Two zinc coordination polymers showing five-fold interpenetrated diamondoid network and 2D → 3D inclined polycatenation motif

Article abstract of DOI:10.1016/j.inoche.2014.02.051

The reaction of Zn(NO₃)₂, 1,4-bis(1,2,4-triazol-4-yl) benzene (btx), 1,4-benzenedicarboxylicate (1,4-bdc) or fumarate (fum) gives two unusual coordination polymers {[Zn(btx)(1,4-bdc)] 3H₂O}_n (1) and [Zn(btx)_0.5(fum)(H₂O)]_n (2). 1 shows a 5-fold interpenetrated three-dimensional diamondoid network. 2 displays a 2D → 3D inclined polycatenation motif consisting of two sets of equivalent 2D (6,3) layers. The luminescence and thermal stability were investigated.

Full text of DOI:10.1016/j.inoche.2014.02.051

Inorganic Chemistry Communications 44 (2014) 41–45
Contents lists available at ScienceDirect
Inorganic Chemistry Communications
journal homepage: www.elsevier.com/locate/inoche
Two zinc coordination polymers showing five-fold interpenetrated
diamondoid network and 2D → 3D inclined polycatenation motif
a
Yan-Fen Peng a,b, Ling-Yun Zheng a, Shan-Shan Han a, Bao-Long Li a, , Hai-Yan Li
⁎
a
Key Laboratory of Organic Synthesis of Jiangsu Province, College of Chemistry, Chemical Engineering and Materials Science, Soochow University, Suzhou 215123, PR China
b
Department of Material and Chemical Engineering, Chizhou University, Chizhou, Anhui 247000, PR China
a r t i c l e i n f o
a b s t r a c t
Article history:
The reaction of Zn(NO3)2, 1,4-bis(1,2,4-triazol-4-yl)benzene (btx), 1,4-benzenedicarboxylicate (1,4-bdc) or fuma-
rate (fum) gives two unusual coordination polymers {[Zn(btx)(1,4-bdc)] 3H2O}n (1) and [Zn(btx)0.5(fum)(H2O)]n
(2). 1 shows a 5-fold interpenetrated three-dimensional diamondoid network. 2 displays a 2D → 3D inclined
polycatenation motif consisting of two sets of equivalent 2D (6,3) layers. The luminescence and thermal stability
were investigated.
Received 14 January 2014
Accepted 28 February 2014
Available online 12 March 2014
Keywords:
Diamondoid network
Polycatenate
© 2014 Elsevier B.V. All rights reserved.
5-Fold interpenetrated
Zinc coordination polymer
Luminescence
In recent years, more and more chemists were involved into rational
design and synthesis of coordination frameworks because of their fasci-
nating topology structures and attentional properties such as lumines-
cence, catalysis and gas absorption [1–13]. In order to get such
intriguing topologies and functional materials, the crucial step is to em-
ploy appropriate organic building blocks as well as metal ions. Auxiliary
multicarboxylate ligands can influence the structure of the coordination
polymers owing to the fact that they can satisfy charge-balance and even
mediate the coordination of the metal centers, and more importantly
they can provide diverse ligands and versatile coordination modes
[14–18]. Flexible bidentate N-donor ligands such as bis(imidazole) [19,
20] and 1-substituted bis(triazole) [21–25] ligands are widely used to
construct coordination polymers because flexible ligands can adopt dif-
ferent conformations according to the geometric needs of the different
metal ions. Meanwhile many coordination networks are particularly
intriguing because of the presence of periodic entanglements, in
which independent motifs are entangled together in different modes.
Interpenetrating and polycatenation networks are two main sub-
groups of entanglements which need to break internal connections
to separate the individual nets [26–34]. Two entanglements showing
interesting 2D → 3D inclined polycatenation based on 2D (4,4) network
are synthesized recently [31,32]. We synthesized two interesting
entanglements [2D-Mn(btb)2(NCS)2][1D-Mn(btb)2(NCS)2] and
[Cd3(bbtz)6(H2O)6](BF4)6·1.75H2O showing 2D (4,4) networks and
1D ribbons of rings polycatenated in a three-dimensional (3D)
array [33,34].
In previous work, we synthesized a lot of coordination polymers
using flexible 1-substituted bis(triazole) building blocks, such as 1,2-
bis(1,2,4-triazol-1-yl)ethane (bte) [35,36], 1,3-bis(1,2,4-triazol-1-yl)
propane (btp) [37], 1,4-bis(1,2,4-triazol-1-yl)butane (btb) [38] and
1,4-bis(1,2,4-triazol-1-ylmethyl)benzene (bbtz) [39]. In contrast to 1-
substituted-1,2,4-triazole derivatives, the research of coordination
polymers based on 4-substituted-1,2,4-triazole derivatives is only just
the beginning [40,41]. We also achieved a series of fantastic frameworks
based on flexible 4-substituted-1,2,4-triazole ligand 1,2-bis(1,2,4-
triazol-4-yl)ethane (btre) (Scheme 1) [42–44], such as {[Cd(btre)
Cl]·OH}n, {[Cd(btre)Cl][CdCl(dca)2]·0.5H2O}n and {[Zn(btre)0.5(OH-
bdc)(H2O)2]·1.5H2O}n.
The 4-substituted-1,2,4-triazole bridging ligand 1,4-bis(1,2,4-triazol-
4-yl)-benzene (btx) (Scheme 1) should be a good rigid building block to
construct coordination polymers with large channels and easily result to
entanglements. In the present work, two entangled coordination poly-
mers {[Zn(btx)(1,4-bdc)]•3H2O}n (1) and [Zn(btx)0.5(fum)(H2O)]n (2)
(1,4-bdc = 1,4-benzenedicarboxylicate, fum = fumarate) were synthe-
sized. 1 shows a five-fold interpenetrate 3D diamond network. 2 displays
a 2D → 3D inclined polycatenation framework consisting of two sets of
equivalent 2D (6,3) layers.
The colorless block crystals of 1 and 2 were prepared by the reaction
of Zn(NO3)2, btx and 1,4-bdc or fum [45]. Single-crystal X-ray analysis
[46] revealed that 1 crystallizes in the triclinic system with Pī space
group. The Zn(II) atom is coordinated by two btx nitrogen atoms and
three carboxylate oxygen atoms from two 1,4-bdc ligands in a distorted
trigonal bipyramidal geometry (Fig. 1). There are two kinds of 1,4-bdc
ligands. Two carboxylate groups (O1O2) of one kind of 1,4-bdc ligands
act as bis-chelating mode. Two carboxylate groups (O3O4) of the
⁎
Corresponding author. Tel.: +86 512 65880324; fax: +86 512 65880089.
E-mail address: libaolong@suda.edu.cn (B.-L. Li).
http://dx.doi.org/10.1016/j.inoche.2014.02.051
1387-7003/© 2014 Elsevier B.V. All rights reserved.

42
Y.-F. Peng et al. / Inorganic Chemistry Communications 44 (2014) 41–45
N
N
N
N
N
N
btre
N
N
N
N
N
N
btx
Scheme 1. The ligands btx and btre.
Fig. 3. A single diamondoid network of 1.
all the shortest circuits are displayed as six-numbered circuits with
chair form (Fig. 4) if the Zn(II) atoms are simplified as 4-connected
nodes and the btx ligands and 1,4-bdc ligands as 2-connected linkers
[47]. Because the single diamondoid network has large spacious voids,
it allows adjacent frameworks to interpenetrate to give a 5-fold
interpenetrated three-dimensional diamondoid network (Fig. S1). The
degrees of the diamondoid net interpenetration ranging from 2- to
11-fold are well-known and have been reported [48], but the 5-fold in-
terpenetrating MOFs in the presence of the mixed organic ligands with
different lengths is relatively rare [49,50]. The lattice water molecules
exist in the voids of the 5-fold interpenetrating diamondoid network
of 1 (Fig. 5).
Fig. 1. The coordination environment of the Zn(II) atom in 1 (Symmetry codes: A −x,
2 − y, −z; B −1 − x, −y, 1 − z; C 1 − x, −y, −z; D 1 − x, 1 − y, 1 − z.).
2 crystallizes in the monoclinic system with P21/c space group. The
Zn(II) atom is coordinated by one btx nitrogen atom and two fum oxy-
gen atoms and one coordination water oxygen atom in a distorted tetra-
hedral geometry (Fig. 6). All fum ligands act as bidentate bridging
ligands and link two Zn(II) atoms with the Zn⋯Zn distances of
8.959(2) and 9.334(2) Å. The btx ligands adopt bidentate mode and
join two Zn(II) atoms with the Zn⋯Zn distance of 13.499(2) Å.
Each zinc(II) links three zinc(II) atoms through one btx and two fum
ligands and extends to form a 2D (6,3) network (Fig. 7). The edges of the
rectangular windows of the layers measure 16.487 × 13.499 Å, as
other kind of 1,4-bdc ligands exhibit bis-monodentate mode. The btx
ligands adopt bidentate mode. The Zn⋯Zn distances bridged by 1,4-
bdc ligands are 10.916(2) and 11.097(2) Å. The Zn⋯Zn distances sepa-
rated by btx ligands are 13.712(3) and 13.533(2) Å.
Each Zn(II) center connects four Zn(II) centers through two btx and
two 1,4-bdc bridges in a tetrahedral mode (Fig. 2) and extends to con-
struction of a three-dimensional network (Fig. 3). The topological anal-
ysis of 1 has been performed by considering both the metal ion and the
ligand as topological nodes. The individual three-dimensional motif can
be simplified as a four-connected 66 diamondoid topological net where
Fig. 2. Schematic plot of a single adamantanoid cage of 1.
Fig. 4. Schematic depiction of a single diamondoid network of 1.

Y.-F. Peng et al. / Inorganic Chemistry Communications 44 (2014) 41–45
43
Fig. 5. Schematic depiction of a 5-fold interpenetrated diamondoid network in 1 (showing the lattice water molecules).
bond interactions between the coordination water molecules and car-
boxylate oxygen atoms (O5⋯O2 (−x + 1, −y + 1, −z) 2.652(3) Å,
O5⋯O4 (x, −y + 1/2, z + 1/2) 2.657(3) Å).
The measured and simulated PXRDs confirm the purity of 1 and 2
(Figs. S2, S3). Due to the excellent fluorescent properties of d10 metal
complexes, the solid state photoluminescent properties of 1, 2 and the
free btx ligand were investigated at room temperature. The btx displays
the emission band at 432 nm upon excitation at 370 nm, which can
probably be assigned to the π–π* transitions [51]. 1 exhibits the emis-
sion band maximum at 394 nm and a shoulder peak at 454 nm, upon ex-
citation at 345 nm (Fig. 10). No emission of 2 was observed at the same
experimental condition. Because the Zn(II) ion is difficult to oxidize or
to reduce due to the d10 configuration, the emissions are neither
metal-to-ligand charge transfer (MLCT) nor ligand-to-metal charge
transfer (LMCT) [52]. The emissions at 394 and 454 nm can be tentative-
ly attributed to the intraligand charge transition for 1,4-bdc and btx, re-
spectively [51–53], because the emission at 394 nm for 1 is near to that
of 1,4-bdc (388 nm) [49]. The emission at 454 nm for 1 shows the obvi-
ous red shift (22 nm) compare to free btx ligand.
The thermal stability of the coordination polymers 1 and 2 was ex-
amined by thermogravimetric analysis (TG) in dry nitrogen atmosphere
from 20 to 800 °C. In the TG curve of 1 (Fig. S4), the lattice water mole-
cules were lost from 45 to 180 °C (Calcd.: 10.90%, found: 10.76%). The
anhydrous substance is stable upon heating to 335 °C. Then the weight
decrease continuously happened and did not end until 600 °C. The coor-
dination water molecules of 2 were lost from 50 to 170 °C (Calcd.: 5.94%,
found: 5.96%). The anhydrous substance is stable upon heating to
Fig. 6. The coordination environment of the Zn(II) atom in 2.
defined by Zn⋯Zn distances; these layers are nearly rectangular in
shape, with Zn⋯Zn⋯Zn angles of 77.34° and 102.66°.
The interesting feature of the structure is that two sets of layers par-
allel pack with the angle of 43.1° between two sets of parallel layers. In
Fig. 8, a parallel layer set is shown in blue, while one layer of the other
different parallel layer set is displayed in pink. Two sets of layers cate-
nate to each other form a 2D + 2D → 3D parallel/parallel inclined
polycatenation motif (Fig. 9). Although 2D (6,3) network is rather com-
mon, the 2D + 2D → 3D parallel/parallel inclined polycatenation is un-
usual [31,32]. There are no direct covalent interactions between
catenated layers. The catenated motif is stable through the hydrogen
Fig. 7. A two-dimensional (6,3) network in 2.
Fig. 8. Schematic perspective of parallel/parallel inclined polycatenation motif in 2.

44
Y.-F. Peng et al. / Inorganic Chemistry Communications 44 (2014) 41–45
retrieving.html, or from the Cambridge Crystallographic Data Center,
12 Union Road, Cambridge CB2 1EZ, UK; fax: (+44) 1223-336-033; or
e-mail: deposit@ccdc.cam.ac.uk. Supplementary data associated with
this article can be found, in the online version, at http://dx.doi.org/10.
1016/j.inoche.2014.02.051.
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This work was supported by the Natural Science Foundation of China
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