Synthesis, Structure and Magnetic Property of a Cobalt(II) Metal-Organic Framework

Article abstract of DOI:10.1002/zaac.201700128

The three-dimensional (3D) porous cobalt(II) metal-organic framework (MOF), [Co₃(L)₂(DMA)₂(MeOH)₂·4(DMA)·6(MeOH)]_n (1) [L = fully deprotonated 2,7-bis(4-benzoic acid)-N-(4-benzoic acid) carbazole, DMA = N,N-dimethylacetamide], was synthesized by hydrothermal reaction. Based on X-ray single-crystal diffraction, structural analysis indicates that complex 1 crystallizes in the monoclinic C2/c space group. Complex 1 possesses a 3,6-connected three-dimensional (3D) topological structure with a point symbol of {4²·6}₂{4⁴·6²·8⁷·10²} when a trinuclear Co^II cluster was regarded as 6-connected node and the organic ligands could be regarded as 3-connected linkers between the 6-connected nodes. The framework structure exhibits a one-dimension (1D) channel with an accessible void of 4223.0 ?³, amounting to 42.8 % of the total unit-cell volume (9862.0 ?³). Moreover, the magnetic properties of complex 1 were studied.

Full text of DOI:10.1002/zaac.201700128

Journal of Inorganic and General Chemistry
DOI: 10.1002/zaac.201700128
ARTICLE
Zeitschrift für anorganische und allgemeine Chemie
Synthesis, Structure and Magnetic Property of a Cobalt(II)
Metal-Organic Framework
Dong-Hui Chen,[a,b] Tian-Lu Sheng,[a] Xiao-Quan Zhu,[a,b] Ling Lin,[a,b] Yue-Hong Wen,[a] Sheng-Min Hu,[a] Rui-
Biao Fu,[a] and Xin-Tao Wu*[a]
Abstract. The three-dimensional (3D) porous cobalt(II) metal-organic
{42·6}2{44·62·87·102} when a trinuclear CoII cluster was regarded as
framework (MOF), [Co3(L)2(DMA)2(MeOH)2·4(DMA)·6(MeOH)]n 6-connected node and the organic ligands could be regarded as 3-con-
(1) [L = fully deprotonated 2,7-bis(4-benzoic acid)-N-(4-benzoic acid) nected linkers between the 6-connected nodes. The framework struc-
carbazole, DMA = N,N-dimethylacetamide], was synthesized by hy-
drothermal reaction. Based on X-ray single-crystal diffraction, struc-
tural analysis indicates that complex 1 crystallizes in the monoclinic (9862.0 Å3). Moreover, the magnetic properties of complex 1 were
ture exhibits a one-dimension (1D) channel with an accessible void of
4223.0 Å3, amounting to 42.8% of the total unit-cell volume
C2/c space group. Complex 1 possesses a 3,6-connected three-dimen-
studied.
sional (3D) topological structure with
a
point symbol of
the synthesis and structure of a three-dimensional (3D) metal-
Introduction
organic
framework,
[Co3(L)2(DMA)2(MeOH)2·4(DMA)·
Metal-organic frameworks (MOFs), assembled from organic
ligands and metal nodes, have generated interests due to their
potential applications in gas storage,[1] separation,[2,3] lumines-
cence sensing,[4,5] and catalysis.[6] Compared with traditional
organic and inorganic materials, MOFs show their flexibility
in tunable structures, internal surface areas, and optical proper-
ties.[7,8] However, the design strategies and synthesize methods
of novel MOFs are still challenged. Selecting suitable ligands,
which should have specific properties, is one of the key to
synthesizing MOFs with desired properties.[9]
Among the variety of organic ligands, carbazole-based li-
gands have attracted massive attention due to their eximious
thermal and photochemical stability, outstanding optical-physi-
cal, and electrochemical properties.[10,11] Carbazole could be
functionalized at (2,7-), (3,6-) and N positions. In order to ob-
tain novel carbazole-based MOFs, (2,7-) and N positions were
functionalized and 2,7-bis(4-benzoic acid)-N-(4-benzoic acid)
carbazole (H3L) was synthesized.[12–19] Compared to function-
alized at 3,6 position, 2,7-carbazole-based ligands have better
fluorescent property and lower bandgap.[20] On the other hand,
functionalized at N positions is beneficial to self-assembling
of the porous MOFs.[21]
6(MeOH)]n (1) [L = fully deprotonated 2,7-bis(4-benzoic
acid)-N-(4-benzoic acid) carbazole, DMA = N,N-dimethylacet-
amide].
Results and Discussion
Crystal Structure of Complex 1
Singe-crystal X-ray diffraction study reveals that complex 1
crystallizes in the monoclinic C2/c space group. Structure
analysis shows that complex 1 is a three-dimensional (3D)
framework. The asymmetric unit possesses two fully deproton-
ated L ligands molecules, a linear trinuclear CoII cluster, two
coordinated DMA molecules, two coordinated methanol mol-
ecule, and several free solvent molecules. As shown in Fig-
ure 1, the three CoII ions in the trinuclear CoII cluster are in
different coordinated environment. CoII(1) is six-coordinate by
six carboxyl oxygen atoms of six L ligands and it is in the
middle of the linear trinuclear CoII cluster. Both CoII(2) and
CoII(2Ј) are five-coordinate by three carboxyl oxygen atoms of
three L ligands, an oxygen atom from a DMA molecule, and
an oxygen atom from a methanol molecule. Meanwhile, depro-
tonated L ligands molecules coordinate with trinuclear CoII
clusters as linkers and the 3D framework of complex 1 is ob-
tained (Figure 2).
Due to the properties of H3L, a stable and rigid tricarboxylic
acid ligand, its solvent thermal reaction with CoII salts pre-
dicted to form a novel porous MOF. Herein, we report
The CoII(1)–O bond lengths are in the range from
1.994(3) Å to 2.176(3) Å. The distances of CoII(2)/CoII(2Ј)–O
range from 2.040(2) to 2.186(2) Å. The O–CoII(1)–O angles
are varying from 83.18(14) to 173.30(14)° and the O–CoII(2)/
CoII(2Ј)–O angles are ranging from 88.43(10) to 180.00(14)°.
The selected bond lengths and bond angles for complex 1 are
listed in Table S2 and Table S3 (Supporting Information).
Complex 1 is a 3D framework with a 1D channel, which
has a diameter of 7.0 Å (Figure 3). A PLATON calculation
* Prof. X.-T. Wu
E-Mail: wxt@fjirsm.ac.cn
[a] State Key Laboratory of Structure Chemistry
Fujian Institute of Research on the Structure of Matter
Chinese Academy of Sciences
Fuzhou 350002, Fujian, P. R. China
[b] University of the Chinese Academy of Sciences,
Beijing, 100049, P. R. China
Supporting information for this article is available on the WWW
under http://dx.doi.org/10.1002/zaac.201700128 or from the au-
thor.
Z. Anorg. Allg. Chem. 2017, 643, 999–1003
999
© 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim

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ARTICLE
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Figure 3. View of 1D channel in complex 1 indicated by a yellow
cylinder.
Topologically, the metal node can be regarded as a 6-con-
nected node and organic ligands can be regarded as a 3-con-
nected linker between the metal nodes. The structure of com-
plex 1 can be described as a 3,6-connected network with a
Schläfli symbol of {42·6}2{44·62·87·102} (Figure 4).[22]
Figure 1. Secondary building units (SBUs) of complex 1.
Figure 4. Topological representation of the 3,6-connected network in
complex 1.
X-ray Powder Diffraction
Powder X-ray diffraction (PXRD) for finely ground powder
samples of complex 1 were carried out at room temperature.
The experimental PXRD pattern corresponds well with the
simulated pattern from the data of single-crystal X-ray diffrac-
tion, as shown in Figure 5.
Thermal Analysis
In order to estimate the thermal stability of complex 1, ther-
mogravimetric analysis (TGA) experiments were carried out
on using polycrystalline samples of complex 1 (Figure 6). The
TGA experiments were performed in a nitrogen atmosphere
with a heating rate of 15 K·min–1 in the range of 30–900 °C.
Figure 2. (a) Coordination environment of the deprotonated L ligand
molecule. (b) Organic ligands connected by SBUs in complex 1.
indicated that the total potential solvent volume when the free For complex 1, a weight loss of 8% from room temperature
solvent molecules are removed is 4223.0 Å3, which corre- to 100 °C is ascribed to the loss of free solvent molecules be-
sponds to 42.80% per unit cell volume (9862.0 Å3).
tween the crystals. From 100 to 170 °C, free solvent molecules
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–1
χM vs. T plot to the Curie-Weiss law results in C =
8.34 cm3·K·mol–1 and θ = –4.38 K. The χMT value of complex
1 keeps steadily from room temperature to 150 K with decreas-
ing temperature. This magnetic behavior is usually the signa-
ture of a paramagnetic effect of CoII metal ions in the frame-
works. Upon cooling, the χMT value of compound 1 rapidly
decreased to a value of 6.49 cm3·K·mol–1 at 7.5 K which may
due to the spin-orbit coupling and/or antiferromagnetic cou-
pling between the three CoII ions. The nearest distances of
Co2+···Co2+ in complex 1 is 3.52 Å. Below 7.5 K, the
χMT value of complex 1 increased abruptly to reach
6.80 cm3·K·mol–1 at 2.5 K, and then decreased to
6.70 cm3·K·mol–1 at 2.0 K, which may be exhibit weak ferro-
magnetic behavior at low temperature between trinuclear CoII
clusters.[26–32] The nearest distances between the trinuclear
CoII clusters in complex 1 is 10.15 Å. The slight irregular vi-
bration of χMT value may be attributed to interference of sys-
tem noise and/or a small amount of impure substance.
Figure 5. Simulated (black), experimental (red) powder X-ray diffrac-
tion (PXRD) patterns for complex 1.
in the 1D channel of the framework were removed generally
with a weight loss of 25%. After that, coordinated DMA and
methanol molecules were detached gradually from 175 to
450 °C with a weight loss of 8%. The framework collapses
and decomposes after 450 °C.
Figure 7. Thermal variation of χM and χMT for complex 1. Insert: plot
–1
of the thermal variation of χM for complex 1.
N2 Adsorption Properties
The N2 adsorption property of complex 1 was measured at
77 K. As shown in Figure S2 (Supporting Information), the
reversible N2 sorption isotherm of complex 1 reveals a type-I
N2 adsorption (25.14 cm3·g–1 at 1 atm) with a Brunnauer-Em-
mett-Teller (BET) surface area of 51.85 m2·g–1. We presume
that the low N2 adsorption may be due to the instability of the
framework during the pretreatment of the BET measurement
in vacuo, which is for removing the solvent molecules (DMA
and MeOH) in the framework.
Figure 6. Thermal analysis curves of complex 1.
Magnetic Properties
The magnetic properties were measured using a crystalline
sample, whose phase purity was confirmed by powder X-ray
diffraction. The temperature-dependent magnetic susceptibility
of complex 1 was investigated in the range of 2–300 K at a
direct current field of 1.0 kOe. As shown in Figure 7, the
χmT value of complex 1 at 300 K is 8.19 cm3·K·mol–1, which
Conclusions
A porous metal-organic framework based on 2,7-bis(4-ben-
is appreciably higher than the expected value zoic acid)-N-(4-benzoic acid) carbazole was synthesized and
(6.81 cm3·K·mol–1) of three isolated spin-only CoII ions (S = characterized. Complex 1 exhibits a 3,6-connected 3D frame-
3/2, g = 2.20).[23–25] As shown in Figure 7, the χM of complex work with an 1D channel. The solvent-accessible volume is
1 obeys the Curie-Weiss law over the whole temperature range. 42.8% of the total unit-cell volume as calculated by PLATON
In the temperature range of 2–300 K, the fit of the curve for software. Magnetic measures show that complex 1 exhibits an
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Journal of Inorganic and General Chemistry
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interesting magnetic transformation property. This MOF can
possibly be utilized as novel porous material.
Experimental Section
Materials and Methods: Ethyl 4-fluorobenzoate, 4,4Ј-dibromobi-
phenyl, potassium tert-butoxide, potassium carbonate, Co(NO3)2·
6H2O, tetrakis(triphenylphosphine)-palladium(0), and solvents were
purchased commercially and used directly without further purification.
As shown in Scheme 1, 2,7-bis(4-benzoic acid)-N-(4-benzoic acid)
carbazole (H3L) was synthesized following the reported procedure.[19]
Elemental analyses (C, H, N) were performed with an Elementar Vario
EL-Cube Element Analyzer. Powder X-ray diffraction (PXRD) data
were collected with a Rigaku MiniFlex 600 diffractometer using Cu-
Kα radiation (λ = 0.154 nm). Thermogravimetric analysis (TGA) ex-
periments were carried out with a NETZSCH STA 449C Jupiter ther-
mogravimetric analyzer in flowing nitrogen with the sample heated in
an Al2O3 crucible from room temperature to 1000 °C at a heating rate
of 10 K·min–1. Infrared spectra were recorded with KBr pellets in the
range 4000–400 cm–1 with a Perkin-Elmer Spectrum One FT-IR spec-
trometer. Magnetic susceptibilities of crystalline samples were mea-
sured with a Quantum Design MPMS-XL SQUID susceptometer under
an applied magnetic field of 1 kOe in the 2–300 K range. Diamagnetic
corrections were made using Pascal’s constants.[33] The N2 sorption
isotherm of complex 1 was measured with a Micromeritics ASAP 2020
surface area and porosimetry analyzer at 77 K.
Figure 8. (a) Synthesis of complex 1. (b) Crystals photo of complex
1.
Crystal Structure Determination: A plum block crystal of complex
1 was selected carefully and glued on the top of a thin glass fiber for
single-crystal X-ray diffraction data collection. The data were collected
with a Rigaku Saturn 724HG CCD diffractometer (Mo Kα radiation λ
= 0.71073 Å graphite-monochromator) at 293(2) K. The structure was
solved by direct methods and refined by full-matrix least-squares of
F2 using the SHELX-97 program.[34] Hydrogen atoms were added in
their idealized positions and refined using a riding model. The
SQUEEZE routine of the PLATON software suite was used in remov-
ing highly disordered solvent molecules. The final formulas were cal-
culated according to the Squeeze results combined with the results
from thermogravimetric analysis (TGA) and elemental analyses
(EA).[35,36] A total of 49968 reflections of complex 1 were collected
in the range of 2.06 Ͻ θ Ͻ 27.49° (–33 Յ h Յ 39, –21 Յ k Յ 21,
–28 Յ l Յ 28) and 11281 were independent with Rint = 0.0415. The
2
final R = 0.0668 and wR = 0.2071 (w = 1/[σ2(Fo ) + (0.1339P)2
Scheme 1. Synthesis of 2,7-bis(4-benzoic acid)-N-(4-benzoic acid)
carbazole (H3L).
2
2
+12.3872P], where P = (Fo + 2Fc )/3). S = 1.07, (Δ/σ)max Ͻ 0.001,
Δρmax = 1.78 e·Å–3, Δρmin = –1.06 e·Å–3. Crystal data and structure
refinements are listed in Table 1. Selected bond lengths and bond
angles for complex 1 are summarized in Table S1 and Table S2 (Sup-
porting Information).
Synthesis of [Co3(L)2(DMA)2(MeOH)2·4(DMA)·6(MeOH)]n (1): A
solution of H3L (0.026 g, 0.05 mmol) in DMA (1.5 mL) was directly
mixed with a solution of Co(NO3)2·6H2O (0.058 g, 0.2 mmol) in meth-
anol (0.5 mL) at room temperature. The mixture was sealed in a 10 mL
Teflon-lined autoclave and heated at 80 °C for 96 h. After cooling to
room temperature at a speed of 3 K·h–1, purple block crystals were
collected (yield: 45% based on H3L) (Figure 8). Co3C98H122N8O26:
calcd.: C 58.7, H 6.13 N 5.58%; found: C 58.8, H 6.12, N 5.58%.
The UV/Vis spectrum of complex 1 is shown in Figure S1 (Supporting
Information). IR (KBr): ν˜ = 3594 (w), 3067 (w), 3038 (w), 2926 (w),
1604 (vs), 1547 (s), 1510 (m), 1398 (vs), 1328 (m), 1255 (m), 1182
Crystallographic data (excluding structure factors) for the structure in
this paper have been deposited with the Cambridge Crystallographic
Data Centre, CCDC, 12 Union Road, Cambridge CB21EZ, UK.
Copies of the data can be obtained free of charge on quoting the de-
pository number CCDC-1544683 (Fax: +44-1223-336-033; E-Mail:
deposit@ccdc.cam.ac.uk, http://www.ccdc.cam.ac.uk).
Supporting Information (see footnote on the first page of this article):
(m), 1142(w), 1106 (w), 1015 (m), 947 (w), 853 (m), 819 (w), 783 (s), Additional selected bond lengths and angles, UV/Vis spectrum and N2
740 (m), 709 (w), 653 (w), 597 (w), 562 (w), 484 (m) cm–1.
isotherm volume.
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Journal of Inorganic and General Chemistry
ARTICLE
Zeitschrift für anorganische und allgemeine Chemie
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Empirical formula
Formula weight
Crystal system
Space group
a /Å
b /Å
c /Å
α /°
β /°
Co3C98H122N8O26
2004.84
monoclinic
C2/c
30.220(6)
16.499(3)
21.605(4)
90
113.720(2)
90
9863(3)
γ /°
V /Å3
Z
4
Temperature /K
D /Mg·m–3
μ /mm–1
F(000)
293(2)
0.986
0.55
3020
0.0668,0.2071
2.06 to 27.51
0.0415
–33 Յ h Յ 39
–21 Յ k Յ 21
–28 Յ l Յ 28
1.072
R1a),wR2b)[I Ͼ 2σ(I)]
θ ranges /°
R(int)
h k l ranges
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Acknowledgements
The authors gratefully acknowledge financial support from the
National Natural Science Foundation of China (21233009 and
21203194), the 973 Program (2014CB845603), the Strategic Priority
Research Program of the Chinese Academy of Sciences, Grant No.
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Keywords: 2,7-Bis(4-benzoic acid)-N-(4-benzoic acid) carb-
azole; Cobalt; Magnetic properties; Porous CoII metal-organic
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Received: April 23, 2017
Published Online: July 17, 2017
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