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DOI: 10.1039/C2RA21474A (Communication) RSC Adv., 2012, 2, 11219-11222

Unique 3D CoII/ZnII-coordination polymers with (3,4,5)-connected self-penetrating topology: Syntheses, topological structures, luminescent and magnetic properties†‡§

Wen-Wen Dong a, Dong-Sheng Li *ab, Jun Zhao a, Ya-Ping Duan a, Liang Bai a and Jing-Jing Yang a
aCollege of Mechanical & Material Engineering, Research Institute of Materials, China Three Gorges University, Yichang 443002, P. R. China
bState Key Laboratory of Coordination Chemistry, Nanjing University, Nanjing 210093, China. E-mail: lidongsheng1@126.com; Fax: +86-717-6397516

Received 17th July 2012 , Accepted 31st August 2012

First published on 18th September 2012

Abstract

Under solvothermal conditions, the reactions of CoII or ZnII acetate with mixed-ligand 3-(pyridin-4-yl)-5-(pyrazin-2-yl)-1H-1,2,4-triazole (4-Hpzpt) and isophthalate (H2ip) afford two isomorphic compounds [M3(ip)2(4-pzpt)2(H2O)]n (M = CoII (1), ZnII (2)), which display a new hepta-nodal (3,4,5)-connected self-penetrating net assembled from 2D {[M3(4-pzpt)2]4+}n 63-hcb layers pillared by [M6(ip)4(H2O)2]4+ subunits, and show antiferromagnetic behavior for 1 and strong fluorescence for 2, respectively.

During the past decade, utilizing pre-designed bridging ligands and metal ions to construct the tailored crystalline materials continues to expand at an alarming rate, in part because of the limitless number of possibilities, but also because of their ability to produce aesthetic structures and desired properties for both industrial applications and fundamental science.1–3 In this context, as excellent chelating and/or bridging ligands, dipyridyl-substituted 1,2,4-triazole derivatives have gained much attention for constructing coordination polymers with interesting properties such as spin crossover behavior, fluorescence, and so on.4–6 However, the research of compounds based on such 1,2,4-triazole derivatives revealed that they have a tendency to form low-dimensional structures, such as mono/binuclear compounds or/and 1D coordination chains.7 Thus, an attractive idea is whether new types of high-dimensional networks can be constructed from such ligands, and if so, what would they be like?

To solve this problem, our synthetic strategy is to design new 1,2,4-triazole derivatives with more terminal coordinated sites and to adopt a mixed-ligand system fusing different polycarboxylates for constructing the high-dimensional coordination polymers. Following the first strategy, we have successfully synthesized a 3D (3,4)-connected CdII-coordination polymer based on a new ligand 3-(pyridin-2-yl)-5-(1H-1,2,4-triazol-3-yl)-1,2,4-triazole, which shows a high thermal stability and strong fluorescence at room temperature.8 In view of the above experience, herein, we choose a 1,2,4-triazole derivative tecton 3-(pyridin-4-yl)-5-(pyrazin-2-yl)-1H-1,2,4-triazole (4-Hpzpt) and isophthalate (H2ip), incorporating different metal ions to acquire new extended high-dimensional architectures. Fortunately, we have isolated two isomorphs [M3(ip)2(4-pzpt)2(H2O)]n (M = CoII (1), ZnII (2)), which present a new hepta-nodal (3,4,5)-connected self-penetrating net constructed from 2D {[M3(4-pzpt)2]4+}n 63-hcb layers linked via [M6(ip)4(H2O)2]4+ subunits.

Compounds 1 and 2 were obtained as red or yellow crystalline materials by the reactions of 4-Hpzpt and H2ip with CoII or ZnII acetate at 160 °C for 3 days under hydrothermal conditions. The compositions were confirmed by elemental analysis and IR spectra, and the phase purities of the bulk samples were identified by powder X-ray diffraction (PXRD, see Fig. S1, ESI†)

Single crystal X-ray analysis (ESI†) reveals that compounds 1 and 2 are isomorphic, and hence only the results of 1 are given in the ensuing discussion. Compound 1 crystallizes in the monoclinic space group P21/n and represents a new 3D (3,4,5)-connected self-penetrating coordination network. The asymmetric unit contains three unique CoII ions, two ip2− anions, two 4-pzpt− ligands and one aqua ligand. As shown in Fig. 1, both Co1 and Co2 lie in octahedral coordination. The Co1 center is bonded to three oxygen atoms (O3, O4 and O7) from two ip2− anions and three nitrogen atoms (N1, N3 and N5) from two 4-pzpt− ligands. While the Co2 center is ligated by four oxygen atoms (O1, O2 O5 and O6) from three ip2− ligands and two 2-pyrazinyl nitrogen atoms (N6 and N7) from two 4-pzpt− ligands. Different from Co1 and Co2, Co3 is surrounded by three nitrogen atoms (N8, N11 and N12) from a pair of 4-pzpt− ligands and one monodentate carboxylate oxygen atom (O8) in the basal plane, and one oxygen atom (O9) of the coordinated water molecule at the apical site, displaying the distorted tetragonal pyramid coordination geometry. The Co–O and Co–N bond distances are consistent with the previously reported values9, ranging from 1.999(4) to 2.275(5) Å and from 2.040(5) to 2.226(4) Å for Co–O and Co–N, respectively (see Table S1, ESI†).


Local coordination environments of Co(ii) ions in 1 with atom labeling of the asymmetric unit; the hydrogen atoms are omitted for clarity. Symmetry codes: #1 (−x + 1, −y, −z + 2); #2 (x, y, z + 1); #3 (x − 1/2, y − 1/2, z + 1/2); #4 (−x + 1, −y, −z + 1); #5 (x, y, z − 1); #6 (x + 1/2, −y − 1/2, z − 1/2).
Fig. 1 Local coordination environments of Co(II) ions in 1 with atom labeling of the asymmetric unit; the hydrogen atoms are omitted for clarity. Symmetry codes: #1 (−x + 1, −y, −z + 2); #2 (x, y, z + 1); #3 (x − 1/2, y − 1/2, z + 1/2); #4 (−x + 1, −y, −z + 1); #5 (x, y, z − 1); #6 (x + 1/2, −y − 1/2, z − 1/2).

In 1, 4-pzpt− anions with μ3-η1:η1:η1:η1 bridging mode link CoII centers into a 2D {[Co3(4-pzpt)2]4+}n 63-hcb layer, and adjacent layers repeat in an –ABAB– stacking sequence (see Fig. 2a,b). Also, ip2− ligands adopt μ3-η1:η1:η1:η1 coordination to bridge CoII centers from adjacent three layers, in which one carboxylate group of ip2− (O3C19O4 or O5C20O6) coordinates in a bidentate chelating pattern, and the other (O1C12O2 or O7C27O8) acts as a syn–anti bidentate bridge, resulting in a CoII-dimer with a Co⋯Co (Co2⋯Co2, Co1⋯Co3) separation of 4.15 Å. In this way, three kinds of separate [Co6(ip)4(H2O)2]4+ subunits are formed by ip2− components joining CoII centers (see Fig. 2c). Furthermore, through sharing CoII centers, these separate [Co6(ip)4(H2O)2]4+ subunits pillar the above-mentioned 2D {[Co3(4-pzpt)2]4+}n 63-hcb layers to construct a complicated 3D network (see Fig. 2d).


Construction of the 3D network for 1: (a) perspective view of the layers A and B with typical 63-hcb topology; (b) the –ABAB– packing structure of 2D{[Co3(4-pzpt)2]4+}n layers; (c) view of the three separate [Co6(ip)4(H2O)2]4+ units; (d) perspective view of the 3D framework. The H atoms are omitted for clarity.
Fig. 2 Construction of the 3D network for 1: (a) perspective view of the layers A and B with typical 63-hcb topology; (b) the –ABAB– packing structure of 2D{[Co3(4-pzpt)2]4+}n layers; (c) view of the three separate [Co6(ip)4(H2O)2]4+ units; (d) perspective view of the 3D framework. The H atoms are omitted for clarity.

To get a better insight into the present 3D framework structure, topological analysis was carried out for 1.10 Each Co1 atom was connected by two 4-pzpt− and two ip2− ligands, hence, it can be considered as a 4-connected node. Comparably, each Co2 atom was linked by two 4-pzpt− and three ip2− ligands. Thus, it can be viewed as a 5-connected node. On the other hand, Co3 atoms, two 4-pzpt− and two ip2− ligands all serve as 3-connected nodes (2 (4-pzpt−) + ip2− for Co3, Co2 + 2Co3 for 4-pzpt1−, 2Co1 + Co2 for 4-pzpt2−, Co1 + Co2 + Co3 for ip12− and Co1 + 2Co2 for ip22−). As a result, the topology of 1 can be described as a rare (3,4,5)-connected hepta-nodal network with the point symbol of (83)2(42·6)(4·82)(82·10)(4·83·102)(42·6·85·10·12) (see Fig. 3a). Notably, this network also displays a self-penetrating pattern, within which nonequivalent 10- and 12-membered shortest rings are catenated and connected in thirty-five different ways, which are summarized in Table S2, ESI†. As shown in Fig. 3b–3i, eight representative Hopf links are formed between 10- and 12-membered shortest rings with different connecting chains and crossing. To our best knowledge, only three (3,4,5)-connected self-penetrating coordination nets have been known to date: 24-nodal (33.42.5.7.83)4(33.42.5.72.82) (33.42.5.83.9)(33.43. 52. 6.7)2(33.43.53.6)4(4.5.72.82)2(4.5.7)2(4.7.8)(4.82)(5.72.86.12)(5.73.85.12)(7.84.10)(7.84.12)(72.83.10)2 net [{Ni6(H2O)10(4,4′-bpy)6}V18O51]·1.5H2O,11a 5-nodal (4.63.8.5.10)(4.82)(63.83)(63)2 net [Cd2(L)2(μ3- SO4)(H2O)2]·5H2O (HL = 3,5-di(1H-imidazol-1-yl)benzoicacid)11b and 3D 3-nodal (7.82)(42.62.72)(42. 6.73. 82.92) net [Cu2(H2L)2(4,4′-bpy)2] (H2L = 1,2,3,4-benzenetetracarboxylic acid).11c Thus, the net in 1 defines a completely new (3,4,5)-connected hepta-nodal self-penetrating net.


The self-penetrating net of 1: (a) the hepta-nodal (3,4,5)-connected (83)2(42·6)(4·82)(82·10)(4·83·102)(42·6·85·10·12) topological net. Perspective views of the ring links between 10- and 12-membered shortest rings within 3D net: (b)10a (red)–12a (lime), (c) 10a (red)–12f (yellow), (d) 10a (red)–12g (cyan), (e) 10a (red)–12h (purple), (f) 10a (red)–12i (blue), (g) 10a (red)–12j (gray), (h) 10g (gold)–12a (lime) and (i) 10g (gold)–12b (deep pink).
Fig. 3 The self-penetrating net of 1: (a) the hepta-nodal (3,4,5)-connected (83)2(42·6)(4·82)(82·10)(4·83·102)(42·6·85·10·12) topological net. Perspective views of the ring links between 10- and 12-membered shortest rings within 3D net: (b)10a (red)–12a (lime), (c) 10a (red)–12f (yellow), (d) 10a (red)–12g (cyan), (e) 10a (red)–12h (purple), (f) 10a (red)–12i (blue), (g) 10a (red)–12j (gray), (h) 10g (gold)–12a (lime) and (i) 10g (gold)–12b (deep pink).

Compounds 1 and 2 are air stable and retain their crystalline integrity under ambient conditions. The TGA curves of 1 and 2 (see Fig. S2, ESI†) are similar due to their isostructural nature. The first weight loss of 1.63% (calculated: 1.86%) in the temperature range 260–330 °C for 1 (255–305 °C for 2: observed, 1.61%; calculated, 1.82%) is attributed to the removal of one lattice water molecule. The remaining substance is stable up to 410 °C for 1 (465 °C for 2). With that, further weight loss indicates the decomposition of the coordination framework.

The magnetic properties of complex 1 per Co in the form of the χMT versus T plot (χM is the molar magnetic susceptibility) are shown in Fig. 4. The thermal evolution of χM−1 obeys the Curie–Weiss law, χM = C/(T − θ) over the whole temperature with a Weiss constant, θ, of −6.52 K and a Curie constant, C, of 2.70 cm3 K mol−1. The χMT value at 300 K is 2.76 cm3 K mol−1, which is much higher than the expected value (1.88 cm3 K mol−1) of one magnetically isolated spin-only CoII ion (S = 3/2, g = 2), indicates that an important orbital contribution is involved.12 As T is lowered, χMT decreases continuously to a value of 1.40 cm3 K mol−1 at 2 K. This behavior indicates a weak antiferromagnetic interaction between the CoII ions in the structure. An attempt has been made to fit the øMT results with the magnetic formula for a mononuclear Co(II) complex, calculating the ì value (spin–orbit coupling parameter) and the A parameter, which gives a measure of the crystal field strength to the interelectronic repulsions, being equal to 1.5 for a weak crystal field and 1.0 for a strong field.13 The formula used is

 
ugraphic, filename = c2ra21474a-t1.gif(1)
where x = λ/kT. The best fit is given in Fig. 4 with λ = −124 cm−1, A = 1.13 and θ = −0.21, close to the value reported for free-ion Co(II) complexes λ = −170 cm−1 and A = 1.32.14 The negative θ value indicates the overall antiferromagnetic coupling between the Co(II) ions. Fig. S3, ESI,† shows the estimate of the antiferromagnetic exchange interaction using the simple phenomenological equation.15


χ M T vs. T (□) and χMvs. T (○) for 1. Solid lines represent the best fit through eqn (1).
Fig. 4 χ M T vs. T (□) and χMvs. T (○) for 1. Solid lines represent the best fit through eqn (1).

The solid-state fluorescent properties of 4-Hpzpt and compound 2 have been investigated in the solid state at room temperature. As indicated in Fig. S4, ESI,† compound 2 exhibits an intense emission peak at ca. 512 nm upon excitation at 360 nm, which means a significant red shift of ca. 117 nm relative to those of the free ligand (λmax(4-Hpzpt) = 395 nm and λmax(H2ip) = 388 nm).16 In light of previous studies, the red shift may be caused by a ligand-to-metal charge-transfer (LMCT) transition,17 and further the emission band is also due to the combined effect of both 4-Hpzpt and H2ip ligands. To further understand the fluorescence properties, the fluorescence quantum yield and lifetime of 2 were investigated, and the results showed that its luminescence lifetime (τ) is fitted to two components by a biexponential decay curve, i.e. τ1 = 11.11 ns, 88%; τ2 = 0.3723 ns, 12%, and it is characterized by a high fluorescence quantum yield (Φfl = 0.4942) in the solid state using an integrating sphere.

In conclusion, we have successfully synthesized two 3D isomorphic CoII/ZnII compounds based on 4-Hpzpt and H2ip co-ligands under hydrothermal conditions, which show a novel (3,4,5)-connected hepta-nodal self-penetrating network. Besides, the magnetic study exhibits that there exist antiferromagnetic interactions in 1, and the high solid-state quantum yield along with the fluorescent emission with obvious red shift of 2 show that they may be good candidates for light-emitting materials. This work prompts us to achieve more high-dimensional functional crystalline solids via such a reliable synthetic route by employing mixed-ligand 4-Hpzpt and other aromatic multicarboxylates as spacers, and further efforts on this perspective are under way.

Acknowledgements

This work was financially supported by the NSF of China (21073106), the IPHPEO (Q20101203), and NSF of Hubei Provinces of China (2010CDB10707 and 2011CDA118). We also thank Dr Bin Liu for a meaningful discussion in magnetic study of complex 1.

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Footnotes

† Electronic supplementary information (ESI) available: Additional structural figures, PXRD, TG curves and luminescence spectra of 1 and 2. CCDC reference numbers 847910 and 873469. For ESI and crystallographic data in CIF or other electronic format see DOI: 10.1039/c2ra21474a
‡ Synthesis of 1. A mixture containing Co(OAc)2·4H2O (0.0249 g, 0.1 mmol), 4-Hpzpt (0.0224 g, 0.1 mmol), H2ip (0.0166 g, 0.1 mmol), and water (10 mL) was sealed in a Teflon-lined stainless steel vessel (25 mL), which was heated at 160 °C for 3 days and then cooled to room temperature at a rate of 3 °C h−1. Red block crystals of 1 were collected in a 59% yield (based on CoII). Elemental analysis (%): calcd for C38H24Co3N12O9: C 47.08, H 2.50, N 17.34; found: C 47.01, H 2.55, N 17.39. IR data (cm−1): 3055 (w), 1609(m), 1571 (s), 1538 (s), 1452(m), 1409 (s), 1150 (w), 1022 (w), 850 (w), 748 (s), 732 (s), 720 (s). Synthesis of 2. 2 was synthesized in a similar way to that described for 1. Yield: 65% (based on ZnII). Elemental analysis (%): calcd for C38H24Zn3N12O9: C 46.15, H 2.45, N 17.00; found: C 46.21, H 2.53, N 17.10. IR data (cm−1): 3060 (w), 1610 (s), 1567 (m), 1551 (s), 1446 (m), 1404 (s), 1149 (w), 1024 (m), 854 (w), 749 (m), 736 (m), 720 (s).
§ Crystal data for 1: C38H24Co3N12O9, M = 969.48, monoclinic, space group P21/n, T = 296(2) K, a = 8.5922(11) Å, b = 34.870(4) Å, c = 12.1899(14) Å, β = 91.989(8), V = 3650.1(8) Å3, Z = 4, Dc = 1.764 g cm−3, reflections collected/unique, 37889/8409 [Rint = 0.1362], R = 0.0679, wR = 0.1278 (I > 2σ(I)), R = 0.1455, wR = 0.1631 (all data), GOF = 1.035.
Crystal data for 2: C38H24Zn3N12O9, M = 988.80, monoclinic, space group P21/n, T = 296(2) K, a = 8.6460(8) Å, b = 35.144(3) Å, c = 12.0483(10) Å, β = 92.381(4), V = 3657.8(5) Å3, Z = 4, Dc = 1.796 g cm−3, reflections collected/unique, 36717/8421 [Rint = 0.069], R = 0.0576, wR = 0.1215 (I > 2σ(I)), R = 0.0855, wR = 0.1342 (all data), GOF = 1.086.
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