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THE ESTIMATION OF THE
RATE OF CHANGE OF CHELATE RING
CONFORMATIONS IN
TRISIETHYLENEDIAMINE) COBALTGIDIONS

Thesis for the Degree of B. 3..
MICHIGAN STATE UNIVERSE?!
DAVID L. COX
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ABSTRACTl

THE ESTIMATION OF THE
RATE OF CHANGE OF CHELATE RING

CONFORMATIONS IN TRIS(ETHYLENEDIAMINE)
COBALT(III)IONS

By
David L. Cox

The PMR Spectrum of Co(en)33+ in acid solution over
a large temperature range consists of two broad bands, one
due to amine protons, and one due to methylene protons.
The accepted explanation for this observation is that the
chelate ring conformation is rapidly changing so that the
expected multi—lines spectrum is averaged into two broad
peaks. Using appropriate chemical shift and coupling con—
stant data it is possible to calculate the rate constants
required to fit the available experimental data. for the
cobalt(III)ion complexes in the DZO/szoh solvent system.
Several theoretical systems can be used to explore the rate
of inversion of the chelate ring. The best model system
found was the AA'BB' system for this bidendate system. The

results suggest a AEaCt;l.4 kcal/mole for the ring.

1Work sponsored by Lyman Briggs College

THE ESTIMATION OF THE
RATE OF CHANGE OF CHELATE RING
CONFORMATIONS IN TRIS(ETHYLENEDIAMINE)
COBALT(III)IONS

by

David L. Cox
Lyman Briggs College
Michigan State University

January 26, 1974

Submitted

February 26, 197“
In Completion of LBC #95 B.S.
Requirements For
Lyman Briggs College

Dedicated to

N. L. Sutton

ii

FORWARD

That which is about to transpire between these two
covers represents the final efforts of three years of work
and many resources that will never be seen by the reader.
The peOple, however, I have noted in the next section, and
much of the credit and praise for this work is due in
large part to them.

Any effort of this type is only as good as the infor-
mation and guidance available. In this, I must thank my
advisor, Steven T. Spees, Jr., for his good help. The
results of his advice are presented here.

Special thanks go to Kathy Brown of Lyman Briggs
College who did the final draft typing.

D.L.C.

Christmas 1973
Kalamazoo, Michigan

iii

ACKNOWLEDGEMENTS

I would like to express my deep gratitude to the fol-
lowing individuals and/or groups for the generous help and
support they have provided in the preparation of this work.
By organization,

Lyman Bpiggs College

Dr. Fredrick B. Dutton, Dean, Ret.
Dr. Michael J. Harrison, Dean

Dr. Jane E. Elliott, Assistant Dean
Ms. Dori Card

Ms. Sandra Conner

Dr. Steven T. Spees, Jr., Associate Professor
Dr. Paul M. Parker, Professor

Dr. Edward H. Carlson, Professor
Mr. Geoffrey Gates

Mr. Harold Grossman

Ms. Jennie M. Orr

Ms. Debbie L. Roovoetts

Ms. Mary T. Ashely

Mr. Alan A. Parker

Ms. Susan A. Panek

Mr. Luther F. Cobb

Mr. Mark A. Liebow

Department of Chemistry

Dr. Harry A. Eiok, Assistant Chairman
Dr. Donald G. Farnum

Dr. James E. Harrison

Dr. Fredrick H. Horne

Dr. William C. McHarris

Dr. Max T. Rogers

Dr. Richard H. Schwendeman

Mr. Ralph A. Sides

Department pf Computer Science
Mr. Ron T. Mains
Dr. Julian Kateley
Dr. Harry A. Eick
Mr. Dean H. Franklin
Department of Physics

Dr. Paul M. Parker

iv

Computer Laboratory

Dr. Lawrence W. Vontersch

 

IBM Corporation

Kalamazoo Branch Office
Kalamazoo, Michigan

Upjohn Corporation

Data Processing Department
Portage, Michigan

Western Michigan University

Waldo Library
Kalamazoo, Michigan

 

Merrit Enterprises
East Lansing, Michigan
Calcomp Corporation
Palo Alto, California
D.L.C.

Christmas 1973
Kalamazoo, Michigan

Table of Contents

Table of Charts, Figures, and Graphs

Synopsis .

Historical Perspective

Introduction .

Experimental Section .

Sample Compounds .

Sample Spectra .

Computational Checks .

Computational Methods.

Computer Programs.

Results. .
Discussion .
Conclusions.
Afterword.
Addendum .
Footnotes.
Appendix I
Appendix II.
Appendix III
Appendix IV.

vi

WWNH

Table of ChartsI Figures. and Gpaphs

Introduction

Figure
Figure
Figure
Figure
Figure

Sample Spectra

Table
Results

Table

Graph

Appendix I

Graph 1 .
2 .
Graph 3 .

Graph

Appendix II

Figure
Figure
Figure
Figure
Figure

Appendix II

Table
Table
Table
Table

l .

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. 45

. #7
. #8
. 49
. 50
. 51

Syn0psis

The application of PMR techniques in the field of
inorganic coordination chemistry is relatively recent, pri-
marily develOped in the last ten years. Additionally, the
integration of modern ultrahigh speed digital computers in
the analysis of inorganic experimental PMR evidence is even
more recent. Together, they provide powerful tools for the
resolution of many puzzling questions about transition metal
complexes.

One of the puzzling questions of the last few years
among many in the field of coordination chemistry has cen-
tered around the bidendate ring systems bonded to the
cobalt(III)ion. Until recently, it was not possible to
obtain high resolution variable temperature PMR spectrums of
the ion. Many researchers attributed this 'smearing' to the
strong 0059 interaction with the ring protons. The intro—
duction of NMR double-irradiation techniques, and pulsed
wave sampling have resolved this problem. The broadly smeared
signal can be resolved into a high resolution fine-structure
spectrum. Parallel to this, the problems of computational
analysis have been resolved. Using these advances, this
paper presents theoretical evidence based upon experimen-
tal results for a specific AEact for the inversion of
E0(NHZCHZCH2NH2)3] 3+ of 1.1» kcal moi"1 in the Dzo/szou
solvent system, as well as generalizations about the ther-

modynamic values to be found in several other solvent systems.

2

Historical Perspective

Over the last ten years an impressive array of pa-
persz-l"2 have dealt with the problems encountered in PMR
studies of certain inorganic coordination compounds and
related experimental and theoretical problems. Many of
these early papers were concerned with the problems of
resolution and analysis. Later the emphasis of these papers
shifted to the analysis of high resolution PMR spectrums in
different solvent systems. Finally, the last few papers
have been concerned with solvent and temperature studies
of Cobalt59 complexes. In this evolution many important
questions of structure, bonding and stability were answered.
These papers have gone on to the broader implications of
bidendate chelate ring systems, with reSpect to metal-
hydrogen coupling, ring activation energy, NMR fine struc-
ture constants, ring and complex-solvent interactions.

Parallel to these works have been the efforts of a

u3-uu

few in the field of computational chemistry that have
made analysis of laboratory data rapid and easy. With the
present third generation ultrahigh-speed digital computers,
now available solutions can be had in less than one minute

of machine time.“5

Introductipp
Of all inorganic coordination compounds studied in
recent years, perhaps the tris(ethylenediamine) complexes
of Cobalt59 has been the most studied of all. Other
3

complexes of this ligand are similar in many respects, but
there are important differences in this diamagnetic complex
and similar ones.

In general, they are of the type M(en)3, but all show
different CH2 resonances33, depending on solvent and temp—
erature. The ethylenediamine chelate ring has been found

26

to have a puckered conformation. PMR has made it possible
to determine the various conformations of the ligand, based
upon the Karplus relationship of vincinal proton coupling
constants to the dihedral angle19 formed by the ring.
However, a reexamination of theoretical metal com—
plexes should be presented here, so that several facts may
be noted later. First, with reSpect to the Me-N bonding
distance in M(en)3, it has been shown, that as this distance
increases, an increase in the ring energy is noted for the
complex.33 This indicates that the system acquires greater
degrees of freedom as the bond length increases, so that
between any two conformations, less of an energy barrier
should be present. An examination of the ng electrons of
the M(en)3 complex33, would confirm the above statement.
Thus, as the degree of puckering of the chelate ring in-
creases, a broading of the CH2 signal would be detected.12
This is reasonable, since it is known that, the differences
between the chemical shifts of any two proton sites which
are similarly directed with respect to the greatest metal

ion electron density, the axial protons being shielded more

by the metal ionu7, than the equatorial protons.

5

The metal complex may exist in two different conformers
as shown in Figure 2, 6(del) and A(1el), which are separated
by a very shallow energy barrier.33 Thus, it is possible
for conformer inversion to take place about the metal ion.“8
It should be noted that in the A(lel) configuration (D3) all
three of the chelate rings about the complex are equivalent.
Thus, when conformation inversion occurs, the symmetry is
altered radically (133:3 CZ). Thus the two axial and two
equatorial CH2 protons are related by a C2 symmetry Oper-
ation.3l+

It follows that there must be an exchange rate be-
tween these two conformers provided enough energy is present
in order to produce the exchange.l+7’l+9 This implies temp-
erature dependance, and research)+7 indicates that this is
a reasonable first approximation. Thermodynamically, though,
one conformation will be favored over the other. The impli-
cation of this is both conformers will not normally have the
same energy, and is born out in the fact that a single line

in the PMR is not usually seen,12

with the exception when
both are equal. In that case, a broad peak or fine-structure
is seen, 9-19 depending on the degree of metal-ligand
coupling, and temperature. Thus, for the A configuration

of the chelate rings about the metal ion, the free energy
series has been shown to be,“7

A(666)<A(56l)<A(6AA)<A(All)
the Me-N-C bond angle and the Me-N bond length being the

deciding factors in this series.

6

Since one configuration is heavily weighted in terms
of energy over the others, a set of populations of each
configuration species may be deveIOped. In general, they
are not equal for a M(en)3 complex, but are in fact weighted
heavily towards the A(lel) configuration.33 However, this
can not be predicted from the PMR directly since the intrin-
sic chemical shift difference between the adjacent proton
sites can not be obtained from the spectra of the ethylene-
diamine complex without an exact knowledge of the relative
populations of the various configurations.47 It has been
proven in general that as the Me—N bond increases towards
infinity the chemical shift difference reduces as the
6(del) conformer becomes more populated. Thus the A(665)
state is more populated. This is obvious from thermodynamic
considerations.33 Also, in general, the intrinsic chemical
shift difference is dependent on the Me—N distance.u7 This
is reasonable, when a consideration of the shielding effects
of the metal ion electrons. Also, secondary effects may or
may not enhance the spectra.36 So, in general, for a M(en)3
complex, the CH2 proton environment, based on symmetry, is
AA'BB'.35 Then, from a view of a theoretical M(en)3 metal
complex, the complexes of Cobalt59 may be approached.

Considering Cobalt59 as the central metal ion in the
complex some additional facts may be noted. The structure
of23’47 [Co(NHZCH2.CH2NH2)g13+ is shown in Figure 1. Note
that the Co-N bond distance is shorter than the theoretical

value of a 2.0°A. Also, note that the N-Co-N bond angle

7

is not exactly the theoretical value of 90.00. Due to

these differences, the ring is slightly more puckered than
what a theoretical prediction should predict. Finally,

note that the Co-N-C bond angle is slightly deformed in the
non-planar puckering of the ring. This forces the N-C and
C-C bond lengths to assume unusual values for a single
bonded state. Also, note that due to the oxidation state of
the Cobalt-59 metal ion, the shielding effects will be
pronounced, as well as metal to ligand hydrogen coupling.
The net effect will be to "smear” the PMR signal. This has
been shown12 in Figure 2. As a side note on secondary
effects the formation of hydrogen bonds between the NH2
protons and basic solvents is known to be reflected in

NH2 signal smear.46 However, as with the theoretical

metal complex, Co(en)33+ has a three fold axis of symmetry
46

about which the three ligands lie. This confirms that

a AA'BB' pattern should be seen,12

for the methylene
protons. This pattern is not seen exactly, since Co(en)33+
may have two stereoisomers,12 D-[Co(en);]3+ and
L-Eo(en)3]3+, as well as four different conformers of

each isomer,3

L(555) 59% D(666)
L(65x) 27% D(65x)
L(5xx) 8% D(AA6)
L(AAA) uz D(AAA)

 

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FIGURE 1. Structure of [Co(NH2CHZCH2NH2)33f]. Note
that N“N indicates exact duplication of the detail.

KEY BOND

a N-CO-N

B Co—N-C
KEY BOND

l Co-N

2 N-C

3 0-0

h N—Ncross

5 N-H

6 C-H

AHQLE§
Bond Angle ~85.8o
Bond Angle ~101.3°

LENGTHS

Maximum 2.0AO

Mean 1.953A°

Mean l.u99A°

Mean 1.509AO
Average 2.79-2.83AO
Mean 2.50A°

Mean 1.10A°

theikconfiguration of the chelate ring has the 0-0 bond
parallel to the three—fold axis in the D-form, and the
same is true of the A configuration in the L-formlz.

Thus the system reduces to,37

 

 

555 l D<2%
A66 5x5 66A 3 C<1%
Al5 A5A 6AA 3 B~30%
AAA 1 A~YO%
ratio populations

This result37 leads to the fact that e =65;120° as shown in

A

Figure 2. The dihedral angle W between the N-C-C planes

6

can be used to predict a vincinal coupling constant from

the Karplus equation.9 Thus in the case of the theoretical

2
eab

observed coupling constant between vincinal protons Ha and

metal complex, Jab=JOCOS -C holds, where Jab is the

Hb’Jo is a constant for the dihedral angle 9 of 00-900

between C-Ha and C—Hb and C is a constant.50

 

C\/ no: a; S ram (be)
\ /,I\

FIGURE 2. Newman projections of the conformational
interconversion of A to 5 of the NHZCHZCHZNH2 ring.

11

It has been calculated that to flip from the A form
to the 5 form requires 0.5 kcal mol-1 in free energy.37
However, secondary effects which are temperature dependent

do have a great bearing on the rate of exchange,36 but it

d"51 12

is known that this rate is "rapi at room temperature.
It must be remembered that overall for the entire compound
the energy difference between the conformers with the CH2
group in the axial and equatorial position is close to

2 kcal mold”,12 so that greater than 93% of the ligand is
equatorial with respect to the CH2 groups.12 Note that this
is born out by the PMR spectra presented in this paper. It
should be expected that the rate of exchange will vary di-
rectly with the temperature all other factors being held
constant.52 The results of such a study is presented in
Table 1 showing that the line width does vary as a function
of temperature. Also, note the change Jab values, indicat—
ing that the Karplus angle decreases as the temperature
increases.

It should be noted that neither the CH2 group nor
the NH2 group can be equivalent, even if there is a rapid
conformational equilibrium with no conformational prefer-
ence.36 This gives, as previously noted, rise to the
equitorial and axial signals of the CH2 and NH2 protons,
Figure 3. As already stated, these signals are known to be

highly dependent on solvent effects16

as well as tempera-
ture.37 It is known that the choice of solvents will

effect the relative pOpulations, exchange rate, and the

12

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13

intrinsic chemical shifts of the proton signal.33 Some

solvents such as TFA, Figure A, are known to produce a

16

as shown in Figure 3, while DMSO is known

16

rigid structure
to allow rapid exchange. Another example is the inversion
of the NH2 protons at different temperatures,16 as shown in
Figure 5.

It has been shown that the line shape depends upon
the exchange rate (éfl), chemical shifts (6r), coupling
constants (J), and the natural line width (l/Tzor).5# Of
these factors, the exchange rate is temperature dependent,
and the transverse relaxation time is solvent dependent, as
well as the chemical shifts. Ignoring these effects, it
would be expected that the AA'BB' spectrum of the CH2 pro-
tons would be symmetrical.u7 However, this is not the case,
and thus these effects must be pronounced.5u Next it would
be expected that at low temperatures an increase in line
widths would be observed due to increases in the axial-
equatorial chemical shift difference. Thus it would have
a slower rate of exchange.55 An example of this broad-line
spectrum is the spectrum seen of Co(en)33+ (Figure 2), in
which a very broad band (width at % height~l8Hz) is ob-
served, due to the overlapping lines of the AA'BB' pattern.12

In reference to the broad CH2 band in the PMR of
Co(en)33+, several different effects have been observed by

different researchers. Note that the CH band (19-21 Hz

2
at 2.85 ppm) sharpens (17-19 HZ) when the NH2 protons under-

34

go D20 exchange. The peak may be resolved down to -39°C,

11+

in new.“ .30.; swam oN

Q USN .<.mB H3.” +mmnflmvoo .HO N32 OOH Pm thome Exam” .3 mmDUHm
of:
o.m b, o.m
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15

with a decrease from 21 ops to 18 ops of width at % height
12

2.

a highly unsymmetrical peak is present,3u and it is assumed

with deuteration of the NH Figure 5 shows that at 820C

that the high narrow side of the peak due to the symmetrical
A(D3) configuration, and that the low broad side peak is due
to the 5(02) configuration. As for the NH2 band found in
the PMR of Co(en)33+, at n.48 ppm (3h-37HZ) since the N atom
has a tetrahedral configuration in Space, two kinds of NH2
protons are present, (a) three upwards from the N plane,

and (b) three outwards, perpendicular to the three-fold
axis.16 In some studies,56 the amine peak appears in the
same spectral range as the water peaks, and thus it is dif—

ficult to observe these upon exchange. In neutral to basic

10

solution, the peak disappears somewhat, because of rapid

exchange of the NH2 protons with the water protons. However,
due to different conformers, it would be expected that two

broad distinct NH2 peaks would be seen if a rigid structure

12

is present , and if not, a single line due to the PMR time

average effects.l6 What is observed is however highly de-
pendent on the solvent system used in the PMR study.3u
Another factor that is known to influence the reso-

lution of the Co(en)33+ fine—structure is the metal to

ligand proton coupling constant (JCo-H)‘ It is known that

the sharpness of the H lines tend to indicate that the

axial
JCo-N-C-H constant is greater for the equatorial than for

#6

the axial protons. Values of J

Co-H,axial~2'75 and

~ 46 . . .
JCo-H,equatorial 2.93 have been suggested, indicating

16

I-—-—""\
61’ 51’

FIGURE 5. 100 MHz PMR spectrum of NH2 proton signal
in Co(en)33+ in isobuthric acid at different tempera-
tures.

17

that the Cobalt-59 coupling is long range and large, due to
the scalar coupling between protons from the dihediral angle
dependance.“7 The overall effect is to ”smear” the Spectral
peaks of both the CH2 and NH2 proton bands. Thus, the cen—
tral problem of PMR Spectra of Co(en)33+ is to obtain inter-
mediate inversion rates of the puckered five-membered chelate
rings, against the residual paramagnetism and spin—spin

coupling of the protons of 00-59, with reference to pH.57

Experimental Section

2—h2,46-49.5u previously cited

Most of the papers
were concerned with the actual observation of the proton
signal and the resultant verification of observed Signal
parameters by computer techniques. Many of these research-
ers choose to take experimental Spectra and then use a first
order type of analysis upon their data with several common
PMR programs.“3 In this work, a theoretical approach was
taken,‘i§, experimental data was used as a starting point
to develop thru parameter refinement the theoretical PMR
Spectra that approximated an observed laboratory spectra.
Different experimental conditions were chosen in order to
obtain a wide range of PMR spectra fits. From an approach
of this type, such items as the JCo-N values, AEact of the
ring.Aspliting, andxpopulations can be found explicitly
based upon the fact that it is nearly impossible to obtain
this type of data for the Co(en)33+ system from experimen-

tal PMR spectra. The advantage is that many of the second

and higher order corrections and analysis parameters may be

18

included in a given calculation, and varied to fit the
predicted spectra to the actual PMR Spectra for a given
experimental data set. The experimental data set in every
case was used as basic input in the computations, in addi-
tion to the parameters to be fitted, chosen from ”best"
known values, then refined upon successive calculations.
The method is similar to iteration with the exception that
only parameter values in realistic ranges are allowed in
the refinement process.

The basic experimental data for Co(en)33+ chosen
was the work of Sudmeier, 2:; al;,58 being the most recent
variable temperature study of the decoupled, deutrated

12 was also

chelate structure. The work of Spees, et. al.,
consulted for historical reasons, and in addition unpublished
research data in parameter choice was used, as were private

communications from Spees.51'52'55

Sample Compounds
All sample compounds used by the original authors
were prepared by well known procedures.58’12'3'1u'19’30’3u
These works should be consulted for exact preparation tech-

niques.

Sample Spectra
With the exception of the Spectra of Spees,5l-52'55’12
all other spectra consulted were in the original journal
article cited. All experimental data reported in each

article was verified before use by insertion into the original

l9

 

 

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as.o m.ma- m.: 5.: 3.0 mma.o c.a cc HH
as.o m.ma- m.: m.: d.m cea.o m.a mm H
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W 3M. ems me NW. me meemws Baum
+MAvaoo mom mhmpwamumm Hmupomgm Hapsoswgomxm .H mqm<e

mm

20

program. No major discrepancies were found to exist in this
data, other than a normal error range of the data present in
all such first order type approximations. In each case,
spectra were copied and very carefully matched to the pre—
dicted PMR spectra computed. An error tolerance of reason-
able amounts was employed, consistent with the range of the

original authors in any matching spectra employed.

Computational Checks
As a check on the calculated PMR spectra for each
case considered, all input paraMeters were varied with in
the error range allowed to confirm goodness of fit. Any
major deviations noted were grounds for complete recalcu-
lation to obtain a better spectral fit. In all cases this
was necessary, a better fit resulted, and the final para-

meters were noted.

mepptational Methodg

A general theory of line shapes in high-resolution
PMR spectra of liquids can be deve10ped59-75 in the frame-
work of the Liouville representation of quantum mechanics.
It can be shown59.6O that both short memory as well as strong-
correlation effects can Simultaneously be accounted for in
a compact and transparent manner if the full—state vector
is projected into a composite liouville subspace. The
equation of motion is governed by a complex non-hermitian
Operator that may be broken up into an ordinary Hermitian

Liouville operator, a relaxation Operator, and an exchange

21

62 that the total informa-

Operator. It can be demonstrated
tional content of an unsaturated steady-state PMR spectrum
can be contracted into two complex vectors, a radio frequency-
independent ”shape vector," and a "Spectral vector," which

is a trivially Simple function of the radio frequency.

Thus, calculations for exchanges of a system can determine

the rate constants and activation parameters present ac-

curately in the system of interest.

Computer Programs

The equations refered to in the previous section
were programed in to a Fortran V program for a 320K Control
Data Corporation 6500 machine with a Calcomp 1200 series
drum plotter. Intermixed machine language, Compass, was
used to interface with the plotter. In the process of
conversion and interface several corrections and additions
to the original program were made. These have been noted
in the listing. All computing was done at the Michigan
State University Computer Laboratory in.East Lansing.

The input to the program, called DNMR3, consisted
of chemical Shifts, coupling constants, pOpulations, rate
constants, the effective transverse relaxation time, and
the scaling parameters for the resultant plot. These para-
meters are read in by a subroutine STADAT. A subroutine
BASIS generates the spin-product basic functions for a
Specified number of coupled spin % nuclei, and HAMILT

assembles the Hamiltonian submatrices. The Shape and

22

Spectral vectors along with some auxiliary index arrays are
computed in PRJECT. The composite submatrices are assembled
in TRAMAT, and diagonalized individually by a package of
routines called PERMUT, EIGEN, ALLMAT, NVRT, TRAMAT, CONVEC,
and MAGEQ. ‘In these the eigenvalues and the right eigenvalues
are found by an iterative inverse power deflation algorithum.
NURT is used to invert the resultant matrix to produce the
left eigenvectors, which are accumulated in the shape and
spherical vector. Finally in a routine called SPECT, the
plotting is done. In doing the calculations in this way,
the acutal time of finding a solution is reduced greatly
since the program takes full advantage of all symmetry and
magnetic equivalence factors present.

As a reference check, the resultant spectrum was
used as input to L000ANIII.”3 This is a program that em-
ploies an interative method for a least—squares analysis,
which is not affected by symmetry in the hamiltonian, and
yields an estimate of the ellipsoid of error in the con-
vergance. As a final check, NMRITJ‘"3 was used. This is
a PMR iterative program which compiles the Hamiltonian
matrix from chemical Shielding parameters and Spin-spin
coupling constants. The matrix is diagonalized, and the
resultant eigenvalues are then compared with the energy
levels derived from the calculated spectra. Differences
are then used as the iteration process times to make con-
vergence. Both LOCOANIII and NMRIT were written in

Fortram IV in a modified form for use with the CDC 6500

23

system available. The entire process of parameter refinement
for each case took on the average 4 runs of each program in

succession.

BSEEIES

A number of different temperature cases were con-
sidered within the specific solvent system chosen. The
solvent system of N-deuturated Co(en)33+ in neutral D20 was
used without the use of any Spectator ions as the experimen-
tal data basis set.58 This experimental data is summarized
in Table I. The data used was verified as accurate by pre-
viously mentioned computational checks. In each temperature
case the original input data was refined as the additional
parameters were added. These refined experimental data
parameters are presented in Table II.

In determining a Spectra match at given temperature
for a rate constant the computational plot of the spectrum
was matched on the basis of half-width at half-height. A
constant width value was the basis for the rate constant,
extracted, with a normal error tolerance of 10.25 cps.

As input parameters, the effective transverse re-
laxation time, T2, was the most difficult to determine. As
previously noted, the T2 value is not constant over a wide
temperature range. However, the assumption was made that
the variation is on the order of less than an order of
magniture for the Specific temperature cases considered.
These values were estimated from the width at half height

(*w), ie, T2=1/2flw. The values are noted also in Table II.

h».

 

he moan: acm.a mes.o m.ma- e.s m.m «.0 wma.o o.m ma HHH
coaxm som.a mms.o m.ma- m.: s.: e.a mma.o o.H om HH
moaxa mad.o mms.o m.ma- m.: m.: m.o csa.o N.H mm H
-oom Icon a m m m x 2mm x 0 ends
a a a me e ems ems mme mme m4 mmaHz .msma
n mZHA

 

mm +mc 2300 no.“ mpopmamm .2956on cmpmasgmo IHnmoEoEfinomxm .N Ema...

25

107 o
E = 1. 412 kcal mol-1
:*=. .5. 562 kcal mol 1 ring-1
- -35 eu
O
106
9+
2:
<1:
54
E
to
c)
0 E3
105 a
O
0.2 0.1+ 0.6 0.8

3+ Temperature (lOB/T)
Co(en)3 ion, decoupled in.D20, rate constant (log K, see

vs. temperature (103/T, OC)

1)

26

With respect to the rate constants, it has been
noted by researchers76 in the Co(en)33+ system that the k

1 and 109 sec.-1 on the basis of

values should be between 10
solvent-solute interaction, and lattice relaxation effects.
With this range as a basis an apprOpriate rate constant in
each case. From these, a graph of log k vs. l/temperature

yielded a straight line with slope equal to the AE

activation
. —1 N ,1
of the ring, 1.412 kcal mole , and values ofAHring=O.5,62
kcal mole-Iring-l, AS°=-35 eu.

With respect to the model systems used in the cal—
culation of the spectra of the N-deutrated, decoupled
Co(en)33+ ion in D20, only the AA'BB' system was found to
be applicable, since the rate of chelate exchange was not
sufficiently high enough to allow the substitution of the
AB system. Doing so, produced gross errors which could not
be resolved by any means.

In regards to the value of the JCo-H constants in

the non-decoupled system for Co(en)33+, the values of

Jaxia1~2'75 ppm, J
46

et. al.,

equatorial~2'93 ppm suggested by Fung,
were found in several computations with the above
results to ”smear” the spectrum sufficiently in the AA'BB'C
system to approximate closely the observed PMR spectrum.
This AA'BB'X computation neglected the intrinsic spin of
Co-59 (I=7/2) as well as any quadrapole coupling effects.

By theoretical arguments, both effects can be shown to not

enhance the Spectra calculations significantly with respect

to the overall effect being studied.77

27

Discussion
In the context of the solvent system considered, an
activation energy, enthaply, and entrOpy for the chelate ring
of Co(en)33+. This has been deve10ped for the total system,
and from the figure of 0.5 kcal mole“l per ring stated

1 overall which is well within

1

earlier37 gives 1.5 kcal mole-
the computation figure of 1.412 kcal mole- deve10ped in
this paper. The difference must reflect the deviation of
the solvent system from the ideal solvation system. If a
solvent system was chosen which was more polar than the
test system, it would be expected that the electron density

to decrease for the T electrons, the Co-N distance to in-

2%
crease slightly, and the CH2 protons to become less shielded
with respect to the equatorial hydrogen protons, a decrease
in the A conformer due to the lowering of the exchange energy

barrier. Thus, a decrease in the AE for the ring

activation
should be noted, as well as a corresponding increase in the
exchange rate. This would be reflected in a reduced half-
width, and if the solvation system of 0.1M PO“: and D20 is
chosen, these are noted by one researcher58 in the PMR
Spectrum. Since these effects occur, the chelate ring may
be thought of as being "unlocked" by the soluation system.

A general rule may be postulated considering these cases,
ie, the more polar the nature of the solvent system employed

with the Co(en)33+, the more chelate ring will be able to

undergo conformational changes.

28

With respect to the very unique temperature depen-
dance of Co(en)33+ already deve10ped, several factors may
be taken into account in the explanation depending upon the
model system chosen, different factors are postulated to
predominance. If the spectator ions as well as the viscosity
of the solvent are considered, along with the solvent-complex
molecule size the observed PMR spectra may be explained. It
has been postulated that as the effective polarity of the
total solvation system increases, a decrease in line width
Should occur. If hydrogen bonding is present in the solva-
tion system, a population altering condition will also
occur, with the conformers becoming more equal in weighting.
This solvent-complex interaction, based on the calculations
of this paper, may alter the exchange rate, thru the effec-
tive transverse relaxation time. These efforts are in
addition to the effect of solvent molecule Size. If the
solvation lattice about the complex is altered by increasing
the solvent molecule size by the addition of spectator ions,
the case about the complex will increase, thus "unlocking"
the ring. Also, if the spectator ions are polar in nature,
the ionic effects--imparted to the solvent system will con-
tribute to this ”unlocking" effect upon the ring. An exam-
ple of this type of effect is the solvation systems of TFA
or DMSO and the result effects upon the peak widths.37’3u'u8-u9
The TFA solvation system locks up the chelate ring and thus
"smears" out the PMR signals of the CH2 protons, while the

DMSO solvation system being polar, has the effect of unlocking

29
the chelate ring, and allowing a fine structure to appear.
This indicates a lowering of the energy barrier and a
resultant exchange rate alteration consistent with the
previously postulated rule. If the total Co(en)33+ system
is considered in relation to the temperature dependance with
reference to other transition metal complexes of ethylene-
diamine several factors may be presented to explain this
observation Co—59 has one of the greatest quadrapole moments
of the transition metals which influence the magnetic hamil-
tonian. As the temperature increases, it would be expected
that the bonds would be more flexed by the ring distortions
due to the quadrapole influence. These bonds will be held
in check by the adjoining NH2 groups along with the natural

12 and N14

tendancy of the C atoms to resist radical bonding
angle strains, regardless of temperature. In other M(en)3
complexes the bonds are more rigid and less subject to strain,
due to the absence (or lessening) of the quadrapole term in
the 00-59 hamiltonian. At low temperatures, it would be
expected that the solvent molecules would have limited mo-
tion, due to increase viscosity, along with the complex
molecules. As the temperature increased the solvent and
complex molecules should undergo greater motion, moving the
activation energy barrier downwards. However, the solvent
molecules must increase motion at a greater rate than the
complex, given the above postulated hindrences. During

this process, the CH2 protons would be subjected to vari-

able solvent and hydrogen bonding. This will be reflected

30

in the observed PMR signal as a change in the line width.

It would follow that less complex-solvent bonding interac-
tions the higher the activation ring energy. These factors
suggest that for the Co(en)33+ complex, solvent effects are
pronounced secondary effects. Since the degree of secondary
solvent effects is in relation to the quadrapole form in the
Co-59 nucleus, other transition metal complexes of ethylene—
diamine must not display these solvent effects as greatly

in their PMR spectrums.

This large quadrapole term would as tend to account
for the size of the JCo-H constants, which are large con-
sidering the distances involved. These large values smear
out the CH2 proton Signal in Co(en)33+ complexes, but in
other complexes, noteably Ru(en)33+, a fine-line spectra is
observed. The distances are longer in the Ru(en)33+ case
along with the fact that the quadrapole term is much less.
In the other complexes of ethylenediamine better resolution
is noted in the PMR Spectra, and thus the JMe-H values must
also be decreased in line with decreased solvent effects.

Finally, with reSpect to the question of the effec-
tive transverse relaxation time and the resultant rate con-
stant for a specific temperature case, it must be noted
that no great deviation Should be expected in the T2 for
changing temperatures. There will be some change in T2
due to temperature change, but calculations done for this
paper indicate that it is only reasonable values of T2 will

allow for the correct set of k values to be used based on

31
51

previously noted analysis. These emperically reasonable
values are as previously noted within a factor of ten of each
other, based on the relation of the width at half—height to
the T2 value. If value of T2 were chosen to reflect a re-
laxation time much shorter than postulated, the calculations
indicate that no contribution of the ring exchange rate would
be necessary to achieve peak collapse. If this were the
case no ring motion would be present or if any occured it
would be very light, since the relaxation process would
predominate. This is definitely known to be not correct,
and many researcherslz’26’3u’37 have reported evidence for
ligand motion in Co(en)33+. This must discredit any sugges-
tion of a solvent relaxation phenomenon being present, and
support completely the case for the ligand motion presented
in this paper.

Finally, it should be noted that some researchers,

12

noteably SpeeS, 23?.EE3’ saw water peaks 1n the NH2 pro-

ton range in the PMR of Co(en)33+. These widths78 noted
for the H20 proton peaks also support the case for a T2
value which allows for the exchange rate to be between

101 and 102 sec-l. Measurement of these peaks yields a
half—width at half-height at different temperatures that
give values of T2 that correSpond well with the calculated

T2 values used in this paper.

Conclusions

The success of the results of this work indicate
that the method employed herein is useful in other cases
of transition metal complexes, not only of ethylenediamine
but other ligands. Many such systems undergo conformational
change and thus will give rise to a PMR signal that may be
interpreted by these methods. Some organic compounds also
fall into this analysis technique. The major reason why
this work is perhaps potentially useful is in the analysis
of conformational isomers of biological metal complexes,
such as heme. Many biological molecules are known to be
coordination complexes of transition metals. The PMR Spec-
tra of these molecules may be analyzed by the techniques
used here. In any event, the analysis techniques pre-
sented in this paper do prove that theoretical conforma-
tional analysis of an observed PMR spectra is possible,

and that viable results can be expected from such methods.

Afterword
The author would like to thank Lyman Briggs College
for its generous support of the project, as well as Dr.
Steven T. Spees, Jr., for his assistance. To many other
individuals who have not been mentioned credit is also
due. The results of this work were presented at the Spring

1974 meeting of the American Chemical Society, in Los Angeles.

32

ADDENDUM

Since this work was submitted for publication, several
additional items concerning the computations have been dis-
covered. They are listed below with a Short discussion that
follows.

(1) The J(trans)(ie. for the H-C-C—H dihedral angle,
¢=l80°) and J(gauche)(ie, ¢=60°) spin coupling
constants are too small and too large, compared
to other en complexes.

(2) Distortions of W of the N-C-C-N dihedral angle,
to values larger than 600 are required in order
to explain the magnitudes of the coupling con-
stants.

(3) Because there are no extraneous lines present in
the AA'BB' patterns, it is unlikely than any
conformer other than.555 or All is present to
greater than'~2% abundance. The postulation of
Slow kinetic for ring inversion is not correct.

Because of rapid interconversion, each vicinal coupling
constant is a weighted average of its values in.A and 5 con-

formers, and the following is true

lezfx J12“)”5 J12”) (l)
JlB-efA .1130 )+f6 J13(5 ) (2)
Jlfi‘A J34(1 )+f6 J3u(5 ) (3)

where f; and f5 are the fractions of time spent by each ring

in the A and 6 conformations, respectively since

33

34

fA + f5=l (4)
and then f5 can be eliminated in eq. 1—3. The Karplus rela-

tions of the form,

J=Alcosz¢ 005455900 (5)
J=A2cos2¢ 90°s¢s18o° (6)
coherce ¢ is the H-C-C-H dihedral angle, it can be shown that
.1120 )zizeos2(e,+w,) (7)
J12(6)=Alcosz(66—W5) (8)
J13(A)=Alcos2WA (9)
J13(6)=A1cos2w6 (lo)
J3u(x)=Alcosz(9A-WA) (11)
534(5 )=A2cosz(96 “N5 ) (12)

putting these together.

J12: fAAzcos 2(e +w )+A 16cos2(e -w6 ) -f Alcos 2(95 -w6 ) (13)
J13 =f A lcoszw +A1cos2W6 -f A lcosZW’a (l4)

,5er A 1°08 2(5A 4”; HAZCOSZ (95% )-fAA cosz(96+W6) (15)

2
It was assumed that

(l) 9, =65 =120°

(2) W1=W5

(3) A fixed ration of Al/A2

This new information suggests not only different chem-
ical shifts between the conformations, but also different
chemical coupling constants between the conformations. The

results of this calculation will be summarized in a paper

that is expected to be published in the Journal of Inorganic

Chemistry.

35

1Work Sponsored by Lyman Briggs College.

2E. J. Corey, J. C. Bailer, Jr., J. Am. Chem. Soc., 81, 2620
(1959)

3A. M. Sargeson in Transition Metal Chemistry, Vol. 3, R. L.
Carlin, Ed., Marcel Dekker, Inc., New York, 19 , p. 303+.

“H. L. Smith, B. E. Douglas, Inorg. Chem.,’5, 784 (1966).

5A. J. McCaffery, s. F. Mason, B. J. Norman, A. M. Sargeson,
J. Am. Chem. Soc., 89, 1304 (1968).

6Sr. H. Elsbernd, J. K. Beattie, J. Am. Chem.,‘2l, 4573 (1969).

7J. L. Sudmeier, A. J. Senzel, Anal. Chem., 40, 1693 (1968),
J. Am. Chem. Soc.,‘29, 6860 19 8

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Soc. Japan, 42,3184 (1969)

9M. Karplus, J. Chem. Physc., 30,11 (1956); J. Am. Chem. Soc.
85. 2870 (1963)

D. B. Powell, N. Sheppard, J. Chem;_Soc.,’81, 791 (1959).
11

10

P. Clifton, L. Pratt, Proc. Chem. Soc., 339 (1963).

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5. 2103 (1966)

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(1966).
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18

N. C. Li, L. Johnson, J. N. Shoolery, J. Phys. Chem.,‘jj,
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19D. A. Buckingham, J. P. Collman, Abstracts, l42nd National

Meetipg of the American Chemical Societ , Atlantic City,
New Jersey, Sept. 1962, P- 36N.

D. R. Eaton, W. D. Phillips, D. J. Caldwell, J. Am. Chem.
500-. 55. 397 (1963).

 

20

 

36

21D. B. Powell, N. Sheppard, J. Am. Chem. Soc.,’42, 791 (1959).

22F. Clifton, L. Pratt, Proc. Chem. Soc., 339 (1963).

23A. Chakravorty, R. H. Holm, Inorgi Chem. , 1521 (1964);
A. Chakravorty, J. P. Fennessey, R. H. 01m, Inorg. Chem.,
A. 26 (1965).

24R. J. Day, C. N. Reilley, Anal. Chem.,’36, 1073 (1964).

25R. J. Kula, D. T. Sawyer, s. 1. Chan, C. M. Finley, J. Am.
Chem. Soc., 85, 2930 (1963).

26Y. Saito, K. Natatusa, M. Skiro, H. Kuroya, Bull. Chem.

Soc. Japan, 30. 795 (1957)-
27K. Natatusa, Bull. Chem. Soc. Japan, 35, 832 (1962).

28Y. Saito, H. Iwaski, H. Ota, Bull. Chem. Soc. Ja apw ,36,

1543 (1963)

29F. P. Dwyer, A. M. Sargeson, L. B. James, J. Am. Chem. Soc. ,
86, 590 (1964).

30 F. P. Dwyer, T. E. McDermott, A. M. Sargeson, J. Am. Chem.
Soc., 85. 2913 (1963)

31T. E. McDermott, A. M. Sargeson, Australian J. Chem., 16,
334 (1963) "’

32E. J. Curey, J. C. Bailer, J. Am. Chem. Soc., 84, 2620 (1959).

33J. R. Gollo 1y, . J. Hawkins, J. K. Beattie, Inorg. Chem.,
10. 1732 %l97l)-
W

34

L. R. Froebe, B. E. Douglas, Inorg. Chem. , 9, 1513 (1970).

35L (R. Beattie, H. Elsbernd, J. Am. Chem. Soc., 92,1946
1970

36T. G. Appleton, J. R. Hall, C. J. Hawkins, Inorg. Chem., 9,
1299 (1970) ”V

37J. L. Sudmeier, G. L. Blackmer, J. Am. Chem. Soc., 92,
5238 (1970)

38H. L. Smith, B. E. Douglas, J. Am. Chem;_§oc., 86, 3885 (1964);
Inorg. Chem. , 5, 784 (1966).

39A. J. McCaffery, S. F. Mason, B. J. Norman, Chem. Commun. ,
49 (1965)

37

40A. J. McCaffery, S. F. Mason, B. J. Norman, A. M. Sargeson,

J. Chem. Soc., 29, 1304 (1968).

”1L. E. Erickson, J. w. McDonald, J. K. Howie, R. P. Clow,
J. Am. Chem. Soc., 22, 6371 (1968).

#20. E. Looney, W. D. Phillips, E. L. Rielly, J. Am. Chem. Soc.,
32. (1957 -

43Specifica11y, programs such as LOCOAN III, a NMR least-
squares fitting program by S.Caste11ano and A. A. Bothner—
by, J. Chem. Phys., 41, 8363 (1964). NMRIT, A/NMR energy
level program by J. D. Swalen and C. A. Reiley, J. Chem.
Phys., 37, 21 (1962); DNMR3, a dynamic NMR 1east-—squares
fitting program, by G. Binsch, J. Am. Chem. Soc., 91,1304
(1969). All are available from the Quantum Chemistry Program
Exchange, University of Indiana, Bloomingdale, Indiana.
uuAlso, many more such programs have been compiled in "Computer
Programs for Chemistry,” D. F. Detar, ed., W. A. Benjamin,
New York, 1968.

“5A8 an example, a Control Data Corporation 6500 SERIES computer
with a normal outboard eguipment configuration and instruc-
tion set can do about 10 operations per minute, which is
rapid.

“6B. M. Fung, Irene H. Wang, Inorg. Chem.,;fi, 1867 (1969).

u7J. K. Beattie, L. H. Novak, J. Am. Chem. SOC‘!’22! 620 (1972).

“8D. A. Buckingham, I. E. Maxwell, A. M. Sargeson, and H. C.
Freeman, Inorg. Chem;, 9, 1291 (1970).

498. S. Eaton, J. R. Hutcheson, R. H. Holm, and E. L. Muttertes,
J. Am. Chem.;§oc., 94, 6411 (1972).
50The work of Sudeimer (37), et. al., showed that vincinal
coupling constants 2J12, 13, J3“ obey Karplus equations

of the form J=Acos%, 9 the dihedral angle A=Al, 1+0O 90°

A=A2 if 9094 180° and Al/A2=4/3.5.
510n the order of lOBSec"l for an idealized exchange rate-
S. T. Spees, Private communication.

528. T. Spees, and D. L. Cox, unpublished theoretical research
data, July 1972.

53Abstracted in part from J. L. Sudmeier, G. L. Blackmer,
C. H. Brandley, and F. A. L. Anet, J. Am. 4Qhem. Soc., 94,
760 (1972). Ref 37

38

5”A. Allerhard, H. S. Guterosky, J. Jones, and R. A. Meinzer,

J. Am. Chem. Soc., 58, 3185 (1966).
55S. T. Spees, Jr., Private communication, August 1973.

56R. C. Henney, H. F. Hotzclaw, R. C. Larson, Inorg. Chem.,
5. 940 (1966).
F

57It should be noted that for Co(en)33+ the TC is greater, the
smaller the T, due to quadrapole relaxation, i.e., T2 resolu-
tion is not constant over a broad temperature range.

58J. L. Sudmeier, G. L. Backmer, C. H. Bradley, F. A. L. Anet,
J. Am. Chem. Soc., 24, 757 (1972).

59H. S. Gutowsky, D. W. McCall, C. P. Slichter, J. Chem. Phys.,
_21, 279 (1953); H. S. Gutowsky, C. H. Holm, J. Chem: Phys.,
25, 1228 (1956).
N

69E. L. Hahn, D. E. Maxwell, Phys. Revu, 88’ 1070 (1952).

61H. M. McConnell, J. Chem. Phy§;,’§§, 430 (1958).
62

F. Block, Phys. Rev., 29 460 (1946).

63M. Saunders, TetrahedrongLetters, 1966 (1963).

6“H. S. Gutowsky, R. L. Vold, E. J. Well, J. Chem. Phys., 43,
4107 (1965) 'V'

65A. Allerhand, E. Thiele, J. Chem. Phys., 45, 902 (1966).

66T. D. Alger, H. S. Gutowsky, R. L. Vold, J. Chem. Ph xs., 47,

3130 (1967)
67R. A. Sack, Mol. Phys.,’1, 163 (1958).
68F. W. Anderson, J. Phys. Soc. Japan,’2’ 316 (1954).
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70R. Kubo, J. Phys. Soc. Japan, 9, 935 (1954), Nuoro Cimento,
Suppl., 6, 10638(1951)

71R. K. Wanesness, F. Bloch, Phys. Rev.,’89, 728 (1956).
72F. Bloch, Phys. Rev., 102, 104 (1956); 105, 1206 (1957).
73J. I. Kaplan,“J. Chem. Phys., 28, 278 (1958); 29, 462 (1958).

39

748. Alexander, J. Chem. Phys., 37, 967 (1962): 38, 1787 (1963);
N N

no, 2741 (1964).

750. S. Johnson, J. Chem. Phys., 41, 3277 (1964).
76J. E. Dye, Department of Chemistry, Michigan State University,
Private communication, February 1974.

77Obviously in any rigorous and formal solution to this problem
these effects must be included in the computational solution.
However, for these effects to be able to be determined by
matching experimental and computational spectra, a very high
resolution of experimental Spectra would be needed. Currently
such resolution is not accurately possible. Further, the
contributions of the quadrapole and spin terms of Co-59 in
this would not be very great in relation to the other
combined terms.

788. T.4Spees, unpublished research data, Communicated January

197 .

APPENDIX

40

41

Appendix I. Table of computed results of Co(en)33+
AA'BB' system

Graph 11. Co(en)33+ ion PMR data, signal width vs.
temperature, at 60 MHZ

Graph III. Co(en)33+ ion PMR data, in D20, signal
width vs. temperature of CH2 protons

Graph IV. Co(en)33+ ion in D20, PMR data, at 60,
100MHz, signal width vs. temperature

Appendix II. Representative computed spectrum of Co(en)33+

at 60 MHZ, in D20

Appendix III. Tables of Co(en)33+ ion solvent system studies

Appendix IV. Program listings

42

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

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AH mm mm. 0.0m o.o s.s m.NH- m.n m.o o.mm N.mH 9mmw N.mH
m :s. 0.0m, o.oa m.n N.ma- .s n.m o.mm H.ma o.mm H.ma
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43

‘7'
/~=> /
123:1“

Temperature (103/T)

TRIS(ETHYLENEDIAMINE) COBALT(III)ION PMR DATA RESU
SIGNAI.WIDTH AT HALF HEIGHT vs. TEMPERATURE 960 MH

Source: Spees

8

QTS

12/73

60

g-
0»

Width at Half Height (CPS)

N
O

44

28

24

20

18

14
12

10

only 0
60 MHz

2.8 3.0 3.2 3.4
Temperature (103/T)

COBALT-59: TRIS(ETHYEENEDIAMINE) COBALT(III)ION in.D20
PMR DATA4WIDTH OF PROTON SIGNAL AT HAEF HEIGHT vs. TEMPERATURE

3.6 3.8

Source: Spees

12/ 73

 

 

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45

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0.0 0.0 0.0 . 0.0 0.0

 

Appendix II

Representative Computed PMR

3+
Spectrums of Co(NH2CHZCH2NH2)3

46

EYH’

 

L1 4
I ‘1
FIGURE 1 3+ Z
Calculated PMR Spectrum of Co(en)3 at 60 MH
Set 1 Set 2 T2 = 1.0
W(l) 20. 34. J(l,2) ‘~'~ 9.9
W(Z) 34. 18. J(l,3) = 4.3
W(3) 20. 34. J(l,4) 1' -l3.5
W(4) 34. 18. J(3,4) = 4-5
1 .79 .21 , k 2 50.0
(W/2) : 38.

47

<§H‘*

 

I L__|
1 1
FIGURE 2 3+
Calculated PMR Spectrum of Co(en)3 at 60 MHZ
”AB = 16.0 (W/2) == 37
T2 = 1.0
k = 60.0
A = .79
J(1.2) = 9.9
J(l,3) = 4.
J(1,Ll') : '1305 [+8
J(3.4) = 4-5

FIGURE 3
Calculated PMR

AGAB
J(l.2)

C...
A
H
V
II II II II II

 

Spectrum of Co(en)33+ at 60 MHZ
= 14.0

 

49

 

 

15Ha

 

L J
U I
FIGURE 4 +
Calculated PMR Spectrum of Co(en)33 at 60 MHz
AGAB = 14.0
J12 = 9'9
J14 : -1305
J3“ = [4'05
T2 = 1.0
k ”= 50.
A = .79
(W/Z) = 29-5

50

 

L 1.4
r— I
FIGURE 5 ‘3+ z
Calculated PMR Spectrum of Co(en)3 at 60 MH
AGAB = 14.0
J(l.2) = 9-9
J(1.3) = ”-3
J(l,4) = ~13.5
J(3.4) = 4-5
T2 = 1.0
k = 102 103
A = -79
(W/2) = 37.5 50.0

51

APPENDIX III

Cobalt Ion Solvent System Studies

52

:m

 

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Table 2

Band widths at half height (VI/2) for Co(en)
in various D20 salt solutions.3

Complex

Co(en)3 Cl

3

54

Salt Solution

D20

0.1M
0.5M
1.8M
0.1M
0.5M
1.8M
0.1M
0.5M
1.9M
1.1M

K3P0u
K3P04
K3P0u
NaZSeou
NaZSeOu
NaZSeou
NaZSeO3
NaZSeO3
Na Se03

2
NaCl

WZZ CH2

17
8
8

13

14

10

13

ll
8

11

16

3 Cl

3

 

55

Table 3 Band widths at half height (W/2) of 0o(en)3 (010”)3

in D20 solution at differing temperatures.3u

Temperature, 0C W52 CH2 (8,ppm)
4 7(2.80)
21 13(2.84)
39 19(2.84)
64 25(2.84)
82 27(2.84)

Table 4 Band widths at half heights (W/2) of Co(en)3 013

in 60% by weight H2804 in D20 (~6-9fi by weight
complex).55

Temperature ‘WZZ CH2 W12 NH2 app
39 14.5 17.0 481

12 12.5 16.5 496

-1 l .0 19.0 506

-45 31.5 48.0 538
-59 39-5 70-5 548

APPENDIX IV

Program Listings

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