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

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From: Lalor, Fergus (f.lalor$##$ucc.ie)
Date: Thu Nov 11 2004 - 09:24:30 EST


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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