Single-Molecule Magnetism in Dy2 Cluster Based on a Schiff Base Ligand

Article abstract of DOI:10.1002/zaac.202000089

Two dinuclear Ln^III-based clusters, namely [Dy₂L₂(NO₃)₂(DME)₄] (1) and [Gd₂L₂(NO₃)₂(DME)₄] (2) [H₂L = (E)-2-((2-hydroxybenz

Full text of DOI:10.1002/zaac.202000089

Journal of Inorganic and General Chemistry
DOI: 10.1002/zaac.202000089
ARTICLE
Zeitschrift für anorganische und allgemeine Chemie
Single-Molecule Magnetism in Dy2 Cluster Based on a
Schiff Base Ligand
Yingying Wang,[a] Zhuangdong Yuan,[a] Yunjie Guo,[a] Xuxiao Ma,[a] Zitong Meng,[a] Jingquan Sha,[a] and
Haifeng Zhang*[a]
Abstract.
Two
dinuclear
LnIII-based
clusters,
namely Dy1A) and 3.860 Å (Gd1–Gd1A). Two Dy1–O–Dy1A and Gd1–O–
[Dy2L2(NO3)2(DME)4] (1) and [Gd2L2(NO3)2(DME)4] (2) [H2L = (E)- Gd1A angles are 109.4° and 109.8°, respectively. Magnetic studies
2-((2-hydroxybenzylidene)amino)phenol] were obtained under hydro-
thermal condition. Two LnIII ions are bridged by two phenolic hy-
reveal a weak antiferromagnetic interaction between Gd ions in com-
plex 2, and single-molecule magnet behavior for 1 with Ueff = 49.9 K
droxyl oxygen atoms, and the distances of them are 3.829 Å (Dy1– and τ0 = 1.54ϫ10–6 s.
In this work, we have used O-hydroxybenzaldehyde Schiff-
Introduction
base (E)-2-((2-hydroxy- benzylidene)amino)phenol (H2L) in
combination with N,N-dimethylacetamide (DME) for the syn-
thesis of two dinuclear complexes, and the Dy2 complex exhib-
ited SMM behavior. Herein, we present the syntheses, crystal
structures and magnetic properties of these two complexes.
Generally speaking, the single molecule magnet is com-
posed of independent single molecules, which can maintain the
magnetization intensity for a long time at low temperature and
without external magnetic field. Its appearance makes it pos-
sible to develop memory devices with nanometer size magnetic
complexes as basic units.[1,2] In recent years, there is a growing
interest in constructing novel SMMs with the paramagnetic
lanthanide ions (especially DyIII, HoIII, ErIII, and TbIII). Be-
cause the large anisotropy barrier is crucial for SMM, lantha-
nide ions with their advantages of large ground-state spin and
significant intrinsic anisotropy can meet this demand.[3] Many
lanthanide SMMs with varying ranges of nuclearities have
been prepared.[4–10] Among all the lanthanide-based SMMs,
[Ln2]SMMs have attracted significant attention of the chemists
and physicists in the world.[11–40] There are many reasons for
this, for example, (i) compared with other polynuclear clusters,
the synthesis of [Ln2] is easier to control; (ii) the structure-
property relationships of the dinuclear systems could be easily
investigated by modifying the functional groups of the ligands;
(iii) in studying the magnetic interaction between two lantha-
nide atoms, they represent the simplest structural units; and
(iv) it is relatively convenient to determine the possible orien-
tation of anisotropy in the dinuclear system. We believe that
Ln2 is the most basic structure in explaining the nature of sin-
gle molecule magnets (such as the relationship between single
ion relaxation and molecular entity relaxation; the influence of
magnetic interaction on magnetization relaxation, the possible
orientation of anisotropy).
Results and Discussion
Description of the Structures 1 and 2
The molecular structures of 1 are depicted in Figure 1. Sin-
gle crystal X-ray diffraction reveals that complexes 1 and 2
are isomorphous, herein only the structure of representative
complex 1 will be described in detail. Complex 1 is in the
monoclinic space group P21/n. The asymmetric unit consists
–
of one DyIII ion, one L2– ligand one NO3 and two DME li-
gands. The Dy1 atom is coordinated by three phenolate oxygen
atoms from two L2– ligands and one nitrogen atoms from one
L2– ligand, two oxygen atoms from two DME ligands, and two
–
oxygen atoms from NO3 . The Dy1 and Dy1A are bridged by
two μ-phenolate oxygen atoms(O2), and the distance of them
is 3.829 Å. Two Dy1–O–Dy1A angles are both 109.4(1)° (Fig-
ure 1a). The L2– anions is in μ2:η2:η1:η1 mode as shown in
Figure 1. The eight-coordinated DyIII center has an O7N
sphere and displays a distorted triangular dodecahedron ar-
rangement. The bond lengths of Dy1–O1, Dy1–O2, Dy1–O2A,
Dy1–O3, Dy1–O4, Dy1–O6 and Dy1–O7 are 2.197(2),
2.367(2), 2.323(2), 2.599(2), 2.443(2), 2.377(2) and 2.316(2) Å,
respectively. The length of Dy–N bond is found to be 2.495(2) Å.
The program SHAPE 2.1 was used to analyze the exact ge-
ometry of the octa-coordinated dysprosium ion,[43] and close
analysis of the selected resulting data are listed in Table S1
(Supporting Information). The triangular dodecahedron (D2d)
geometry for 1 with a minimum CshM value of 5.49 was deter-
mined, which indicates the coordination environment of Dy1
ion is close to a distorted triangular dodecahedron configura-
tion.
* H. Zhang
E-Mail: zhhf1980@163.com
[a] Department of Chemistry and Chemical Engineering
Key Laboratory of Inorganic Chemistry in Universities of Shan-
dong
Jining University
Qufu, 273155, P. R. China
Supporting information for this article is available on the WWW
under http://dx.doi.org/10.1002/zaac.202000089 or from the au-
thor.
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rapidly below 10 K. This phenomenon indicates weak antifer-
romagnetic interactions between two GdIII ions.
Figure 2. Temperature dependence of the χMT product in the range of
1.8–300 K at 1.0 kOe for 1 and 2. The solid red line of 2 correspond
to the best fits in the range of 1.8–300 K.
In order to obtain more insight into the magnetic coupling
between the GdIII ions, we fitted the magnetic data of 2 with
the isotropic spin Hamiltonian H = –2JSGd1SGd1A. The mag-
netic data in the temperature range of 1.8–300 K can be well
fitted and the best-fitting parameters for 2 are J = –0.043 cm–1,
g = 2.03. The negative J value confirms the weak antiferro-
magnetic interactions between two GdIII centers in 2.
The field-dependent magnetization measurements per-
formed for 1 and 2 at fields of 0–70 kOe under 2 K are shown
in Figure 3. For 1, the magnetization increases very rapidly at
low magnetic fields, then a slow linear increase in high-field
region without saturation even at 70 kOe. The magnetization
value at 70 kOe is 10.50 Nβ, which is lower than the theoreti-
cal saturation value of 20.00 Nβ. This behavior may be caused
by the significant magnetic anisotropy and/or possibly low-
lying excited states in all systems.[44–46] For 2, the magnetiza-
tion value at 70 kOe is 13.79 Nβ, which is close to the ex-
pected theoretical value of 14.00 Nβ for two GdIII ions.
Figure 1. (a) The molecular structure of 1. (b) Coordination polyhe-
dron of the DyIII ion in 1.
Although complex 1 joins a big family of Dy2 clus-
ters,[11–40] none of the complexes crystallized from the DME
solution, and the DME oxygen atom also serves as a coordina-
tion site in 1. These features indicate the improvement of the
synthesis method and the structural novelty of complexes 1
and 2.
Magnetic Studies
Direct current (dc) magnetic properties were investigated on
polycrystalline samples for clusters 1 and 2 in the 1.8–300 K
range under an applied magnetic field of 1000 Oe. As shown
in Figure 2, at room temperature, the χMT value of 1 is
25.97 cm3 mol–1 K, which is slightly lower than the theoretical
value of 28.34 cm3·mol–1·K for non-interacting spins of two
DyIII ions (6H15/2, S = 5/2, L = 5, g = 4/3). Upon cooling, the
value of χMT decreases gradually and then more sharply
reaches a maximum value of 6.82 cm3 mol–1 K at 1.8 K. This
magnetic behavior indicates that weak antiferromagnetic ex-
change interaction may exist. For complex 2, the χMT value is
16.12 cm3·mol–1·K at room temperature, which is closed to the
value expected for two magnetically isolated GdIII (8S7/2, S =
7/2, L = 0, g = 2) of 15.75 cm3·mol–1·K. With the decrease of
Figure 3. Field dependence of the magnetization of 1 and 2 obtained
temperature, the χMT values decrease gradually and then at 2 K.
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The dynamic magnetic properties of 1 were probed to fur-
ther understand its magnetism. The temperature dependence of
alternating current (ac) susceptibilities for 1 was performed in
the temperature range of 22–2 K at the indicated frequencies
of 1, 10, 32, 100, 320, 666, 780, and 1000 Hz under an applied
zero dc field. As shown in Figure 4, the ac magnetic suscep-
tibilities of 1 display the temperature and frequency dependent
characters in both the in-phase (χMЈ) and out-of-phase (χMЈЈ),
which are the typical features associated with the single mol-
ecule magnet behavior. Temperature dependence of 1 was also
confirmed by the frequency dependence of χMЈ and χMЈЈ in the
range 2–10 K (Figure 5). The peaks of the frequency-depend-
ent χMЈЈ susceptibilities shift to a broad range under a zero dc
field.
Figure 5. Frequency dependence of the in-phase [χMЈ, (a)] out-of-phase
[χMЈЈ, (b)] ac susceptibility under an applied zero Oe field for 1.
factors τ0 = 1.54ϫ10–6 s and the obtained τ0 value is consis-
tent with the expected for a SMM (10–6–10–11 s).[47]
Figure 4. Temperature dependence of the in-phase [χMЈ, (a)] out-of-phase
[χMЈЈ, (b)] ac susceptibility under an applied zero Oe field for 1.
The Cole-Cole plots of complex 1 show one semicircular
shape from 2 to 10 K (Figure 6), which confirms the presence
of one relaxation process. These plots are well fitted using a
generalized Debye Model. The obtained values of α are in the
range 0.004 to 0.16, indicating a moderate distribution of mag-
Figure 6. Cole-Cole plots measured at 2–10 K in zero-dc field; the
solid lines are the best fit to the experimental data.
At low temperature, lnτ vs. 1/T plots indicate that other re-
netic relaxation times, especially at low temperature. At high laxation pathways may exist. As processes including spin-
temperature, the relaxation time obeys the Arrhenius law: τ = lattice relaxation of Quantum Tunneling of the Magnetiza-
τ0 exp(Ueff/kBT) [Equation (1)] (Figure 7). The best fitting re- tion (QTM), Raman and Orbach are considered, The magnetic
–1
–1
sults give energy barriers Ueff = 49.9 K and pre-exponential data of 1 were fitted with equation: 1/τ = τQTM + CTn + τ0
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Synthesis of [Dy2L2(NO3)2(DME)4] (1): A mixture of H2L (0.0214 g,
0.1 mmol), Dy(NO3)3·6H2O (0.0456 g, 0.1 mmol), NaOH (0.0080 g,
0.2 mmol), EtOH (1.5 mL) and DME (0.5 mL) was sealed in a Pyrex-
tube (10 mL). The tube was heated for 72 h at 353 K. After cooling
to room temperature, yellow crystals of 1 were obtained in a yield of
36% (0.0218 g based on Dy). C42H54N8O14Dy2: calcd. C, 41.35; H,
4.46; N, 9.19%; found: C, 41.52; H, 4.38; N, 9.03%. IR (KBr, selected
data ): ν˜ = 1636 (s), 1612 (s), 1585 (m), 1481 (m), 1467 (s), 1450 (m),
1406 (w), 1384 (m), 1350 (w), 1310 (m), 1280 (m), 1262 (w), 1171
(w), 1147 (w), 1029 (w), 918 (w), 830 (w), 745 (m), 601 (w), 488 (w)
cm–1.
Synthesis of [Gd2L2(NO3)2(DME)4] (2): Complex 2 was prepared
using the same method as that of 1 except that Dy(NO3)3·6H2O was
replaced by Gd(NO3)3·6H2O. Yield: 29% (0.0175 g based on Gd).
C42H54N8O14Gd2: calcd. C, 41.71; H, 4.50; N, 9.27%; found: C, 41.81;
H, 4.42; N, 9.13%. IR (KBr, selected data ): ν˜ = 1633 (s), 1612 (s),
1581 (m), 1481 (m), 1466 (s), 1449 (m), 1407 (w), 1385 (m), 1349
(w), 1309 (m), 1279 (m), 1261 (w), 1171 (w), 1147 (w), 1029 (w),
918 (w), 829 (w), 745 (m), 600 (w), 487 (w) cm–1.
Figure 7. Relaxation time lnτ vs. T–1 plot for 1 under zero-dc field.
The blue solid lines represent data fits to Equation (1) and the red
solid lines represent data fits to Equation (2).
exp(–Ueff/kBT) [Equation (2)].[48,49] The best fit is in good
agreement with the data over the entire temperature range and
gives the parameters of Ueff = 56.5 K, τ0 = 2.11ϫ10–7 s, τQTM
= 1.59ϫ10–3 s, C = 0.75 s–1·K–4.56, n = 4.56.
Two Dy2 complexes, [Dy2(NO3)2(L)2(DMF)4] and [Dy2(L)-
2(NO3)2(MeOH)4] have been reported with the same li-
gand[50,51] but using different auxiliary ligands. To our sur-
prise, their magnetic properties are totally different indicating
that the structural change could lead to variation of the mag-
netic properties.
X-ray Diffraction Crystallography: Crystals suitable for X-ray struc-
ture analysis were carefully collected. Measurements were made on
Bruker Smart Apex II diffractometer with graphite-monochromated
Mo-Kα radiation (λ = 0.71073 Å) using the ω-2θ scan technique. Semi-
empircal multi-scan absorption corrections were applied by SADABS
and integration of diffraction profiles were applied by SAINT. The
crystal structures were solved by direct methods and refined by full-
matrix least-squares technique using the SHELXTL refinement pack-
age.[41,42] The crystallographic data for complexes 1 and 2 are listed
in Table 1. The selected bond lengths and angles are listed in Table 2.
Conclusions
Table 1. Crystal data and structure refinement for complexes 1 and 2.
In conclusion, we have successfully obtained two iso-
structural dinuclear lanthanide clusters using a Schiff-base li-
gand under solvothermal conditions. The dinuclear framework
is composed of two ligands which are doubly-deprotonated,
two chelated nitrate anions and four coordinated DME mol-
ecules. Both the metal centers are surrounded by NO7 environ-
ments in distorted triangular dodecahedron (D2d) arrangement
with a minimum CshM value of 5.49. The magnetic properties
of them are investigated, and cluster 1 displays slow magnetic
relaxation behavior with Ueff = 49.9 K, τ0 = 1.54ϫ10–6 s. This
work demonstrates the potential applications of the Schiff-base
ligands in the construction of SMMs.
1
2
Empirical formula
Formula weight
Crystal system
Space group
a /Å
b /Å
c /Å
α /°
β /°
C42H54N8O14Dy2
1219.94
monoclinic
P21/n
11.808(2)
14.180(2)
15.195(3)
90
107.561(3)
90
2425.7(7)
2
C42H54N8O14Gd2
1209.45
monoclinic
P21/n
11.765(2)
14.142(3)
15.196(3)
90
107.225(3)
90
2414.9(7)
2
γ /°
V /Å3
Z
Dc /g·cm–3
1.670
1.663
θ range for data collection 1.93 ~ 27.52
1.94 to 27.72
°
Experimental Section
μ /mm–1
3.127
2.793
Reflections collected /
unique
Rint reflections
Data / restraints / param-
eters
F(000)
Goodness-of-fit
Final R
14492/ 5511
14173 / 5495
General: H2L was prepared by mixing salicylaldehyde and 2-ami-
nophenol in 1:1 molar ratio in hot methanol. The reagents and chemi-
cals were obtained from Sinopharm Chemical Reagent Co., Ltd, China
and used as purchased without further purification. IR spectra were
recorded in the range 4000–400 cm–1 on a Nicolet 470 FT-IR spectro-
photometer. Powder XRD patterns were recorded on a Rigaku D/Max-
2500 diffractiometer at 40 kV and 100 Ma with a Cu-target tube and
a graphite monochromator. Elemental analyses for C, H and N were
carried out on a Perkin–Elmer 2400 analyzer. Magnetic susceptibility
data were collected on a Quantum Design MPMS-7 SQUID magne-
tometer.
0.0220
5511 / 0 / 355
0.0188
5495/1/355
1212.6
1.024
R1 = 0.0217, wR2
= 0.0478
R1 = 0.0290, wR2
= 0.0506
1205.4
1.030
R1 = 0.0208, wR2
= 0.0456
R1 = 0.0296, wR2
= 0.0495
R indices (all data)
Δρ(max, min) /e·Å–3
0.48 and –0.79
0.76 and –0.55
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Shandong Province Higher Educational Science and Technology Pro-
Table 2. Selected bond lengths /Å and angles /° for complexes 1 and 2.
gram (J12LD54), the Youths Science Foundation of Jining University
(no. 2017BSZX09), and the Talent Culturing Plan for Leading Disci-
plines of University in Shandong Province.
1
Bond
Bond
Dy1–O7
Dy1–O2
Dy1–O6
Dy1–O1
2.316(2)
2.367(2)
2.377(2)
2.197(2)
Dy1–O3
Dy1–N1
Dy1–O4
Dy1–O2#1
2.599(2)
2.495(2)
2.443(2)
2.323(2)
Keywords: Single molecule magnet; Schiff-base ligand; Lan-
thanides; Dinuclear clusters; Energy barriers
Angle
Angle
O2–Dy1–N1
O2#1–Dy1–O4
O2–Dy1–O4
O6–Dy1–O7
O1–Dy1–O7
O1–Dy1–O6
O3–Dy1–O7
O3–Dy1–O6
O3–Dy1–O1
N1–Dy1–O7
N1–Dy1–O6
N1–Dy1–O1
N1–Dy1–O3
O4–Dy1–O7
66.00(6)
142.07(6)
79.24(6)
72.18(8)
81.75(8)
143.33(7)
73.41(9)
113.72(8)
81.61(8)
138.02(8)
142.27(7)
73.54(7)
69.87(7)
92.01(8)
O4–Dy1–O6
O4–Dy1–O1
O4–Dy1–O3
O4–Dy1–N1
O2–Dy1–O7
O2#1–Dy1–O7
O2–Dy1–O6
O2#1–Dy1–O6
O2–Dy1–O1
O2#1–Dy1–O1
O2–Dy1–O3
O2#1–Dy1–O3
O2#1–Dy1–N1
76.43(7)
130.88(7)
50.33(7)
79.94(7)
152.97(7)
104.47(8)
80.89(6)
76.58(7)
123.20(7)
85.79(7)
117.05(7)
167.40(7)
106.89(6)
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O4–Gd1–N1
O1–Gd1–N1
O1–Gd1–O4
O3–Gd1–N1
O3–Gd1–O4
O3–Gd1–O1
O7–Gd1–N1
O7–Gd1–O4
O7–Gd1–O1
O7–Gd1–O3
O6–Gd1–N1
O6–Gd1–O4
O2–Gd1–O7
O2–Gd1–O6
69.88(7)
72.88(7)
82.05(7)
80.00(7)
49.93(7)
130.80(7)
138.16(8)
73.87(8)
82.19(8)
92.39(8)
142.48(7)
113.45(7)
153.67(7)
81.71(6)
O6–Gd1–O1
O6–Gd1–O3
O6–Gd1–O7
O2#1–Gd1–N1
O2–Gd1–N1
O2#1–Gd1–O4
O2–Gd1–O4
O2–Gd1–O1
O2#1–Gd1–O1
O2#1–Gd1–O3
O2–Gd1–O3
O2#1–Gd1–O7
O2#1–Gd1–O6
143.73(7)
76.52(7)
72.06(8)
106.59(6)
65.25(6)
168.37(7)
116.10(7)
122.22(6)
86.32(6)
141.39(6)
78.97(6)
104.69(8)
76.33(6)
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of the data can be obtained free of charge on quoting the depository
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Received: February 21, 2020
Published Online: ᭿
CrystEngComm 2018, 20, 777–786.
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Journal of Inorganic and General Chemistry
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Y. Wang, Z. Yuan, Y. Guo, X. Ma, Z. Meng, J. Sha,
H. Zhang* ......................................................................... 1–7
Single-Molecule Magnetism in Dy2 Cluster Based on a Schiff
Base Ligand
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