Re: ORGLIST:Hazard in using picric acid to characterise a Mo complex containi ng four -C6H4NEt2 groups?

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From: Jacob Zabicky (zabicky$##$bgumail.bgu.ac.il)
Date: Mon Nov 15 2004 - 00:58:58 EST


Dear Fergus,

Your fears are quite well based. On perusing the International Chemical
Safety Card of picric acid, published by the UN Chemical Safety Program
(http://www.ilo.org/public/english/protection/safework/cis/products/
icsc/dtasht/_icsc03/icsc0316.htm), one finds that "Shock-sensitive
compounds are formed with metals, particularly copper, lead, mercury
and zinc.", which probably are well known. However, students should not
be the people testing new explosives.

All the best,

Jacob

Prof. Jacob Zabicky
Institutes for Applied Researcfh
Ben-Gurion University of the Negev
P. O. Box 653
Beer-Sheva, 84105
Israel
-------------------------------------
zabicky$##$bgumail.bgu.ac.il
Tel. +972-8-6461271
Fax. +972-8-6472969
-------------------------------------
Private: P. O. Box 12366
Beer-Sheva, 84863
Israel
Tel. +972-8-6496792

On Nov 11, 2004, at 16:24, Lalor, Fergus wrote:

> A student of mine is attempting to structurally characterise a large
> (MW ca.
> 1300) organometallic complex containing four Mo(CO)2 fragments and,
> inter
> alia, four C6H4NEt2 fragments. The complex itself doesn't crystallise
> well
> so we wish to convert it into an ionic derivative which might be more
> cooperative. Attempted quaternisation of the tertiary amino groups with
> Et3OPF6 just caused decomposition. I remembered from my own graduate
> student
> days that it was then routine to characterise basic organic materials
> in the
> form of their crystalline picrate salts. A *very* small-scale test
> indicates
> that our compound does indeed form a crystalline picrate. However I am
> a
> little nervous in proceeding on a larger scale in case the picrate
> turns out
> to be shock-sensitive and/or the picric acid degrades the complex to a
> molybdenum picrate - I understand that some metal picrates are highly
> explosive. Any comments/suggestions?
> Regards -
> Fergus Lalor
>
> Dr. Fergus John Lalor
> Senior Lecturer
> Department of Chemistry
> University College
> Cork
> Ireland.
> Telephone: 00353-21-4902317
> Fax: 00353-21-4274097
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