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Crystal Structures and Physical Properties of Ag(I) Coordination Polymers with Unsymmetrical Dipyridyl Ligand
Crystal Structures and Physical Properties of Ag(I) Coordination Polymers with Unsymmetrical Dipyridyl Ligand
Bulletin of the Korean Chemical Society. 2013. Nov, 34(11): 3477-3480
Copyright © 2013, Korea Chemical Society
  • Received : June 27, 2013
  • Accepted : August 09, 2013
  • Published : November 20, 2013
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About the Authors
Eunji Lee
Hyunsoo Ryu
Suk-Hee Moon
Department of Food and Nutrition, Kyungnam College of Information and Technology, Busan 617-701, Korea
Ki-Min Park

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Experimental
All chemicals were of analytical regent grade and used without further purification. The IR spectra were recorded on a VERTEX 80v FT-IR spectrometer with KBr pellet in the range 4000-400 cm −1 . Elemental analysis was carried out on a CHNS-932 elemental analyzer. Thermogravimetric analysis (TGA) was performed under nitrogen on a SDT Q600 thermogravimetric analyzer. The sample was heated using a 10 ℃/min heating rate from 25 to 900 ℃. The solidstate excitation and emission spectra were performed on a RF-5301 spectrophotometer.
Preparation of N,N-(2-Pyridyl)(2-pyridylmethyl)amine (L). L was synthesized according to literature procedure. 7
Synthesis of {[Ag(L)]·(ClO4)·(DMSO)}n (1). A MeOH (5 mL) solution of AgNO 3 (43.0 mg, 0.254 mmol) was added dropwise to the MeOH solution (10 mL) of L (50.0 g, 0.231 mmol) at room temperature. The white precipitate in 94% yield formed immediately. The precipitate was filtered off, washed with methanol and diethyl ether, and dried in vacuo. Single crystals suitable for X-ray analysis were obtained by vapor diffusion of diethyl ether into DMSO solution. Yield: 63%. Anal. Calc. for C 13 H 17 AgClN 3 O 5 S (%): C, 33.17; H, 3.64; N, 8.93. Found: C, 33.28; H, 3.73; N, 10.05. IR (KBr pellet, cm −1 ): 3228, 3072, 3034, 2854, 1606, 1576, 1518, 1459, 1426, 1332, 1161, 1115, 1089 (ClO 4 ), 789, 716, 636, 628. mp 268-269 ℃ (decomp.).
Synthesis of {[Ag(L)]·(BF4)·(DMSO)}n (2). The synthetic procedure was almost the same as for 1 except for the use of AgClO 4 instead of AgBF4. Yield: 57%. Anal. Calc. for C 13 H 17 AgBF 4 N 3 OS (%): C, 34.09; H, 3.74; N, 9.17. Found: C, 34.15; H, 3.78; N, 9.24. IR (KBr pellet, cm −1 ): 3228, 3072, 3033, 2874, 2584, 1606, 1576, 1519, 1458, 1426, 1332, 1161, 1039 (BF 4 ), 789, 716, 533, 522. mp 265-266 ℃ (decomp.).
Synthesis of {[Ag(L)]·(PF6)·(DMSO)}n (3). The synthetic procedure was almost the same as for 1 except for the use of AgClO 4 instead of AgPF6. Yield: 67%. Anal. Calc. for C 13 H 17 AgF 6 N 3 OPS (%): C, 30.25; H, 3.32; N, 8.14. Found: C, 30.18; H, 3.48; N, 8.02. IR (KBr pellet, cm −1 ): 3226, 3070, 3034, 2874, 1608, 1575, 1517, 1459, 1423, 1331, 1161, 1029, 835 (PF 6 ), 786, 716, 637, 558. mp 270-271 ℃ (decomp.).
X-ray Crystallography. Single crystal diffraction data of 1 and 2 were collected on a Bruker Smart diffractometer equipped with a graphite monochromated Mo K α (λ = 0.71073 Å) radiation source and a CCD detector. The 45 frames of two dimensional diffraction images were collected and processed to obtain the cell parameters and orientation matrix. A total of 1271 frames of two-dimensional diffraction images were collected, each of which was measured for 5 sec. Decay was monitored by 50 standard data frames measured at the beginning and end of data collection. The crystal showed no significant decay. The frame data were processed to give structure factors using the SAINT. 13 The structure was solved by direct methods and refined by full matrix least squares methods on F 2 for all data using SHELXTL software. 14 In all compounds, all atoms except oxygen atoms in DMSO molecule were disordered over two sites with equal site occupation factors of 0.5. The nonhydrogen atoms were refined anisotropically. All hydrogen atoms except that of amine in all compounds were placed in calculated positions and refined with a riding model. The H atom of amine was located from difference Fourier map and refined with riding constraints. Crystallographic data and structural refinement data for compounds 1-3 is summarized in Table 1 . Crystallographic data for the structures reported here have been deposited with CCDC (Deposition No. CCDC-646600 ( 1 ), CCDC-946601 ( 2 ), and CCDC-946602 ( 3 )). These data can be obtained free of charge via http:// www.ccdc.cam.ac.uk/conts/retrieving.html or from CCDC, 12 Union Road, Cambridge CB2 1EZ, UK, E-mail: deposit @ccdc.cam.ac.uk (or FIZ, D-76344, Eggenstein-Leopoldshafen, Germany, E-mail: crysdata@fiz-karlsruhe.de).
Acknowledgements
Supporting Information.Supplementary crystal data, figures for2and3, and TGA of1-3are included. This material is available free of chargeviathe internet at http:// www.kcsnet.or.kr/bkcs.
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