Best, as silver salt or with good solubility in organic solvents, where the cation-BF4/PF6/ClO4-cation is less soluble (ion-exchange).
Explanation: Attempting to crystallize a mono-cation complex where I unlikely got only cry. of de-comproportionated (close second oxidation) or ligand-exchanged (PF6, ClO4 or BF4 anions) products. System exhibits hemi-labile function. Preparation by oxidation of the neutral complex through corresponding silver-salts (in various solvents, like hexane, methylenchlorid, acetonirtile or toluene). From CV and SEC two reversible oxidations.
Have the Impression that "side-reactions" occurs with crystallization.
Anion-exchange with BARF-salt (Tetra(Di-fluoro-)phenyl-Borane)Na(+) lead to a stable salt which is amorphous and absolute insoluble. Electrocryst. and sublimation aren`t suitable, leads to decomposition. Anions of "huge" carboxylates are ligand exchanging and coordinating.
Suggestion? Alkyl-sulfonates?
(CF3SO2)2N(+)Li(-) - very suspicious to your task
BARF-Na is Tetrakis[3,5-bis(trifluoromethyl)phenyl]boron sodium but not (Tetra(Di-fluoro-)phenyl-Borane)Na(+) http://www.sigmaaldrich.com/catalog/product/fluka/72017
the Bis(trifluoromethane)sulfonimide anion, may an option, hope it`s not to nucleophilic
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