A low symmetry cluster meets a low symmetry ligand to sharply boost MOF thermal stability

Article abstract of DOI:10.1039/d0cc04543h

A new approach in which a low symmetry cluster meets a low symmetry ligand to sharply boost the thermal stability of a MOFviaadditional inter-linker interactions is presented for the first time, leading to the successful synthesis of a novel binuclear Co-

Full text of DOI:10.1039/d0cc04543h

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The Lower Symmetric Cluster Meets the Lower Symmetric Ligand
to Sharply Boost MOFs’ Thermal Stability
Yajun Gao,‡a Mingxing Zhang,‡c Cong Chen,a Yong Zhang,d Yuming Gu,d Qian Wang,b Wenwei
Received 00th January 20xx,
Accepted 00th January 20xx
Zhang,a Yi Pan,a Jing Ma,d and Junfeng Bai*a,b
DOI: 10.1039/x0xx00000x
www.rsc.org/
A new approach that the lower symmetric cluster meets the lower be activated, in particular, a lot of the binuclear based MOFs
symmetric ligand for sharply boosting MOFs’ thermal stability by due to the relatively weak bonding based upon these lower
additional inter-linker interactions was first presented, leading to a clusters.6 Among these, there are some exceptions, like the Cu-
successful synthesis of the novel binuclear Co-based MOF, paddlewheel cluster based MOFs with the relatively low
{[Co2(L1)2DMF]•1.5DMF•0.75MeOH•1.5H2O}∞ (H2L1 = 5-(pyridin-3- thermal stabilities around 250 C or less.7 Thus, construction of
yl) isophthalic acid) (NJU-Bai62, NJU-Bai for Nanjing University Bai highly stable MOFs from them is a great challenge.
group), with exceptional thermal stability up to 450 °C. This work
Herein, we present a novel approach that the lower
may open up a new avenue for constructing robust MOFs from the symmetric cluster meets the lower symmetric ligand to sharply
abundant, unstable, and lower symmetric binuclear clusters which boost inherently unstable binuclear Co-based MOFs’ thermal
have usually been ignored by most MOFs’ chemists.
stability by additional inter-linker interactions, and NJU-Bai62
was afforded. In comparison with similar MOFs, NJU-bai63,
{[Co2(L1)2]•2DMA•H2O}∞, and {[Co2(L2)2]•4DMF•2H2O}∞ (H2L2 =
5-(pyridin-4-yl) isophthalic acid) (termed as NOTT8, reported by
Nottingham University), this method was further revealed
clearly (Figure 1). Notably, NJU-Bai62 exhibit exceptional
thermal stability up to 450 C, which is comparable to those of
the famous thermostable MOFs based on polynuclear clusters
(nuclearity ≥ 3) or rod-shaped building blocks, and the highest
among MOFs based on binuclear clusters. In addition, NJU-
Bai62 with the high CO2 adsorption capacity and CO2 selectivity
may be a potential candidate for CO2 capture.
Solvothermal reaction of Co(NO3)2•6H2O, H2L1, DMF and
MeOH led to purple NJU-Bai62 with the space group P1. The
tightly twisted binuclear Co-cluster is composed of four carboxyl
groups, two nitrogen atoms from six distinct H2L1 ligands and
one oxygen atom from DMF molecule (Figure S2a). Both of the
two Co atoms in this asymmetric cluster adopt 6-coordinated
geometry, in which Co1 is surrounded by four O atoms and one
N atom from four separate ligands and one O atom from
terminal DMF, while Co2 is encircled by five O atoms and one N
atom from five separate ligands (Figure S2e). For matching the
seriously distorted cluster, the ligand shows irregular
coordination mode, the pyridine ring and isophthalic acid
moiety of the ligand are not coplanar. Meanwhile, the ligand
links three Co-clusters through one N atom and two carboxyl
groups. One carboxyl shows bridging-chelating and bridging
modes, the other one is chelating and bridging modes (Figure
S2i). Furthermore, the Co-clusters are connected by the ligands
Metal-organic frameworks (MOFs) are a class of intriguing
porous materials and have shown great potential in many
applications, including gas storage and separation, catalysis,
chemical sensing, etc.1 Many applications heavily rely on the
permanent porosity of MOFs. Thus, being stimulated by MOF-5
from Yaghi group,2 many researchers have developed one
promising strategy of the introduction of highly symmetric
multinuclear metal clusters with high connectivity into MOFs to
enhance their thermal stability, et al,3 due to that these could
not only build the strong bonding between clusters and linkers,
but also provide the directionality that enable symmetry-
adapted linkers extend naturally and keep away from each
other,4 resulting in MOFs with high thermal stabilities for
supporting the existence of high porosity.5
Thanks to the above strategies, many stable MOFs with
permanent porosity have been reported in the past decades.
However, many MOFs with visible channel or cage can still not
a. State Key Laboratory of Coordination Chemistry, School of Chemistry and
Chemical Engineering, Nanjing University, Nanjing 210023, China
b. School of Chemistry and Chemical Engineering, Shaanxi Normal University, Xi’an
710119, China. E-mail: bjunfeng@nju.edu.cn; bjunfeng@snnu.edu.cn
c. School of Chemistry and Chemical Engineering, Nantong University, Nantong,
Jiangsu, China
d. Key Laboratory of Mesoscopic Chemistry of Ministry of Education, School of
Chemistry and Chemical Engineering, Nanjing University, Nanjing 210023, China.
† Electronic Supplementary Information (ESI) available. CCDC 2006010-2006012.
For ESI and crystallographic data in CIF or other electronic format see
DOI: 10.1039/x0xx00000x
‡ These authors contributed equally to this work.
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in mode 1 to form the 2D layers with hcb topology, then further
pillared by the ligands in mode 2 to form a porous
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DOI: 10.1039/D0CC04543H
Fig. 1 a), b) and c) The binuclear Co-clusters, ligands and 1D channels in NJU-Bai62, NJU-Bai63, and NOTT, respectively; d), e) and f) The
variable-temperature powder X-ray diffraction (VT-PXRD) patterns of NJU-Bai62, NJU-Bai63, and NOTT, respectively.
3D framework (Figure S3a). Thus, two different 1D channels previous H-to-ring center distance and the H-to-O distance
with the pore sizes of about 5.6 × 5.0 Å2 and 5.6 × 3.8 Å2 are become shorter (Table S2).
generated in NJU-Bai62, respectively (Figure S4h). From the
For comparison, the similar MOFs, NOTT and NJU-Bai63 were
viewpoint of structural topology, the clusters and ligands could also synthesized and their properties have been explored. The
be regarded as 6-connected and 3-connected nodes, (3,6)-connected NOTT with symmetric H2L2 ligand and slightly
respectively. Consequently, NJU-Bai62 is a (3,3,6)-connected distorted Co-paddlewheel cluster exhibits rtl topology (Figures
network with the point symbol {4·62}2{42·68·85} (Figure S5a). The 1c, S3c and S5d). Rectangular channels with diameters of about
tightly twisted and lower symmetric cluster of this MOF links the 6.0 × 6.0 Å2 could be found in the framework (Figure S4b). After
neighbor ligands by abundant edge-to-face C-H···π interactions9 decreasing the symmetry of the ligand via substituting H2L2 with
and C-H···O hydrogen bonding10, in which the H-to-ring center H2L1 ligand, the obtained NJU-Bai63 with the similar topology
distance is ca. 2.81-3.45 Å and the H-to-O distance is ca. 2.34- as NOTT shows no obviously change in the configuration and
3.26 Å (Figures S6a, S6c and Table S2). Those weak inter-linker connection of node (Figures 1b, S3b and S5c). Like our previous
interactions may help to suppress shape-shifting of the ligand work,7d the symmetry decreasing of the ligand consequently
and the following dissociation of MOFs, thus forming highly made the distance between the ligands much more contracted
stable structure.
than that of NOTT, and the channel along the a axis is reduced
The X-ray single-crystal structure of the activated NJU-Bai62 to about 4.0 × 2.4 Å2 (Figure S4e).
has also been determined and further revealed that after all the
NOTT and NJU-Bai63 would decompose immediately in
solvent molecules in the channel and the coordinated DMF are methanol, while NJU-Bai62 could survive in nearly all low
completely removed (Figures S2f and S8), and the two carboxyl boiling point solvents. The VT-PXRD analyses reveal that NOTT

groups within mode 2 gradually changes to unified bridging could only survive below 50 C (Figures 1f and S9c). When the
mode (Figure S2j). Concomitantly, the rotating of the pyridine ligand’s symmetry is lowered solely, the NJU-Bai63’s survival
ring and carboxyl group of H2L1 ligand results in narrowing both temperature becomes around 250 °C (Figures 1e and S9b).
of the pore size to the same size of about 5.6 × 3.3 Å2 (Figure When the symmetries of the ligand and cluster are lowered
S4j). Very interestingly, besides previously mentioned weak simultaneously and match each other, NJU-Bai62 exhibits
inter-linker interactions, more new ones are also generated exceptional higher thermal stability and could maintain its
after the activation process (Figures S6b and S6d) and the structure up to 450 °C (Figures 1d and S9a). Such high thermal
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stability is comparable to those of many famous thermostable 0.9 wt %) and CH4 (43.8 and 25.2 cm3 g-1, corresponding to 3.0
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DOI: 10.1039/D0CC04543H
MOFs based on polynuclear clusters (nuclearity ≥ 3) or rod- and 1.8 wt %) at 273 and 298 K under 1 bar.
shaped building blocks and the highest among MOFs based on
The selectivities of NJU-Bai62 for CO2/N2 (0.15:0.85) and
binuclear clusters (Figure 2, Tables S3 and S4). The electrostatic CO2/CH4 (1:1) mixtures were further calculated by the ideal
interaction may play a dominant role maintaining the MOFs’ adsorbed solution theory (IAST) method based on the
structure at high temperature. To compare the relative strength experimental single component isotherms. As shown in Figure
of electrostatic interactions of NJU-Bai62, the activated NJU- 3d, the selectivities of CO2/N2 and CO2/CH4 are 113.9 and 13.6
Bai62, NJU-Bai63 and NOTT, we used the coulomb potential to at 273 K and 1 bar, respectively, and 65.5 and 10.4 at 298 K and
calculate the electrostatic interactions at the DFT (PBE) 1 bar, correspondingly. In addition, the separation ratio of CO2
optimized structures with the periodic boundary condition versus N2 and CH4 for NJU-Bai62 were also calculated from the
model (Tables S9-12 and Figures S17-18). The results show that ratio of the initial slopes based on the isotherms (Figures S15
electrostatic interaction energy per atom of the activated NJU- and S16). The selectivities for CO2/N2 are 55.0 and 42.7 at 273
Bai62 is the highest among them (Table S12). On basis of the and 298 K, respectively, which are comparable to those of
DFT optimized structure, the XRD curves of the activated NJU- several reported Co-MOFs (Table S7).
Bai62 at 450 °C was simulated by Pawley refinement method
(Figure S18). The difference between the experimental and
simulated XRD curves is tinny, indicating that NJU-Bai62 has
excellent thermal stability up to 450 °C.
Fig. 3 a) N2 sorption isotherm of NJU-Bai62 at 77 K; b) CO2, N2, and CH4
adsorption isotherms of NJU-Bai62 at 273 and 298 K (filled symbols:
Fig. 2 Comparison of the thermal stabilities of NJU-Bai62 with some
adsorption; open symbols: desorption); c) The isosteric CO2 adsorption
representative MOFs with permanent porosity based on the VT-PXRD
enthalpy of NJU-Bai62; d) IAST predicted selectivities for CO2/N2 (0.15:0.85)
patterns.
and CO2/CH4 (1:1) mixture of NJU-Bai62 at 273 and 298 K.
For investigating the permanent porosity of NJU-Bai62, the
To further understand these observations, the adsorption
enthalpy (Qst) of CO2 for NJU-Bai62 was calculated by the virial
method using the experimental isotherm data at 273 and 298 K.
At zero loading, the CO2 adsorption enthalpy is 31.3 kJ mol-1
(Figure 3c), reflecting a strong interaction between the
framework and CO2 molecules. Additionally, CO2 adsorption
sites were investigated by the Grand Canonical Monte Carlo
simulations (Figure S19) and the binding energy between the
activated NJU-Bai62 and CO2 molecules was calculated by using
density functional theory (DFT) (Figure S20). The simulation
results reveal that the Co sites could provide moderate
interaction toward CO2, leading to high CO2 adsorption uptakes.
In summary, we provide an unprecedented approach that the
lower symmetric cluster meets the lower symmetric ligand to
sharply boost MOFs’ thermal stability by additional inter-linker
interactions. The afforded MOF, NJU-Bai62, exhibits excellent
thermal stability up to 450 C, which is comparable to those of
many famous thermostable MOFs based on polynuclear
clusters (nuclearity ≥ 3) or rod-shaped building blocks.
Interestingly, compared with the similar and reported MOF,
NOTT, its thermal stability is significantly higher, and is the
N2 adsorption isotherm was measured at 77 K, as shown in
Figure 3a. NJU-Bai62 exhibits a reversible type-I isotherm. The
Brunauer−Emmett−Teller (BET) and Langmuir surface area of
NJU-Bai62 were estimated to be about 1076.1 and 1150.0 m2 g-
1
,
respectively. Furthermore, the selective adsorption
properties of CO2 over N2 and CH4 for NJU-Bai62 were
conducted at 273 and 298 K (Figure 3b). At 0.15 bar, the uptake
amounts of CO2 are 63.7 and 31.8 cm3 g-1, corresponding to 11.1
and 5.9 wt %, respectively, which are a little bit lower than that
of NJU-Bai77d, (11.8 and 8.0 wt % at 273 and 298 K) and higher
than those of some well-known MOFs, such as ZIF-7811(6.4 and
3.3 wt % at 273 and 298 K), NH2-MIL-53(Al)1f,12 (3.1 wt % at 298
K), Cu-BTTri1313 (2.9 wt % at 298 K), Bio-mof-1114 (5.4 wt % at
298 K), Fe-BTT15 (5.3 wt % at 298 K), HKUST-116 (3.8 wt % at 298
K), and MOF-517 (2.1 and 0.75 wt % at 273 and 298 K). In
addition, at 1 bar, the uptake amounts of CO2 are 130.6 and 91.2
cm3 g-1, corresponding to 20.4 and 15.2 wt %, respectively,
which are higher than the values of most reported Co-MOFs
(Table S7). However, in contrast to CO2, NJU-Bai62 could only
adsorb little N2 (14.3 and 7.1 cm3 g-1, corresponding to 1.8 and
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Belmabkhout, M. Suyetin, P. M. Bhatt, L. J. Weselinski, V. Solovyeva,
highest among the reported MOFs based on binuclear clusters.
Furthermore, NJU-Bai62 shows high CO2 adsorption capacity
and CO2 selectivity and may be a promising candidate for CO2
capture. Our work could open up a new avenue for constructing
robust MOFs from the abundant, unstable, and lower
symmetric binuclear clusters which have usually been ignored
by most MOFs’ chemists.
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K. Adil, I. Spanopoulos, P. N. Trikalitis, A.-H. Emwas and M. Eddaoudi,
DOI: 10.1039/D0CC04543H
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Conflicts of interest
There are no conflicts to declare.
Acknowledgements
We acknowledge Cheung Kong Scholars Program, the Hundred
Talents Program of Shaanxi Province, the National Natural
Science Foundation of China (21771121) for their supports.
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