Inorganic Chemistry Communications 90 (2018) 69–72

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Inorganic Chemistry Communications

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Short communication

Isostructural lanthanide metal-organic frameworks comprised of left-

handed helical chains: Synthesis, structure and luminescent properties
Jia Lin a, Yinglin Cui a, Chunxian Ke a, Xueqiong Zhang a, Xiaoming Lin a,⁎, Yuepeng Cai a, Yongbo Wu a,b,⁎⁎
a
School of Chemistry and Environment, South China Normal University, Guangzhou Key Laboratory of Materials for Energy Conversion and Storage, 510006, PR China
b
South China Normal University, School of Physics and Telecom Engineering, 510006 Guangzhou, PR China

a r t i c l e i n f o a b s t r a c t

Article history: Six isostructural three-dimensional (3D) lanthanide metal-organic frameworks (Ln-MOFs), [Ln(μ2-OH)(PDC)
Received 24 January 2018 (H2O)2]·DMF (Ln = Pr (1), Nd (2), Eu (3), Tb (4), Ho (5), and Yb (6), H2PDC = pyridine-3,5-dicarboxylic
Received in revised form 16 February 2018 acid), have been successfully synthesized under solvothermal conditions and characterized by single crystal X-
Accepted 20 February 2018
ray diffraction, IR spectroscopy, elemental analysis and thermal gravimetric analysis. The framework contains un-
Available online 22 February 2018
usual Ln-carboxylate/μ2-OH left-handed helical chains, which are extended by PDC2− linkers to form 3D net-
works with 1D hexagonal channel. The lanthanide contraction effect induces the decreases of average Ln-
distances from Pr to Yb. Due to the efficient sensitization of PDC2− ligand, complexes 2 and 6 display strong char-
acteristic luminescence in the near-infrared (NIR) region, respectively. Moreover, the luminescent properties of
complexes 3 and 4 are also studied in the solid state at room temperature.
© 2018 Elsevier B.V. All rights reserved.

1. Introduction Ln-MOFs with various aromatic-carboxylic groups or pyridine-

Lanthanide metal-organic frameworks (Ln-MOFs) have been com-
pelling research direction due to diversified topological structures
[1–4], superior properties and gigantic prospective applications in nu-
merous domains, such as luminescence [5–8], molecular magnetism
[9], gas storage/separation [10–13], proton conductivity [14] and catal-
ysis [15]. It is universally acknowledged that trivalent lanthanide ions
are promising candidates for constructing unique luminescent materials
owing to their high luminescence quantum yield, narrow and intense
band emission, giant Stokes shift, and long luminescence lifetimes
[16–19]. A lot of aromatic-carboxylic groups or pyridine-carboxylate li-
gands have been demonstrated to be good luminescent chromophores,
which are good sensitizers to stimulate lanthanide ion luminescence
[20–22].
Ln-MOFs bearing active recognized sites are generally considered as
great luminescent probes and sensors for the recognition and sensing of
cations, anions, small molecules, vapors, pH values and even tempera-
ture [23–26]. Additionally, combining different lanthanide ions into
isostructural Ln-MOFs is an effective method to generate functional
Ln-MOFs [27–29]. In order to further investigate 3D Ln-MOFs and
their intrinsic properties, we have been bent on synthetizing diversified
⁎ Corresponding author.
⁎⁎ Correspondence to: Y. Wu, School of Chemistry and Environment, South China
Normal University, Guangzhou Key Laboratory of Materials for Energy Conversion and
Storage, 510006, PR China.
E-mail addresses: linxm@scnu.edu.cn (X. Lin), wuyongbo@m.scnu.edu.cn (Y. Wu).
carboxylate ligands and luminescent ions under solvothermal reactions
and exhibited excellent luminescent properties [30–35]. Herein, we
successively report the synthesis, structural and luminescent investiga-
tions of six isostructural Ln-MOFs, [Ln(μ2-OH)(PDC)(H2O)2]·DMF (Ln
= Pr (1), Nd (2), Eu (3), Tb (4), Ho (5), and Yb (6), H2PDC = pyri-
dine-3,5-dicarboxylic acid) based on the unusual Ln-carboxylate/μ2-
OH left-handed helical chain. Meanwhile, complexes 2, 3, 4, and 6 ex-
hibit strong luminescence from the Ln3+ centers because of the sensiti-
zation of PDC2− ligand.
Complexes 1–6 were prepared by a mixture of Ln(NO3)3·6H2O
(0.5 mmol), H2PDC (0.5 mmol), two drops of HOAc, DMF (4 mL) and
H2O (4 mL) sealed in a Teflon-lined autoclave and heated under autog-
enous pressure at 120 °C for 3 days. After being cooled to room temper-
ature, six isostructural Ln-MOFs were obtained and washed with DMF.
The formula of [Ln(μ2-OH)(PDC)(H2O)2]·DMF was further confirmed
by elemental analysis and thermal gravimetric analysis (TGA). Single
crystal X-ray structure analyses reveal that complexes 1–6 are
isostructural and crystallize in the hexagonal spontaneous resolution
P6122 space group. As a representative example, the crystal structure
of 1 is described in detail. Complex 1 has a three-dimensional frame-
work, the asymmetric unit of which consists of one Pr(III) ion, one
fully deprotonated PDC2− ligand, one μ2-OH, two coordinated water
molecules, and one lattice DMF molecule. As shown in Fig. 1, Pr(III)
ion is nine-coordinated by four carboxylate O atoms from four carboxyl-
ate groups of distinct PDC2− ligands, one N from pyridyl group of the
fifth different PDC2− ligand, two O atoms from a μ2-OH, and two oxygen
atoms from coordinated water molecules, forming a distorted tricapped

https://doi.org/10.1016/j.inoche.2018.02.010
1387-7003/© 2018 Elsevier B.V. All rights reserved.
70 J. Lin et al. / Inorganic Chemistry Communications 90 (2018) 69–72

trigonal prism coordination geometry (Fig. 1b). Each PDC2− ligand brid-
ges five Pr(III) ions through carboxylate groups or pyridyl groups with
the unique μ5-η1:η1:η1:η1:η1 mode (Fig. 1c). Interestingly, the
interlinkage between Pr(III) ions and PDC2− ligands through
monodentate/bridging carboxylate groups give rise to an infinite 1D
Pr-carboxylate left-handed helical chain along the ac plane (Fig. 1d)
and c-axis (Fig. 1e). Followed by the further coordination of Pr(III)
ions and N atoms from PDC2− ligands, 1D Pr-carboxylate left-handed
helical chains are extended to a 3D framework with the window sizes
of ~ 9.4 × 9.4 Å2 (Fig. 1f). Furthermore, the chains are strengthened by
μ2-OH atom bridging adjacent Pr(III) ions, resulting in unusual Pr-
carboxylate/μ2-OH chains (Fig. 1g and h). Meanwhile, a narrower 1D
hexagonal channel with the effective dimensions of ~3.1 × 3.1 Å2 is ob-
served along the c-axis (excluding van der Walls radii of the atoms).
PLATON analysis reveals that the 3D framework is composed of voids
of 42.5% that represent 1972.3 Å3 per unit cell volume and 838.3 Å3
total potential solvent area volume. Based on above description of the
crystal structures, complexes 1–6 are isomorphous. The average Ln\\O
and Ln\\N bond lengths and Ln⋯Ln separations decrease from Pr3+ to
Yb3+ ions, consistent with the decreasing sequence of ionic radii due
to the effect of lanthanide contraction. The average bond lengths of
Ln\\O for 1–6 continuously decrease from 2.481 (for 1), 2.477 (for 2),
2.447 (for 3), 2.427 (for 4), 2.405 (for 5) to 2.377 Å (for 6). Generally,
as the sizes of the Ln3+ ions decrease, the repulsions among the coordi-
nation atoms around one metal center increase, until the crystal struc-
ture becomes unstable and then forms a new structure [36,37].
Around the nine-coordinated Ln3+ centers from 1 to 6, the Ln-N
separations decrease significantly from 2.75 to 2.52 Å, which is also im-
itated by Ln⋯Ln separations from 4.540 to 4.422 Å.
Thermal gravimetric analysis (TGA) of 1–6 was carried out to exam-
ine the stability of the framework. TGA measurement was performed in
the temperature range of 25–800 °C in the air atmosphere. In line with
the isostructural structures of 1–6, TGA curves of 1 and 6 are herein
discussed. As shown in Fig. S1, their TGA curves display the similar ther-
mal decomposition behaviors. The TGA curves in the range of 25–200 °C
show a first weight loss of 16.83 (for 1), and 15.62% (for 6), respectively,
corresponding to loss of one guest DMF molecule (calcd. 16.91, and
15.74%, respectively). The second weight loss occurred from 200 to
350 °C, which could be attributed to the loss of two coordinated H2O
molecules for 1 (calcd/found = 8.33/8.41%) and for 6 (calcd/found =
7.75/7.71%). The further heating above 400 °C leads to the framework
decomposition due to the loss of PDC2− ligands.
The solid-state emission spectra of complexes 2, 3, 4 and 6 at room
temperature were measured from the visible to the near-infrared re-
gion. As shown in Fig. 2a, complex 2 displays three strong emission
bands in the NIR region, derived from the typical f-f transitions of the
Nd(III) ion at 4F3/2 → 4I9/2 (895 nm), 4F3/2 → 4I11/2 (1062 nm), and 4F3/
4 2−
2 → I13/2 (1336 nm), respectively, indicating that PDC sensitizes
Nd3+ ions via the antenna effect. Similar to complex 2, the NIR lumines-
cent spectra of complex 6 (λex = 336 nm) exhibits a NIR emission at
around 980 nm (Fig. 2b), which can be assigned to the 2F5/2 → 2F7/2 tran-
sition of the Yb(III) ion. Observation of NIR luminescence for complexes
2 and 6 supports that PDC2− ligands serve as an energy-acceptable “an-
tenna” for the central Ln3+ ions [38]. On the other hand, the emission

Fig. 1. (a) Coordination environment of the Pr(III) ion; (b) Tricapped trigonal prism coordination geometry of the Pr(III) ion; (c) Coordination modes of PDC2− ligands; (d) and (e) 1D Pr-
carboxylate left-handed helical chain; (f) 3D framework constructed by Pr3+ ions and PDC2− ligands along the c-axis; (g) and (h) 1D Pr-carboxylate/μ2-OH chain; (i) Polyhedral view of 3D
frameworks showing the 1D hexagonal channels along the c-axis. All the lattice solvent molecules and H atoms are omitted for clarity.
 J. Lin et al. / Inorganic Chemistry Communications 90 (2018) 69–72
Fig. 2. Solid-state luminescence spectra of (a) 2 (λex = 319 nm), (b) 6 (λex = 336 nm), (c) 3 (λex = 331 nm), and (d) 4 (λex = 316 nm).
spectrum of complex 3 displays the characteristic emission of Eu(III)
ions (λex = 331 nm), namely, 5D0 → 7F0 (568 nm), 5D0 → 7F1
(592 nm), 5D0 → 7F2 (619 nm), 5D0 → 7F3 (652 nm) and 5D0 → 7F4
(703 nm) (Fig. 2c). As we know, the intensity of 5D0 → 7F1 (magnetic di-
pole transition) is insensitive to the coordination environment, while
the intensity of 5D0 → 7F2 (electric-dipole transition) increases as the
site symmetry decreases. The relative intensity of 5D0 → 7F2 and 5D0
→ 7F1 transitions are used as a measure of the coordination state and
site symmetry of the Eu(III) ions. In the spectra of complex 3, the inten-
sity ratio of 2.65 for I(5D0 → 7F2)/I(5D0 → 7F1) is much higher than the
typical value for a centrosymmetric Eu(III) ions, indicating that the sym-
metry of the Eu(III) ion site is low and the Eu(III) ion lacks an inversion
center. Furthermore, the appearance of the symmetry forbidden emis-
sion 5D0 → 7F0 at 568 nm suggests that the Eu(III) ions occupy low-
symmetry coordination sites with no inversion centers, which is in
agreement with the results of X-ray structural analysis. As expected,
the emission spectrum of 4 (λex = 316 nm) indicates the well-
resolved magnified luminescence of the f-f transitions, which is contrib-
uted from the energy transfer from PDC2− ligands to Tb(III) ions. The
evident characteristic transitions of Tb(III) ion in compound 4 can be ob-
served at 491, 545, 585 and 621 nm, which are contributed from the 5D4
→ 7F6, 5D4 → 7F5, 5D4 → 7F4 and 5D4 → 7F3 f-f transitions, respectively
(Fig. 2d).
In summary, we have successfully reported the synthesis, structure
and luminescence investigations of a series of isostructural [Ln(μ2-OH)
(PDC)(H2O)2]·DMF (Ln = Pr (1), Nd (2), Eu (3), Tb (4), Ho (5), and
Yb (6)) under solvothermal condition. The 3D framework exhibits 1D
Ln-carboxylate left-handed helical chain. Complexes 3 and 4 display
strong characteristic luminescence in the visible region and complexes
2 and 6 reveal NIR emission. These results prove that they may be
regarded as candidates for luminescent materials.
Acknowledgments
The authors are grateful for financial aid from the National Natural
Science Foundation of China (Grant No. 21471061 and 21671071),
71
Applied Science and Technology Planning Project of Guangdong Prov-
ince, Guangzhou, China (No. 2015B010135009, 2017A010104015, and
2017B090917002), Innovation team project of Guangdong Ordinary
University (No. 2015KCXTD005), the great scientific research project
of Guangdong Ordinary University (No. 2016KZDXM023).
Appendix A. Supplementary material
CCDC 1818877-1818882 contain the supplementary crystallo-
graphic data for 1–6. The data can be obtained free of charge via
http://www.ccdc.cam.ac.uk/data_request/cif, or from the Cambridge
Crystallographic Data Centre, 12 Union Road, Cambridge CB2 1EZ, UK;
fax: (+44) 1223–336-033; or e-mail: deposit@ccdc.cam.ac.uk. Addi-
tional structural figures and tables are available as electronic supple-
mentary information in the online version. Supplementary data to this
article can be found online at https://doi.org/10.1016/j.inoche.2018.02.
010.
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