Alternate Synthetic Pathway Leading to Isolation of a Dinuclear Single-Molecule Magnet

Article abstract of DOI:10.1002/ejic.201800327

Using the Schiff-base ligand 1,5-bis(salicylidene)carbohydrazide (H₃bsc) a unique dinuclear dysprosium(III) compound, [Dy₂(μ-OH)(bsc) (NO₃)₂(DMF)₃(H₂O)]·THF·2DMF (1·THF·2DMF), has been synt

Full text of DOI:10.1002/ejic.201800327

A Journal of
Accepted Article
Title: Alternate Synthetic Pathway Leading to Isolation of Dinuclear
Single-Molecule Magnet
Authors: Jun-Yu Wei, Ting-Jung Hsu, Chia-Wei Wang, Che-Jung Kuo,
and Po-Heng Lin
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To be cited as: Eur. J. Inorg. Chem. 10.1002/ejic.201800327
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10.1002/ejic.201800327
European Journal of Inorganic Chemistry
COMMUNICATION
Alternate Synthetic Pathway Leading to Isolation of Dinuclear
Single-Molecule Magnet
Jun-Yu Wei,[a] Ting-Jung Hsu,[a] Chia-Wei Wang,[a] Che-Jung Kuo,[a] and Po-Heng Lin*[a]
Abstract:
Bis(salicylidene)carbohydrazide (H3bsc), an unique dinuclear
dysprosium(III) compound, [Dy2(μ-OH)(bsc)
(NO3)2(DMF)3(H2O)]·THF·2DMF (1·THF·2DMF), has been
Using
the
Schiff-base
ligand,
1,5-
the dinuclear unit, 1,5-Bis(salicylidene)carbohydrazide (H3bsc)
was designed without the methoxyl group, which leads to only
two potential coordination sites. An unexpected Dy6 single-
molecule
magnet,
[Dy6(μ3-
synthesized. The structural and magnetic properties are fully studied
and single-molecule magnetic behaviour with an energy barrier (Ueff
= 123 K) has been observed.
O)(bsc)3(CO3)3(MeOH)14(H2O)](OH)Cl3·2MeOH·2H2O
(B·2MeOH·2H2O),13 was synthesized, which exhibits slow
relaxation of the magnetisation under zero applied dc field with a
value of Ueff/kB = 101.9 K. The structure was assembled
thereafter by three dinuclear units in a triangular arrangement,
Single-Molecule Magnets (SMMs) observing superparamagnet-
like behaviour generally result from the presence of large spin
ground state (ST) and Ising-type magnetoanisotropy (D).1 In this
decade, pure lanthanide SMMs, in particular DyIII, have been
intensively studied due to the large spin-orbit coupling, which
increases the D value for the complex resulting in higher energy
barriers.2 The multinuclear complexes have been synthesized
with nuclearity of the SMMs based on dysprosium(III) ranging
from mononuclear to a Dy36 cluster.3 The high energy barrier of
SMM might be governed by the interplay between the ligand
field effect, the symmetry of metal ions and the hyperfine
coupling and magnetic interaction.4 In order to explore the real
physical origin of this behaviour, the simplicity of the dinuclear
lanthanide units has been applied for further evaluation.
Complexes with different bridging motifs have been investigated
due to the ability to probe magnetic interactions between
lanthanide ions, such as N23−-bridged Tb2 complex,5 phenoxide
bridged Dy2 complex,6 fluoro-bridged Dy2 complex7 and sulfur-
bridged organometallic Dy2 complexes.8 Moreover, dinuclear
complexes with two different local geometries of DyIII ions have
also been synthesized. Asymmetric dinuclear molecules with
two-step relaxation process of SMM properties are good
examples for understanding the effect of D values.9,4e On the
other hand, the presence of quantum tunneling of magnetization
(QTM) negatively affects the magnetic bistability, which induces
a reduction in the effective anisotropic barrier.10 In pure
lanthanide based SMM systems, the weak super-exchange
interactions between the lanthanide ions can also be significant
enough to suppress QTM.11 With the aim to further understand
lanthanide SMM system, more dinuclear complexes are
necessary to be synthesized.
2-
which were linked through CO3 bridges. With this in mind, we
have focused our attention on synthesizing dinuclear or
trinuclear units with the same ligand, H3bsc, whose magnetic
property details may be further explored by simplifying the
magnetic interaction or anisotropic axes alignments.
Scheme
methoxybenzylidene)carbonohydrazide
Bis(salicylidene)carbohydrazide (H3bsc, right).
1.
Coordination
modes
of
1,5-Bis(2-hydroxy-3-
left) and 1,5-
(H2hmc,
Dimethylformamide (DMF) was selected for the syntheses, since
the coordination of the lanthanide ions in a polar aprotic solvent,
such as DMSO or DMF, is a prevalent phenomenon that has
been applied for crystallization due to its role as both terminal
ligands and co-solvent.14 Herein, the DyIII unit was successfully
2
isolated by adding DMF in the solvent system. The details of
magnetic properties have been studied, which show dinuclear
complex exhibiting SMM properties with a value of Ueff/kB = 123
K.
In our previous research, nonanuclear complex, [Dy9(μ3-O)4(μ-
OH)6(hmc)4(NO3)4(DMF)4](OH)·H2O·THF·DMF
(A·H2O·THF·DMF), was synthesized by 1,5-Bis(2-hydroxy-3-
methoxybenzylidene)carbonohydrazide (H2hmc), which has four
potential coordination sites (Scheme 1, left). 12 In order to isolate
[a]
Jun-Yu Wei, Ting-Jung Hsu, Chia-Wei Wang, Che-Jung Kuo, Prof.
Po-Heng Lin
Department of Chemistry, National Chung Hsing University,
250 Kuo Kuang Rd., Taichung 402, Taiwan
E-mail: poheng@dragon.nchu.edu.tw
Figure 1. Molecular structure of complex 1. Color code: Dy (yellow), O (red), N
(blue), C(gray) and selected H(black). H atoms were omitted for clarity. The
reaction conditions were described at the bottom.
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the document.
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European Journal of Inorganic Chemistry
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To a solution of Dy(NO3)3·5H2O (0.50 mmol) in THF (15 ml) was
added a solution of H3bsc (0.25 mmol) and ethylenediamine
(EDA) (0.5 mmol) in DMF/THF (7 and 8 ml, respectively).
Different dysprosium salts have been applied in the reactions,
since no crystal of dinuclear complex was obtained by using
DyCl3·6H2O which we selected before. The resulting pale yellow
solution gave well-formed pale yellow crystals in 64% yield. The
structure of the dinuclear complex, [Dy2(μ-OH)(bsc)
(NO3)2(DMF)3(H2O)]·THF·2DMF (1·THF·2DMF), crystallized in
the monoclinic P21/n space group (Figure 1). Since CO32- as a
linker for dinuclear units was formed by strong base, EDA was
selected as a weaker base. DMF was chose as a terminal
solvent molecule to fill the coordination sites as well as to
prevent the formation of a large metal cluster. Selected bond
distances of two DyIII ions were shown in Table S1.
Moreover, since the positions of terminal H2O and DMF are very
close (Dy1-O6 and Dy2-O11 bonds of 2.358(4) Å and 2.360(4) Å
as well as O6-Dy1-Dy2
and O11-Dy2-Dy1 angles of
113.09(11)° and 110.13(11)°, respectively) and the bond
distance differences of ligand as we mentioned above were
insignificant, the bond distances and angles around the Dy
center are also very close result in both Dy centers have similar
coordination geometries. (Figure 2) The coordination geometries
of Dy1 and Dy2 were both triangular dodecahedron with
significant differences as determine by SHAPE 2.1. (Table S2)
which could lead to different relaxations systems we mentioned
below.
The pentadentate ligand coordinates to the Dy centers in the
dinuclear unit by two designed coordination pockets via three O
atoms (O2, O3 and O4) and two N atoms (N1 and N4). Two
crystallographically independent DyIII ions are bridged by the
enol group of the ligands and one μ-OH- with a Dy1-O3-Dy2
and Dy1-O1-Dy2 angle of 110.62(15)° and 115.96(16)°,
respectively. The Dy-Dy distance is 3.8422(4)Å. Both DyIII ions
are eight coordinate and the remaining four coordination sites of
each lanthanide ion are filled by one nitrate anion and two
solvent molecules (O5 of the DMF molecule and O6 of the H2O
for Dy1 as well as O10 and O11 of two DMF molecules for Dy2).
Charge balance considerations for the molecule indicate that the
ligand must have three negative charges resulting from the
ligand being in the enol-form of two deprotonated phenoxides
(O2 and O4) and one deprotonated enol (O3). This is surprising
Figure 2. Top: The coordination polyhedra of two octa-coordinated DyIII ions.
Bottom: The coordination polyhedral with molecular structure.
that complex
1 with enol form was different with the
carbohydrazide derived Schiff base complexes A and B which
were found to exhibit the keto form. The comparison of selected
bond distances of ligand for complexes 1, A and B are
presented in Scheme 2. Although the difference of bond
distances of C2-N2 (1.324(7) Å) and C2-N3 (1.364(7) Å) in
complex 1 are relatively insignificant, the difference (less than
0.04 Å) between double and single bonds of carbohydrazide
derived ligands in 3d or 4f metal clusters were observed.15
Moreover, difference of the central C-O distances of three
complexes in Scheme 2, dC48-O8 = 1.260(15) Å, dC7-O3 = 1.276(11)
Å, and dC2-O3 = 1.290(7) Å for complexes B, A and 1,
respectively, are also not very obvious. However, we can
confirm the enol form of bsc3- with the ligands have been
reported in its enol form with a dC-O ≤ 1.29 Å. 15a,16
Figure 3. Temperature dependence of the χT product of complexes 1 at 1000
Oe. Inset: M vs. HT-1 plot at indicated temperatures for complex 1.
Direct current (dc) magnetic measurements were performed
between 1.8 and 300 K, with an applied dc field of 1000 Oe. The
temperature dependence of the χT product can be observed in
Figure 3. At room temperature the observed χT value was 28.65
cm3 K mol-1 under 1000 Oe applied dc field. These values are
consistent with the theoretical value of 28.34 cm3 K mol-1 for two
non-interacting DyIII ions (6H15/2, S = 5/2, L = 5, g = 4/3, χT =
14.17 cm3 K mol-1). The χT product displays a gradual decrease
Scheme 2. Top: Different deprotonated forms of keto and enol forms of H3bsc;
Bottom: The selected bond distances of core structures of complexes 1 (right),
A (middle) and B (left) in Å .
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with temperature, until ~100 K where a more dramatic decrease
is observed to 24.53 cm3 K mol-1 at 1.8 K, under 1000 Oe. The
drop of χT at low temperature could be related to
antiferromagnetic interactions, inherent magnetic anisotropy
from DyIII ions, the Stark levels depopulation and/or the
occurrence of SMM behavior.
within this complex that the QTM is probably supressed by the
exchange interaction between the DyIII.
Figure 5. Dinuclear core structures of complex 1 (top) and B (bottom) showing
the direction of the anisotropy axes for all DyIII ions. Atom labels are the same
as cif files. Axes modelled using Magellan magnetic software.
Figure 4. Temperature dependence of the out-of-phase (χ”) susceptibility of
Complex 1 without applied dc field.
In order to evaluate the anisotropies of complex 1, the alignment
of the anisotropy axes was determined using Magellan magnetic
software.18 Electrostatic modeling of the lowest lying Kramers
doublets for each DyIII ion reveals that the anisotropy axes of
DyIII ions (Figure 5, top) are close to the Dy-O(phenoxide) bonds
(The angle between the anisotropy axis of Dy2 and Dy2-O4 is
3.09∘; the angle between the anisotropy axis of Dy1 and Dy1-
O2 is 3.11∘). The broad peaks have been attributed to the
anisotropic character of the coordination sphere around DyIII ions
or different orientations of the anisotropic axes within
multinuclear complexes.19 Since the coordination environments
of two DyIII ions are very similar, the possibility of the broad
peaks observed in figure S4 may result from the non-parallel
direction of the anisotropy axes of both DyIII ions. Moreover,
comparing with the calculated anisotropic axes of complex B
was shown in figure 5, bottom and S7. The directions of
anisotropic axes between complexes 1 and B are slightly
different due to the differences of the charge of the ligand and
the bridging molecules.
In conclusion, we successfully synthesized the dinuclear Dy unit
of Dy6 single-molecule magnet by utilised DMF as a terminal
solvent molecule which also exhibits SMM behavior with an
anisotropic barrier of Ueff = 123 K (τ0 = 7.6 x 10-7 s). Since the
coordination environments of two DyIII ions are similar which was
not changed a lot by enol form of ligand, the non-parallel
anisotropic axes directions have been also indicated the broad
peak in high frequency are mainly result from anisotropic axes
directions. This example demonstrated that the symmetry unit of
multinuclear cluster may be also observed SMM properties
which offered more information for understanding how to
synthesize new SMMs with higher anisotropic barriers towards
beneficial future applications.
Isotherm magnetisation data was collected between 1.8 and 8 K
(Figure S1). The M vs. H plot displays a rapid increase in the
magnetisation at low magnetic fields, after which a gradual
plateau beginning at 1 T forms. The M vs. HT-1 data (Figure 3,
inset) also displays that isotemperature lines to not overlay on a
single master curve, thus further confirming the presence of non-
negligible magnetic anisotropy and/or low-lying excited states.
In order to assess the relaxation dynamics of the complex,
alternating current (ac) susceptibility measurements were
performed with an ac field of 3.5 Oe oscillating at frequencies up
to 10000 Hz. We have measured the frequency-dependence of
the in-phase (χ′) and out-of-phase (χ″) magnetic susceptibilities
under zero applied dc fields, where clear peaks are seen to shift
to lower frequencies as the temperature is decreased, indicative
of slow magnetic relaxation (Figure 4 and S2) The effective
energy barrier and relaxation time were obtained through fitting
the data of high temperature regime using the Arrhenius
equation (τ = τ0exp(Ueff/kT), which elicited a value of Ueff = 123 K
(τ0 = 7.60*10-7 s), as can be seen in Figure S3. The presence of
a full broad peak can be observed with a maximum located
around 25 K at 1000 Hz without applied dc field which may
result from two relaxation systems due to the different
geometries and/or the direction of anisotropic axes on two DyIII
ions. (Figure S4) Fitting the Cole–Cole plots (Figure S5) with a
Debye model yields large values of the α parameter ranging
from 0.18 to 0.30 (Table S3), confirming the wide distribution of
the relaxations.
Since the quantum tunneling of the magnetization (QTM) that
can occur was suppressed by applying optimum dc fields, the
find-field experiments were also performed.17 (Figure S6) The
addition of a static field was found to have only a little effect on
the relaxation dynamics of 1, and thus we may conclude that
zero field quantum tunneling of the magnetization is not efficient
Acknowledgements
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This work was supported by National Chung Hsing Uni-versity
and the financial support from the Ministry of Science and
Technology, Taiwan (MOST 105-2113-M-005-011). We thank Dr.
Ming-Hsi Chiang in Academia Sinica and Prof. Hui-Lien Tsai in
National Cheng Kung University for assistance with the dc and
ac magnetic measurements, respectively.
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Keywords: Single-Molecule Magnets
• Dinuclear Unit •
Dysprosium Complex
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Using the Schiff-base ligand, 1,5-
Bis(salicylidene)carbohydrazide
Jun-Yu Wei, Ting-Jung Hsu, Chia-
Wei Wang, Che-Jung Kuo, Po-Heng
Lin*
(H3bsc),
a
unique
dinuclear
dysprosium(III) compounds, [Dy2(-
OH)(bsc)(NO3)2(DMF)3(H2O)] · THF ·
2DMF, has been synthesized. The
structural and magnetic properties
are fully studied and single-molecule
magnetic behaviour with an energy
barrier has been observed.
Page No. – Page No.
Alternate Synthetic Pathway
Leading to Isolation of Dinuclear
Single-Molecule Magnet
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