Chemistry in Acetone Complexes of Metal Dications: A Remarkable Ethylene Production
Pathway
Jianhua Wu, Dan Liu, Jian-Ge Zhou, and Frank Hagelberg*
Computational Center for Molecular Structure and Interactions, Department of Physics, Atmospheric Sciences,
and Geoscience, Jackson State UniVersity, Jackson, Mississippi 39217
Sung Soo Park
Computer-Aided Engineering Group, Samsung Electro-Mechanic Co. Ltd., Suwon, South Korea
Alexandre A. Shvartsburg
Biological Sciences DiVision, Pacific Northwest National Laboratory, P.O. Box 999,
Richland, Washington 99352
ReceiVed: December 13, 2006; In Final Form: March 15, 2007
Electrospray ionization can generate microsolvated multiply charged metal ions for various metals and ligands,
allowing exploration of chemistry within such clusters. The finite size of these systems permits comparing
experimental results with accurate calculations, creating a natural laboratory to research ion solvation. Mass
spectrometry has provided much insight into the stability and dissociation of ligated metal cations. While
solvated singly charged ions tend to shrink by ligand evaporation, solvated polycations below a certain size
exhibit charge reduction and/or ligand fragmentation due to organometallic reactions. Here we investigate
the acetone complexes of representative divalent metals (Ca, Mn, Co, Ni, and Cu), comparing the results of
collision-induced dissociation with the predictions of density functional theory. As for other solvated dications,
channels involving proton or electron transfer compete with ligand loss and become dominant for smaller
complexes. The heterolytic C-C bond cleavage is common, like in DMSO and acetonitrile complexes. Of
primary interest is the unanticipated neutral ethylene loss, found for all metals studied except Cu and particularly
intense for Ca and Mn. We focus on understanding that process in the context of competing dissociation
pathways, as a function of metal identity and number of ligands. According to first-principles modeling,
ethylene elimination proceeds along a complex path involving two intermediates. These results suggest that
chemistry in microsolvated multiply charged ions may still hold major surprises.
1. Introduction
Complexes of metal ions with organic and biological mol-
ecules are a topic that combines problems central to many areas
of science. Of interest to physical chemistry is the formation of
solvation shells and order in solutions
1
and the structural and
phase transitions in finite systems.
2
For inorganic chemistry,
the issues are metal coordination in solid-state complexes
3,4
and
fundamental organometallic reactivity including the metal
catalysis of bond cleavages.
5,6
For biochemistry, ligated metal
ions are useful models to understand biological and toxicological
processes that involve metal binding,
7-9
for example with
respect to hemes and metalloproteins.
7
From the analytical
viewpoint, peptides and other organic molecules cationized by
metals tend to fragment differently from protonated analogs.
10-13
This often provides more specific or complementary mass-
spectrometric identifications, in particular aiding isomer separa-
tions
12
and proteomic sequencing strategies.
10,11
The variable
yet finite size of microsolvated metal ions makes them an ideal
laboratory to develop and validate theoretical methods, such as
the geometry optimization algorithms and model potentials
needed to describe larger complexes, mesoscopic “droplets”,
and solutions.
14,15
For smaller complexes, first-principles
calculations
16-18
are crucial to interpret and guide experimental
work.
The field of microsolvated metal ions has started from singly
charged species, which remain the subject of most studies to
date. Those complexes are readily produced by many means,
including sequential adsorption of vapor molecules on a bare
metal cation. Condensation of neutrals on ions is exothermic,
and such clusters grow to essentially any size, depending on
the vapor temperature and pressure. Ligation of multiply charged
metal ions in that manner is prevented by charge reduction. The
second and higher ionization energies (IE) of nearly all metals
exceed 12 eV (Table 1), while the first IE (IE1) of typical
organic molecules range
19
from 8 to 12 eV (9.7 eV for acetone
considered here). Hence the transfer of electron from a ligand
(L) to metal ion (M) is normally exothermic and occurs on
contact, followed by immediate dissociation driven by Coulomb
repulsion. Even when the IE1 of L exceeds the second IE (IE2)
of M, charge reduction precluding complex formation may still
proceed by other routes. For example, an attempt to add water
(IE1 ) 12.6 eV) to Ca
2+
results in an interligand H
+
transfer
yielding
20
CaOH
+
and H
3
O
+
.
However, polyvalent metal ions are stable in bulk solutions
due to charge stabilization by many solvent molecules. Hence
* To whom correspondence should be addressed. E-mail:
frank.d.hagelberg@ccaix.jsums.edu.
4748 J. Phys. Chem. A 2007, 111, 4748-4758
10.1021/jp068574z CCC: $37.00 © 2007 American Chemical Society
Published on Web 05/16/2007