate material into a watch glass and "roll" another smaller watch glass around on the crystals that form.
That's easy to do in the dark and you can see the scintillations through the glass.

Clearly I still think it's cool. :-)



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[*] posted on 4-12-2023 at 12:45


Cool. I don't have any alkylpyridinium cations or triethylamine, but I do have tetramethylammonium chloride. Might give that a try (not with europium, but with cheaper lanthanides).



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[*] posted on 6-12-2023 at 08:34


Next days I will try to prepare some of the triboluminescent complex with the TEA.
I also finally got some pure terbium. Let's see what I can do with it :cool:
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[*] posted on 21-12-2023 at 13:57


I just want to say firstly, thank you for posting your experiments, ItalianChemist. It is always a joy to learn new things and you just taught me more about complexes. I am excited about the prospect of medicine being bound up in metal complexes, copper or whatever is safest for the body. Porphyrins are what come to mind. This is probably something more and more seen as the years tick by. Please keep up the good work, noting the effect if lights on such things is very important. I know more organic LEDs and laser diodes will be coming out and this avenue could be a way..
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