Modulating SMM behaviors in phenoxo-O bridged Dy2 compounds via different β-diketonate

Article abstract of DOI:10.1016/j.ica.2020.119595

Two new Dy₂ compounds, [Dy(TTA)₂L]₂ (1) and [Dy(dbm)₂L]₂ (2) (TTA = 2-thenoyltrifluoroacetone, and HL = 2-[(4-chlorophenyl)imino]methyl]-8-hydroxyquinoline and dbm = dibenzoylmethane), were synthesize

Full text of DOI:10.1016/j.ica.2020.119595

InorganicaChimicaActa507(2020)119595
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Research paper
Modulating SMM behaviors in phenoxo-O bridged Dy2 compounds via
different β-diketonate
Yin Ling Houa,⁎, Ting-Ting Yangb, Wen-Xin Zhaob, Chen-Juan Fanb, Li-Li Yanb, Xiao-Fen Guanb,
Jia Jia, Wen-Min Wangb,⁎
a School of Life and Health Science, Kaili University, Kaili, 556011, PR China
b Department of Chemistry, Taiyuan Normal University, Jinzhong 030619, PR China
A R T I C L E I N F O
A B S T R A C T
Keywords:
Dinuclear dysprosium compounds
Structures
Magnetic properties
Single-molecular magnets behaviors
Two new Dy2 compounds, [Dy(TTA)2L]2 (1) and [Dy(dbm)2L]2 (2) (TTA = 2-thenoyltrifluoroacetone, and
HL = 2-[(4-chlorophenyl)imino]methyl]-8-hydroxyquinoline and dbm = dibenzoylmethane), were synthesized
via solvent evaporation method, and the structures and magnetic properties of them have been characterized.
The X-ray structural analysis show that both 1 and 2 are binuclear dysprosium complexes with similar structure,
and the two central Dy atoms are bridged by two phenoxo-O atoms of two 8-hydroxyquinoline Schiff base
ligands. The only difference is the coordinate β-diketonate. Magnetic measurements indicated that the two Dy2
compounds display different single-molecular magnets (SMMs) behaviors with Ueff /kB = 29.4 K for 1 and Ueff
/kB = 43.5 K for 2.
1. Introduction
Tong group reported a stable pentagonal bipyramidal Dy(III)-based
SMM, namely [Dy(bbpen)Br], it has a record effective energy barrier
Over the past two decades, the design and construction of Ln(III)-
based single-molecule magnets (SMMs) have attracted much interest
and attention due to their potential applications for using in high-
density magnetic information storage, quantum computing devices, and
molecular spintronics [1]. The compounds exhibit slow relaxation of
magnetization on molecular level, and they normally display in-phase
and out-of-phase ac signals and/or magnetic hysteresis-loops below the
blocking temperature (TB), which are so-called single-molecule magnets
(SMMs) [2]. In 2003, the first Ln(III)-based single molecule magnet
(SMM), [Pc2Ln]-·TBA+(Ln = Tb and Dy, Pc = dianion of phthalocya-
nine; TBA+ = N(C4H9)4+), was discoveried by Naoto Ishikawa group
[3]. Whereafter, lots of Ln(III)-based compounds showing slow relaxa-
tion of magnetization have been reported [4]. For a favourable single-
molecule magnet (SMM), large effective energy barrier (Ueff) and high
blocking temperature (TB) are two key and significant factors [5]. Focus
on the two key factors, a lot of outstanding and interesting works for Ln
(III)-based SMMs have been reported [6]. Throughout these studies,
Gao, Tong, Zheng, and Layfield groups have conducted pioneering work
in the design and synthesis of Dy(III)-based SMMs [7]. It seems that and
mononuclear and binuclear Ln(III)-based compounds can display ex-
cellent SMMs behaviors. Here, a number of works focus on how to en-
hance energy barriers (Ueff/kB) of Ln(III)-based SMMs [8]. In 2016, the
over 1000 K (Ueff/kB = 1025 K) [9]. Later on, Zheng group reported a
nearly perfect pentagonal bipyramidal Dy(III)-based SMM with formula
[Dy(OtBu)2(py)5][BPh4] having a larger Ueff/kB of 1815 K [10]. In
2018, research of this aspect has achieved a breakthrough, Layfield
group reported a dysprosium metallocene cation [(Cp/Pr5)Dy(Cp*)]+
(Cp/Pr5 = penta-isopropylcyclopentadienyl, Cp* = pentamethylcyclo-
pentadienyl) with a largest effective energy barrier (Ueff/kB) of 2219 K
and blocking temperature TB = 80 K [11]. It is the largest effective
energy barrier of all the reported Dy(III)-based SMMs at present. These
excellent and outstanding works attracted much more inorganic and
materials chemistry researchers for focusing the deep study of Ln(III)-
based SMMs.
Attempts to seek efficient synthetic strategies to assemble Dy(III)-
based SMMs and further to explore the outstanding magnetic proper-
ties, in the paper, we designed and obtained two dinuclear Dy(III)-
based compounds, [Dy(TTA)2L]2 (1) and [Dy(dbm)2L]2 (2). The two
Dy2 compounds were synthesized by using an 8-hydroxyquinoline
Schiff base ligand (HL) and two β-diketones (Schemes 1 and 2). The
structures and magnetism of 1 and 2 have been deeply studied. Com-
plexes 1 and 2 show very similar structural features with a Dy2 core,
however, we find that by adjusting the coordination environment of Dy
(III) ion of 1 and 2 via two β-diketones yielded different single-
⁎ Corresponding authors.
E-mail addresses: hyl0506@126.com (Y. Ling Hou), wangwenmin0506@126.com (W.-M. Wang).
https://doi.org/10.1016/j.ica.2020.119595
Received 20 December 2019; Received in revised form 14 March 2020; Accepted 14 March 2020
Availableonline16March2020
0020-1693/©2020ElsevierB.V.Allrightsreserved.

Y. Ling Hou, et al.
InorganicaChimicaActa507(2020)119595
Z = 2 (Table 1). For 1 (Fig. 1), the dinuclear dysprosium complex is
composed of two Dy3+ ions, four TTA- and two L-, and each central
Dy3+ ion is eight-coordinated with a N2O6 coordination environment.
According to the computational result by using SHAPE 2.0 software
(see Table S1), each central Dy3+ ion possess a distorted triangular
dodecahedron geometrical configuration. The coordination mode of HL
and TTA of are shown in Figs. S1 and S2. The ligand HL serves as a
tridentate ligand and chelates the central Dy1 atom through one
phenoxide oxygen atom (O1), one pyridyl ring nitrogen atom (N1) and
one imine nitrogen atom (N2), and the TTA− adopts a bidentate mode
to chelate the central Dy1 atom. The two central Dy3+ ions are bridged
by two μ2-phenoxide oxygen atoms (O1 and O1a) of two ligands HL.
The two Dy atoms and two μ2-phenoxide oxygen atoms form a paral-
lelogram Dy2O2 core with a Dy–O–Dy angle of 108.77(8)°, and the
Dy┄Dy distance is 3.8319(15) Å. Moreover, in 1, the lengths of the
Dy–O bonds are in the range of 2.306(5)–2.408(5) Å, the Dy1–N1 and
Dy1–N2 bond distances are 2.461(5) and 2.661(6) Å, respectively; the
O–Dy–O angles are in the in the range of 70.17(17)–150.62(18)°. These
bond distances and angles of 1 are comparable to those of the reported
Ln(III)-based complexes [13].
As shown in Fig. 2, the molecular structure for 2 is composed of two
Dy3+ ions, four dbm− and two L−. The coordination environment and
geometrical configuration of central Dy3+ ion are almost the same as
these of 1 (see Table S1), the only difference is the Dy–O and Dy–N
bond distances. The Dy–O bond distances are in the range of
2.294(2)–2.434(2) Å, the Dy1–N1 and Dy1–N2 bond lengths are
2.489(3) and 2.672(3) Å, respectively. Furthermore, in 2, the distance
of the two neighbouring Dy3+ ions is 3.8776(7) Å and the Dy–O–Dy
bone angle is 109.06(8) °, which are slight bigger than these in 1.
Scheme 1. The structure of ligand HL.
molecular magnets (SMMs) behaviors.
2. Experimental section
2.1. Synthesis of 1 and 2
Dy(TTA)3·2H2O (0.04 mmol) was added to a solution of 15 mL n-
heptane and refluxed for 3 h, then the solution was cooled to 60 °C and
5 mL CH2Cl2 containing HL (0.04 mmol) was added. The mixed solution
was stirred at 60 °C for about 1 h. After reaction finished, the mixed
solution cooled to room temperature. The mixture was filtered and the
filtrate was kept at room temperature, red and needlelike crystals of 1
were obtained after about one week, yield about 41% (based on Dy
(TTA)3·2H2O).
C
Elemental
analysis
(%)
calcd
for
64H36Cl2Dy2F12N4O10S4 (MW = 1773.10): C 43.31, H 2.03, N 3.16.
Found: C 43.45, H 1.91, N 3.27. IR (KBr, cm−1): 1651(s), 1598(w),
1552(w), 1485(m), 1258(s), 1202(s) , 1148(m), 1096(w), 907(w),
842(m), 765(m) , 562(m).
Dy(dbm)3·2H2O (0.03 mmol) was added to a solution of HL
(0.03 mmol) in 20 mL of CH3OH/CH2Cl2 (v/v = 3:1), and the mixture
was stirred at 80 °C for 4 h. Then the mixed solution cooled to room
temperature and filtered. The filtrate was kept at room temperature, red
and needlelike crystals of 2 were obtained after about 10 days. Yield
about 47% (based on Dy(dbm)3·2H2O). Elemental analysis (%) calcd for
3.2. Powder X-ray diffraction
In order to verify phase purities of compounds 1 and 2, the crys-
talline products of them have been characterized by Powder X-ray
diffraction (PXRD) at room temperature (Figs. S3 and S4). The experi-
mental PXRD patterns are in good agreement with the simulated ones
from the single crystal data, indicating the high purities of the syn-
thesized samples of 1 and 2.
C
94H70Cl4Dy2N4O11 (MW = 1898.34): C 59.42, H 3.69, N 2.95; Found:
C 59.46, H 3.58, N 2.83. IR (KBr, cm−1): 1652(s), 1599(w), 1553(w),
1486(m), 1259(s), 1203(s), 1145(m), 1098(w), 907(w), 840(m),
760(m), 561(m).
3.3. Magnetic properties
2.2. Single-crystal X-ray diffraction measurements
Variable-temperature direct-current (dc) magnetic susceptibility for
compounds 1 and 2 were measured under the field of 1000 Oe and
during the temperature range 300–2.0 K. The plots of χMT versus T for
Single crystal X-ray diffraction data of 1 and 2 was collected on a
computer-controlled Rigaku Saturn CCD area detector diffractometer,
equipped with confocal monochromatized Mo Kα radiation with a ra-
diation wavelength of 0.71073 Å using the ω-φ scan technique. The
structures were solved by direct methods and refined with a full-matrix
least-squares technique based on F2 using the SHELXS-2016 and
SHELXL-2016 programs [12]. Anisotropic thermal parameters were
assigned to all non-hydrogen atoms. Crystallographic data and struc-
tural refinement parameters are listed in Table 1. CCDC 1061001 for 1
and 1973326 for 2 contain the supplementary crystallographic data for
this paper. These data can be obtained free of charge from The Cam-
bridge Crystallographic Data Centre.
1
and 2 are shown in Fig. 3. At 300 K, the χMT values are
28.32 cm3 K mol−1 for 1 and 28.37 cm3 K mol−1 for 2, respectively;
which are good agree with the expected value of 28.34 cm3 K mol−1 for
two free Dy(III) ions (6H15/2, g = 4/3). As the temperature is decreased,
the χMT values of 1 and 2 gradually decrease from 300 to 50 K and then
rapidly drop to a minimum value of 8.90 (1), 8.55 (2) cm3 K mol−1 at
2.0 K. Such magnetic behaviors generally due to one or a combination
of the following two phenomena: (1) the progressive depopulation of
the excited Stark sub-levels of the DyIII ions; (2) weak antiferromagnetic
interactions between the two adjacent DyIII ions of 1 and 2 [14].
Alternating-current (ac) magnetic susceptibility of compounds 1
and 2 were undertaken at 3.0 Oe ac field with Hdc = 0 field in order to
investigate the dynamics magnetic behavior. As shown in Fig. 4, com-
plexes 1 and 2 exhibit pronounced frequency-dependent out-of-phase
(χ″) signals and evident peaks are observed, indicating slow magnetic
relaxation with the characteristic of SMM behavior [15]. However, the
χ″ peaks were observed during the temperature range 4.5–9.0 K for 1;
and the shoulder peaks of χ″ signals were appeared during the tem-
perature range 8.5–13.0 K between 711 and 3111 Hz for 2. For further
study the dynamics magnetic behavior of 1 and 2, the frequency de-
pendence of ac susceptibilities were also measured under differ-
ent temperature for 1 (2.0–10.0 K) and for 2 (2.0–14.0 K) (Figs. S5 and
3. Results and discussion
3.1. Structure descriptions of 1 and 2
In this paper, the reactions of ligand HL and Dy(TTA)3·2H2O/Dy
(dbm)3·2H2O in a mixture of n-heptane/CH2Cl2 or CH3OH/CH2Cl2, red
and needlelike crystals of 1 and 2 suitable for single-crystal X-ray dif-
fraction were obtained, respectively. X-ray diffraction analyses reveal
that both compounds 1 and 2 possesse a dinuclear structure, however,
compound 1 crystallizes in the triclinic space group Pī with Z = 1, and
compound 2 crystallizes in the monoclinic space group P21/n with
2

Y. Ling Hou, et al.
InorganicaChimicaActa507(2020)119595
Scheme 2. The structures of TTA and dbm.
Table 1
Crystallographic data and structure refinement summary for 1 and 2.
Complexes
1
2
Empirical formula
Mr
T (K)
C64H36Cl2Dy2F12N4O10S4
1773.10
113(2)
C94H70Cl4Dy2N4O11
1898.34
113(2)
Crystal system
Space group
triclinic
P1
monoclinic
P21/n
a/Å
b/Å
c/Å
10.797(2)
12.891(3)
13.362(3)
69.90(3)
71.01(3)
79.98(3)
1647.5(6)
1
1.787
2.553
2.00 to 25.02
866
11.126(2)
23.786(5)
15.314(3)
90
101.15(3)
90
3976.2(14)
2
1.586
α/°
β/°
γ/°
V/Å3
Z
Dcalcd/g cm−3
μ/mm−1
2.066
1.60 to 27.89
1900
θ/°
F(0 0 0)
Fig. 2. Molecular structure for 2 (hydrogen atoms are omitted for clarity).
Reflections collected
Unique reflns
Rint
13,792
5787
0.0498
1.050
38,855
9451
0.0516
1.103
GOF (F2)
R1, wR2 (I > 2σ(I))
R1, wR2 (all data)
0.0506, 0.1220
0.0574, 0.1275
0.0341, 0.0834
0.0430, 0.0921
Fig. 3. Temperature dependence of the χMT products at 1.0 kOe for 1 and 2.
Orbach relaxation processes, respectively. The best fit was obtained for
n = 5.08, A = 0.3764 s−1 K−5.08, C = 0.08811, Ueff/kB = 30.7 K and
τ0 = 3.98 × 10−6 s for 1, and n = 4.40, A = 0.4773 s−1 K−4.40
,
Fig. 1. Molecular structure for 1 (hydrogen atoms are omitted for clarity).
C = 0.4227, Ueff /kB = 45.7 K and τ0 = 1.29 × 10−6 s for 2 (Fig. 5).
The important parameter values of Ueff/kB and τ0 for 1 and 2 are
comparable to those of reported Dy2 SMMs [17]. The small A and C
value indicate that the relaxation process can dominate by the Orbach
mechanism at the high temperature and the Raman mechanism at the
low temperature.
S6). The out-of-phase (χ″) signals of the ac susceptibility of 1 and 2
show temperature dependences, which further confirms the SMM be-
haviors in 1 and 2.
What is noteworthy that the plots of ln(τ) versus 1/T for compounds
1 and 2 under zero dc field exhibit obvious curvature, which indicates
that perhaps another relaxation pathway is also operative. So, we fitted
the magnetic data with the Eq. (1) [16]:
The Cole–Cole plots of χ″ vs. χ′ for 1 and 2 are shown in Fig. 6, for 1,
it is a relatively symmetrical and semicircle shape, and the best fits the
Cole–Cole curves in the range of 2.0–10.0 K were obtained with
α = 0.13–0.24 using the generalized Debye model. For 2, it shows an
asymmetric shape, and we fitted it by using Debye model and obtained
lnτ = −ln[AT + B + CTn + τ0−−1exp(−ΔE/KB T)]
(1)
where AT + B, CTn and τ0−1exp(ΔE/kBT) represent direct, Raman and
3

Y. Ling Hou, et al.
InorganicaChimicaActa507(2020)119595
Fig. 4. Temperature dependence of the in-phase and out-of-phase components of the ac magnetic susceptibility for 1 and 2 under Hdc = 0 Oe field with an oscillation
of 3.0 Oe.
Fig. 5. Plots of ln(τ) versus T−1 fitting to the Arrhenius law for complexes 1 (left) and 2 (right) under Hdc = 0 Oe field.
α = 0.17–0.32. The α value of 2 is larger than that of 1, which imply a
wider distribution of relaxation time in 2.
Visualization, Investigation, Data curation. Wen-Xin Zhao: Data cura-
tion, Software. Chen-Juan Fan: Data curation. Li-Li Yan: Software.
Xiao-Fen Guan: Supervision. Jia Ji: Validation, Funding acquisition.
Wen-Min Wang: Conceptualization, Methodology.
4. Conclusion
In summary, two new dinuclear dysprosium compounds (1 and 2)
based on an 8-hydroxyquinoline Schiff-base ligand have been synthe-
sized. The structures and magnetic properties of them have been deeply
studied. Although the two phenoxo-O bridged binuclear complexes
with similar structures, ac susceptibility study show that compounds 1
and 2 exhibit different single-molecular magnets (SMMs) behaviors.
Acknowledgment
This work was supported financially by the Science and Technology
Foundation of Guizhou Province (J[2015]2130), the National Natural
Science Foundation of China (21501079), the Scientific and
Technological Innovation Programs of Higher Education Institutions in
Shanxi (No. 201802099, 2019L0817), the Fund for Shanxi “1331
Project” Key Innovative Research Team, Key Laboratory of Ecological
Restoration of Water Pollution (Taiyuan Normal University), and Key
Research and Development Projects of Shanxi Province (Grant No.
CRediT authorship contribution statement
Yin Ling Hou: Writing - original draft, Software. Ting-Ting Yang:
4

Y. Ling Hou, et al.
InorganicaChimicaActa507(2020)119595
Fig. 6. Cole–Cole plots for 1 (left) and 2 (right) measured in zero-dc field. The red solid lines are the best fit to the experimental data, obtained with the generalized
Debye model with α = 0.13–0.24 for 1 and α = 0.17–0.32 for 2. (For interpretation of the references to colour in this figure legend, the reader is referred to the web
version of this article.)
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