A series of new complexes incorporating the functionalized tetrathiafulvalene (TTF) ligands ortho -(CH 3 ) 2 (P(C 6 H 5 ) 2 ) 2 TTF ( o- P2) and (P(C 6 H 5 ) 2 ) 4 TTF (P4) have been prepared and studied by fast atom bombardment mass spectrometry (FABMS). The mononuclear o- P2 complexes [M( o -P2) 2 ](BF 4 ) 2 (M = Fe, Pd, Pt) and [Co( o -P2) 2 (NCCH 3 ) 2 ](BF 4 ) 2 were synthesized from reactions of the free ligand with the fully solvated BF 4 - salts [M(NCCH 3 ) n ](BF 4 ) 2 (M = Fe, Co, n = 6; M = Pd, Pt, n = 4). The dinuclear P4 complex, [Pt 2 (P4)(NCCH 3 ) 4 ](BF 4 ) 4, was produced by reacting the free ligand with PtCl 2 (NC 7 H 5 ) 2 followed by abstraction of the chlorides with AgBF 4 in acetonitrile. Reaction of [Pd(NCCH 3 )](BF 4 ) 2 with 1 equiv of P4 produces the polynuclear compound formulated as [Pd(P4)] n (BF 4 ) 2 n which was characterized by infrared, 1 H, and 31 P{ 1 H} NMR spectroscopies and elemental analysis. The use of FABMS in this study was undertaken in order to elucidate the chemical options of multiply charged cations in the desorption process from the liquid matrix to the gas phase. The use of additives to the FAB matrix ( m -nitrobenzyl alcohol) was demonstrated for the P4 complexes which do not give spectra in this medium due to a high positive net charge. The addition of triflic acid (HOTf or CF 3 SO 3 H) to the FAB matrix/analyte solution was shown to assist in the MS analysis of cationic complexes with up to six charges and a mass range up to m / z 4000. When HOTf is added, bound OTf - anions are formed and are attached to the cationic complex, lowering the net charge to +1. The method of using matrix additives as opposed to chemically synthesizing the OTf - compounds is a convenient in situ method which produces species that are capable of being analyzed by FABMS.
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Asara et al. (1998) studied this question.
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