ARTICLE pubs.acs.org/crystal
An Interpenetrating Architecture Based on the WellsDawson Polyoxometalate and AgI 3 3 3 AgI Interactions Peng-peng Zhang,† Jun Peng,*,† Hai-jun Pang,† Jing-quan Sha,‡ Min Zhu,† Dan-dan Wang,† Ming-guan Liu,† and Zhong-min Su† †
Key Laboratory of Polyoxometalate Science of Ministry of Education, Faculty of Chemistry, Northeast Normal University, Changchun, Jilin 130024, P. R. China ‡ The Provincial Key Laboratory of Biological Medicine Formulation, School of Pharmacy, Jiamusi University, Jiamusi, 154007, P. R. China
bS Supporting Information ABSTRACT: A new compound based on the WellsDawson polyoxometalate, Ag7(bbi)5(OH)(P2W18O62) (bbi = 1,10 -(1,4butanediyl)bis(imidazole)) (1), has been hydrothermally synthesized and characterized by the normal physical methods and single-crystal X-ray diffraction. Compound 1 represents the first interpenetrating framework based on the WellsDawson POMs. The AgI 3 3 3 AgI interactions are crucial in the formation of the two individual motifs: in the first interpenetrating motif, the supported {Ag2}2þ dimers and the P2W18 polyanions form an infinite inorganic chain, then the Agþ monomers and bbi ligands extend the chain to form a three-dimensional framework. The second motif is constructed by the Agbbi meso-helix chains which are stitched by the unsupported Ag7 3 3 3 Ag7 dimers to form a twodimensional layer with huge loops. The electrochemical study exhibits that compound 1 could be used as electrocatalyst in the electrical reductions of bromate. In addition, compound 1 shows a photocatalytic action for degradation of RhB.
’ INTRODUCTION Interpenetrating frameworks are described as architectures which cannot be separated except if one of the individual motifs is broken.1 In their complicated architectures, supramolecular connections (such as electrostatic interaction, hydrogen bond, ππ stacking, and cationπ interactions) among the individual motifs endow them with structural flexibility, which is important in the applications of gas storage, conductivity, biological chemistry, and so on.2 Interpenetration is a subclass of entangled system studied extensively and developed rapidly nowadays. Individual motifs of the interpenetrating architectures are from two-dimensional (2D) nets to three-dimensional (3D) frameworks, and the number of interpenetrating units varies from 2 to 10.3 Ongoing research in interpenetration focuses on the introduction of functional groups with available characters. Polyoxometalates (POMs) are early transition metal oxide clusters composed of Mo, W, V, Nb, and so on. POMs show a wide variety of interesting structural motifs with different sizes and topologies. Besides the classical Keggin, WellsDawson, Anderson, Waugh, Silverton, and Lindqvist types, many new structures have been found, such as closed cages, Wheels, dimeric anions, and transition-metal-centered heteropolyoxometalates.4 POMs are in the nanosize scale and have abundant surface oxygen atoms, which make them excellent inorganic building blocks. In addition, POMs bear versatile properties in such fields r 2011 American Chemical Society
as catalysis, photochemistry, magnetism, electrochemistry, and biochemistry.5,6 Accordingly, POM-based interpenetrating compounds will not only show aesthetic architectures but also possess both properties of flexibility of interpenetration and versatile functions of POMs.7 However, to obtain such compounds is difficult as the nanosized POMs with a big steric hindrance would inhibit the formation of interpenetration. Agþ ion is a prominent metal linker in the POM-based metal organic frameworks (MOFs), for it not only possesses abundant coordination modes such as linear, T-type, “seesaw”, “squarepyramidal”, “trigonal-bipyramidal” and octahedral geometries8 but also is useful in the areas of catalysis, biological chemistry, and so on.9 In addition, the argentophilicity of Agþ ions may conduce the formation of {Ag2}2þ dimers, which may play a key role in the expansion of multiple dimensional structures. {Ag2}2þ dimers acting as linkers can be classified into unsupported and supported ones according to their coordination modes; that is, two Agþ ions in an unsupported {Ag2}2þ dimer are fused only by AgI 3 3 3 AgI interaction, while those in a supported {Ag2}2þ dimer are connected not only by AgI 3 3 3 AgI interaction but also by Received: September 21, 2010 Revised: April 2, 2011 Published: May 09, 2011 2736
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Scheme 1. Illustrations of the Unsupported (a) and Supported (b) {Ag2}2þ Dimers
Table 1. Crystal Data and Structure Refinements for Compound 1 compound
10
’ EXPERIMENTAL SECTION Materials and General Methods. All reagents were purchased commercially and used without further purification. R-K6P2W18O62 3 15H2O and bbi were prepared according to the reported procedure and verified by IR spectrum.12 Elemental analyses (C, H, and N) were performed on a Perkin-Elmer 2400 CHN elemental analyzer. The IR spectrum was obtained on Alpha Centaurt FT/IR spectrometer with KBr pellet in the 4004000 cm1 region. The solid UVvis absorption was carried out on a Cary 500 spectrophotometer. The thermal gravimetric analyses (TGA) were carried out in flowing N2 on a Perkin-Elmer DTA 1700 differential thermal analyzer with a rate of 10.00 °C/min. The X-ray powder diffraction (XRPD) patterns were recorded on a Siemens D5005 diffractometer with Cu KR (λ = 1.5418 Å) radiation. Cyclic voltammograms were obtained with a CHI 660 electrochemical workstation at room temperature. Platinum gauze was used as a counter electrode and Ag/AgCl electrode was referenced. Chemically bulk-modified carbon paste electrode (CPE) was used as working electrode. The photocatalytic activity was tested by a 756 CRT UVvis spectrophotometer. Synthesis of Ag7(bbi)5(OH)(P2W18O62) (1). A mixture of R-K6P2W18O62 3 15H2O (2 g, 0.4 mmol), AgNO3 (0.17 g, 1 mmol), bbi (0.4 g, 1 mmol), and NH4VO3 (0.12 g, 0.1 mmol) were dissolved in 10 mL of distilled water at room temperature. When the pH of the mixture was adjusted to about 7.1 with 1.0 mol L1 NaOH, the suspension was put into a Teflon-lined autoclave and kept under autogenous pressure at 160 °C for 4 days. After slow cooling to room temperature, yellow block crystals were filtered and washed with distilled water (50% yield based on Ag). Anal. Calcd for C50H71Ag7N20O63P2W18 (6086.34): C 9.87, H 1.12, N 4.60. Found: C 9.89, H 1.15, N 4.64. IR (solid KBr pellet, cm1): 3139 (w), 1690 (m), 1655 (m), 1519 (s), 1420 (w), 1344 (w), 1274 (w), 1225 (m), 1140 (w), 1087 (s), 954 (m), 909 (m), 783(s). Preparation of 1CPE. Compound 1 modified carbon paste electrode 1CPE was prepared as follows: 90 mg of graphite powder and 8 mg of compound 1 were mixed and ground together by agate
formula
C50H71Ag7N20O63P2W18
fw T (K)
6086.34 293(2)
crystal system
triclinic
space group
P1
a (Å)
15.6160(12)
b (Å)
17.3650(13)
c (Å)
19.9620(15)
R (o)
75.8130(10)
β (o) γ (o)
89.4680(9) 76.0360(9)
V (Å3)
5085.8(7)
Z
2
Dc (g 3 cm3)
21.707
F(000)
5410.0
final R1a, wR2b [I > 2σ(I)]
0.0442, 0.1325
final R1a, wR2b (all data) GOF on F2
0.0595, 0.1512 0.993
R1 = ∑ Fo||Fc /∑|Fo|. b wR2 = {∑[w(Fo2 Fc2)2]/∑[w(Fo2)2]}1/2. )
a
3.974
μ (mm1)
)
other bridging groups (Scheme 1). Recently, chemists have synthesized several POM-based compounds containing {Ag2}2þ dimers.11 In most of these compounds, the {Ag2}2þ dimers adopt the supported mode which is achieved by coordination of polyanions or organic ligands. A typical unsupported example is [Ag(CH3CN)4]⊂{[Ag(CH3CN)2]4[H3W12O40]},11a in which the {Ag2}2þ dimers joint the discrete segments to form a 3D architecture. Herein, we describe a new compound, Ag7(bbi)5(OH)(P2W18O62) (1), obtained by combination of WellsDawson POM, Agþ ion and the organic ligand bbi, in which the AgI 3 3 3 AgI interactions are crucial in the formation of the interpenetrating architecture. Unlike the examples mentioned above, the {Ag2}2þ dimers in compound 1 adopt both the supported and unsupported modes. Compound 1 represents the first interpenetrating framework based on the WellsDawson POMs and AgI 3 3 3 AgI interactions.
1
mortar and pestle to achieve a uniform mixture, and then 0.1 mL nujol was added with stirring. The homogenized mixture was packed into a glass tube with 1.5 mm inner diameter, and the tube surface was wiped with paper. Electrical contact was established with copper rod through the back of the electrode. Ag/AgCl (3 M KCl) electrode was used as a reference electrode, and a Pt wire as a counter electrode. Photocatalytic Reaction. Powder of 60 mg compound 1 was dispersed into a 1.0 105 mol/L RhB aqueous solution. The solution was stirred in the dark for 30 min to ensure the establishment of adsorption equilibrium before irradiation. Then 3 mL aliquot was sampled and then centrifuged to remove the catalyst. The RhB concentration (C0) was determined by measuring the maximum absorbance at 554 nm as a function of irradiation time using a 756 CRT UVvis spectrophotometer. Then UV spectra of the solutions were recorded after irradiated by two 4-W UV lamps with λmax = 365 nm (Philips, TUV 4 W/G4T5) for 2 h, which gave the corresponding RhB concentration. X-ray Crystallographic Study. X-ray diffraction analysis data for compound 1 were collected on a Bruker SMART-CCD diffractometer, with MoKR monochromatic radiation (λ = 0.71073 Å) at 293 K. The structure was solved by direct methods and refined on F2 by full-matrix least-squares methods using the SHELXTL package.13 Hydrogen atoms attached to water molecules were not located but included in the structure factor calculations. A summary of the crystallographic data and structural determination for them is provided in Table 1. Selected bond lengths and angles of compound 1 are listed in Tables S1 (Supporting Information). Crystallographic data for the structure reported in this paper have been deposited in the Cambridge Crystallographic Data Center with CCDC number of 775926.
’ RESULTS AND DISCUSSION Crystal Structure of Compound 1. Single crystal X-ray structural analysis reveals that compound 1 consists of R-[P2W18O62]6 (abbreviated as P2W18) polyanions, Agþ monomers, {Ag2}2þ dimers, bbi ligands, and hydroxyl14 (Figure 1). P2W18 polyanion 2737
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Figure 3. The coordination modes of the three kinds of bbi ligands in compound 1.
Figure 1. Stick/polyhedral view of the coordination fashions of the P2W18 polyanion, Agþ ions, {Ag2}2þ dimers, and bbi ligands. The hydrogen atoms and hydroxyls are omitted for clarity.
Figure 2. Coordination modes of (a) the supported Ag1 3 3 3 Ag9 dimer, (b) the supported Ag2 3 3 3 Ag2 dimers, and (c) the unsupported Ag7 3 3 3 Ag7 dimer.
contains two [R-A-PW9O34]9 units derived from the R-Keggin polyanion by removal of a set of three corner-shared WO6 octahedra.15 The PO and WO lengths are in the normal ranges. Selected bond lengths and angles are listed in Table S1, Supporting Information. In compound 1, each P2W18 polyanion acts as a penta-dentate ligand coordinating with five Agþ ions. There are nine crystallographically unique Agþ ions, Ag1 to Ag9. In the structure, the distances between Ag1 and Ag9, Ag2 and Ag2, Ag7 and Ag7 are 3.163, 3.152, and 3.312 Å, respectively, which are shorter than the van der Waals radii of two silver atoms (3.44 Å).16 Therefore, the Agþ ions could be classified into two kinds: the Agþ monomer (Ag3, Ag4, Ag5, Ag6, and Ag8) and the {Ag2}2þ dimer (Ag1 3 3 3 Ag9, Ag2 3 3 3 Ag2, and Ag7 3 3 3 Ag7). The Agþ monomers all adopt a linear coordination mode by coordinating with two nitrogen atoms from two bbi ligands. In the {Ag2}2þ dimers, Ag2 coordinates with two oxygen atoms from two P2W18 polyanions and one nitrogen atom from a bbi ligand; Ag7 coordinates with two nitrogen atoms from two bbi ligands; Ag9 coordinates with three oxygen atoms from two P2W18 polyanions and one nitrogen atom from a bbi ligand. The coordination mode of Ag1 is unique in that it further coordinates with two carbon atoms through weak Agþπ interactions (Ag1 3 3 3 C10 = 2.374(19) Å and Ag1 3 3 3 C50 = 2.437(18) Å), besides one oxygen atom from the P2W18 polyanion and one nitrogen atom from the bbi ligand.17 As a result, the Ag1 3 3 3 Ag9 dimer is supported by a bbi ligand and a P2W18 polyanion, and the Ag2 3 3 3 Ag2 dimer is supported by two P2W18 polyanions. The Ag7 3 3 3 Ag7 dimer is unsupported (Figure 2). The bbi ligands can be divided into three kinds according to their coordination fashions and the number of Agþ ions attached: Type a, two terminal nitrogen atoms coordinate to two Agþ ions;
Figure 4. (a) The 3D framework of compound 1. (b) The 1D P2W18 chain connected with the supported {Ag2}2þ (Ag1 3 3 3 Ag9 and Ag2 3 3 3 Ag2) dimers. The bbi ligands are shown in purple sticks.
Type b, like Type a, but an imidazole group additionally coordinates with a third Agþ ion through Agþπ interaction; Type c, one terminal nitrogen atom coordinates to a Agþ ion, and the other one to a {Ag2}2þ dimer18 (Figure 3). The whole structure of compound 1 shows an interpenetrating architecture composed of two independent motifs, a 3D framework, and a 2D layer. In the 3D framework motif, the P2W18 polyanions are linked by the supported {Ag2}2þ dimers (Ag1 3 3 3 Ag9 and Ag2 3 3 3 Ag2) through WOAg bonds, to form a one-dimensional (1D) {Ag2}2þP2W18 chain (Figure 4b). The 1D chains are further extended to a 2D layer (layer {Ag2}2þP2W18Ag4) via horizontal connections of Ag4bbi segments, and then the 2D layers are connected to a 3D framework by the longitudinal extension of Ag5bbi segments (Figure 4a). In the 2D layer motif, first, bbi and Agþ bond together in the order of 3 3 3 Ag3bbiAg8bbiAg3bbi Ag7bbiAg6bbiAg7 3 3 3 , to form a meso-helix chain (Figure 5).19 Furthermore, these chains are stitched to a 2D layer with loops by the unsupported Ag7 3 3 3 Ag7 dimers. Of particular note are the loops, each of which is composed of 14 Agþ and 12 bbi (Figure 6), and this is quite unusual in coordination polymers or in POM-based compounds. The huge loop is alternately threaded by the staff of {Ag2}2þP2W18 and the staff of Ag4bbi from three grid layers of {Ag2}2þP2W18Ag4 (Figure 7). As a result, a 2D þ 3D interpenetrating framework is formed (Figure S1, Supporting Information). Discussion of the Structural Features of Compound 1. In POM chemistry, more and more examples of interpenetrating structure have been reported. They could be sorted to three types 2738
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Figure 5. (a, b) The meso-helix chain in compound 1, the hydrogen atoms are omitted for clarity. (c) Perspective view of the meso-helical chain along the chain direction.
Figure 8. The cyclic voltammogram of the 1CPE in 1 M H2SO4 at different scan rates (from inner to outer: 20, 40, 60, 80, 100, 120, 160, 200, 240, 280, 320, 360 400, 440, and 480 mV 3 s1).
Figure 6. (a) The 2D layer formed by the meso-helix chains through the unsupported Ag7 3 3 3 Ag7 dimer connection. (b) The schematic view of the 2D layer; here the Agþ monomers are shown in purple balls and the unsupported Ag7 3 3 3 Ag7 dimers are shown in red balls.
Figure 7. Interpenetration of the single huge loop and the 3D framework. The huge loop and the 3D framework are shown in black and green respectively for clarity.
according to interpenetrating fashions: Type I, the same polymeric motifs containing POM clusters interpenetrate each other, which is a common fashion;7a,b,20 Type II, metalorganic coordination polymers construct the interpenetrating framework, while POM clusters fill in the space;21 Type III, polymeric motifs of different dimensionality interpenetrate each other, for which only one example (2D þ 3D) has been found.22 Thus, compound 1 belongs to Type III. It is known that interpenetrating frameworks are often formed when large voids of a framework are
occupied by other networks. In compound 1, there are two motifs of 2D and 3D. The 3D motif including large Wells Dawson polyanions perhaps has not enough space to form the interpenetration framework of Type I, and the interpenetration is realized through penetration into the 2D layer motif composed of flexible Cu-bbi chains. Compound 1 is the second example of Type III and represents the first WellsDawson POM-based interpenetrating framework; especially, the interpenetration is formed by AgI 3 3 3 AgI interactions. In the case of compound 1, the AgI 3 3 3 AgI interactions play different roles: The supported {Ag2}2þ dimers (Ag1 3 3 3 Ag9 and Ag2 3 3 3 Ag2) play an assistant role in constructing the 3D motif, and the 3D structure would still be integrated without the AgI 3 3 3 AgI interactions, whereas the unsupported {Ag2}2þ dimers (Ag7 3 3 3 Ag7) play a key role in the formation of the interpenetrating framework, stitching the Ag-bbi chains to the 2D motif and further achieving the interpenetrating structure. XRPD, IR, UVvis Absorption Spectra, and TG Analyses. XRPD experiments were carried out for compound 1 before and after photocatalytic degradation of RhB under UV irradiation. The XRPD patterns are presented in Figure S2, Supporting Information. The diffraction peaks of the simulated and experimental pattern match well, indicating the phase purity of compound 1. Furthermore, the XRPD pattern of compound 1 after the photocatalytic experiment does not show observable change. The IR spectrum of compound 1 is shown in Figure S3, Supporting Information. In the spectrum, characteristic bands at 1087, 954, 909, and 783 cm1 are attributed to ν(PO), ν(W = O), and ν(WOW), respectively. Bands in the regions of 1708 1236 cm1 are characteristics of bbi ligands. In the UVvis absorption spectrum (Figure S4, Supporting Information), there is an absorption band at about λ=266.7 nm, which represents the characteristic of the {Ag2}2þ dimers.23 The TGA measurement also supports the chemical composition (Figure S5, Supporting Information). In the main weight loss region of 250 to 550 °C, the weight loss of 16.81% (calc 16.30%) could be assigned to the decomposition of organic ligands and POMs. Cyclic Voltammetry. Redox property of compound 1 was studied in 1 M H2SO4 aqueous solution. The electrochemical behavior is similar to the P2W18 polyanion based compounds in 2739
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Crystal Growth & Design acidic solution reported in the literature, which means that the active center for electrochemical redox activity is the polyanion. The light potential shifts of them could be ascribed to the differences of the chemical environments. The cyclic voltammograms for 1CPE at different scan rates are presented in Figure 8, in the potential range of þ600 to 800 mV. It can be seen that there exist three reversible redox peaks IIII0 , IIIIII0 , and IVIV0 , which could be ascribed to the three consecutive twoelectron processes of W centers.24 The half-wave potentials E1/2 = (Epa þ Epc)/2 are 122.5, 360.9, and 607.9 mV, respectively. In addition, the irreversible anodic peak I at about 300 mV is assigned to the oxidation of the Ag centers.25 When the scan rate is increased, the peak potentials change gradually: the cathodic peak potentials shift toward the negative direction and the corresponding anodic peak potentials to the positive direction. When the scan rates are lower than 120 mV 3 s1, the peak currents are proportional to the scan rates, which indicates that the redox processes are surfacecontrolled, and the exchanging rate of electrons is fast; however, when the scan rates are higher than 120 mV 3 s1, the peak currents are proportional to the square root of the scan rate, which indicates that the redox process of the 1CPE is diffusioncontrolled (Figure S6, Supporting Information).26
Figure 9. Cyclic voltammogram of 1CPE in the 1 M H2SO4 aqueous solution containing 0.0, 1.0, 3.0, 5.0 mL of KBrO3.
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POMs have been extensively used as the electrocatalysts in the electrocatalytic reductions of bromate, nitrite and hydrogen peroxide, such as reported by Dong, Keita, Toth and Anson and their co-workers.27 Herein, 1CPE is used to catalyze the reduction processes of bromate (Figure 9). With the addition of bromate, the two- and four-electron reduced species change unconspicuously, while the six-electron reduced species of P2W18 polyanion change sharply: the reduction peak currents gradually increase while the corresponding oxidation peak currents gradually decrease. The phenomenon suggests that the bromate is mainly reduced by the six-electron reduced species of W.
’ PHOTOCATALYTIC ACTIVITY It is known that POMs often show photocatalytic activity in the degradation of some organic substances under UV irradiation.28 Here the photodecomposition of RhB under UV light irradiation for different times is carried out to investigate the photocatalytic activity of compound 1. As shown in Figure 10a, the absorbance of the RhB is decreased along with the prolonging of reaction time. Twelve hours later, the absorbance of the RhB is about 67% of the original solution. However, the absorbance of RhB solution with the absence of compound 1 is almost unchanged after 12 h (Figure S7a, Supporting Information). The fact indicates that compound 1 exhibits photocatalytic activity in the degradation of RhB under UV irradiation. Figure 10b shows that with the increasing of reaction time, the C/C0 values are decreased. In addition, the insoluble AgCl and (C16H36N)6(P2W18O62) 3 nH2O are added in the RhB solutions instead of compound 1 for contrast (Figure S7, Supporting Information): AgCl powder did not show observable photocatalytic activity, while (C16H36N)6(P2W18O62) 3 nH2O powder exhibited good photocatalytic activity in the degradation of RhB under UV irradiation. The results of the control experiments indicate that the photocatalytic activity of compound 1 stems from the P2W18O626 component. An XRPD experiment was carried out again for compound 1 isolated after the photocatalytic experiment, which did not show an observable change in the XRPD patterns. This fact indicates that the framework of compound 1 is not collapsed when it suffers photocatalytic degradation of RhB under UV irradiation (Figure S2, Supporting Information).
Figure 10. (a) Changes in the absorption spectra of RhB solution under UV irradiation with the presence of compound 1 from 0 to 12 h. (b) RhB concentration versus reaction time with the presence of compound 1. 2740
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’ CONCLUSION In this paper, a new compound based on the P2W18 polyanion, Agþ ion, and bbi has been hydrothermally synthesized. This compound provides the first WellsDawson POM-based interpenetrating frameworks in which the AgI 3 3 3 AgI interactions are crucial in the formation of the two individual motifs: the supported {Ag2}2þ dimers participate in the formation of the 3D motif and the unsupported ones stitch the Agbbi chains to form a 2D layer with huge loops. This work enriches the POMbased entangle frameworks and expands the role of AgI 3 3 3 AgI interactions in POM chemistry. Furthermore, the compound exhibits electrocatalytic properties toward the reductions of bromate and photocatalytic action for the degradation of RhB. ’ ASSOCIATED CONTENT
bS
Supporting Information. Table of selected bond lengths and bond angles for compound 1; XRPD, IR, TG, CV data, and additional structural figures of compound 1. This information is available free of charge via the Internet at http://pubs.acs.org.
’ AUTHOR INFORMATION Corresponding Author
*Tel: þ86 4315099765; fax: þ86-431-5099667. E-mail: jpeng@ nenu.edu.cn.
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