Supporting Information. A novel microporous metal-organic framework exhibiting high acetylene and methane storage capacities
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1 Supporting Information A novel microporous metal-organic framework exhibiting high acetylene and methane storage capacities Xing Duan, a Chuande Wu, b Shengchang Xiang, c Wei Zhou, de Taner Yildirim, df Yuanjing Cui, a Yu Yang, a Banglin Chen af * and Guodong Qian a * a b c d e f State Key Laboratory of Silicon Materials, Cyrus Tang Center for Sensor Materials and Applications, Department of Materials Science & Engineering, Zhejiang University, Hangzhou , China. gdqian@zju.edu.cn Department of Chemistry, Zhejiang University, Hangzhou , China. Fujian Provincial Key Laboratory of Polymer Materials, Fujian Normal University, 3 Shangsan Road, Cangshang Region, Fuzhou , China. NIST Center for Neutron Research, Gaithersburg, Maryland , USA. Department of Materials Science and Engineering, University of Maryland, College Park, Maryland 20742, USA. Department of Chemistry, University of Texas at San Antonio, One UTSA Circle, San Antonio, Texas , USA. banglin.chen@utsa.edu; Fax: (+1) Materials and Measurements: All the chemicals were commercially available and used without further purification. 1H NMR spectra were recorded on a Bruker Advance DMX 500 spectrometer using tetramethylsilane (TMS) as an internal standard. Elemental analyses for C, H, and N were performed on an EA1112 microelemental analyser. Powder X-ray diffraction (PXRD) patterns were collected in the 2θ=3-30o range on an X Pert PRO diffractometer with Cu Kα adiation (λ= 1.542Å) at room temperature. Thermogravimetric analyses (TGA) were S1
2 conducted on a Netszch TGA 209 F3 thermogravimeter with a heating rate of 10 oc min-1 in an N2 atmosphere. Gas Sorption Measurements: A Micromeritics ASAP 2020 surface area analyzer was used to measure gas adsorption. In order to remove guest solvent molecules in the framework, the fresh sample of ZJU-70 was exchanged with dry acetone for 10 times, filtered and vacuumed at room temperature for 12 h and then at 373 K until the outgas rate was 5 µmhg/min-1 prior to measurements. The sorption measurement was maintained at 77 K with liquid nitrogen and 273 K with ice-water bath (slush), respectively. As the center-controlled air condition was set up at 298 K, a water bath of 298 K was used for adsorption isotherms at 298 K. X-ray Collection and Structure Determination: Crystallographic measurements for ZJU-70 were taken on an Oxford Xcalibur Gemini Ultra diffractometer with an Atlas detector using graphitemonochromatic Mo Kα radiation (λ = Å) at 293 K. The determinations of the unit cells and data collections for the crystals of ZJU-70 were performed with CrysAlisPro. The data sets were corrected by empirical absorption correction using spherical harmonics, implemented in the SCALE3 ABSPACK scaling algorithm 1 All structures were determined by direct methods and refined by the full-matrix least-squares method with the SHELX-97 program package 2. All non-hydrogen atoms, including solvent molecules, were located successfully from Fourier maps and were refined anisotropically. H atoms on C atoms were generated geometrically. Because the solvent molecules in ZJU-70 are highly disordered, SQUEEZE subroutine of the PLATON software suit was used to remove the scattering from the highly disordered guest molecules 3. The resulting new files were used to further refine the structure. The certain degree of framework disorder generates the B level alerts in the checkcif reports. Crystallographic data are summarized in Table S1. S2
3 Table1 S1. Crystallographic Data Collection and Refinement Results for ZJU-70. ZJU-70 Chemical formla C 72 H 42 Cu 6 N 2 O 30 Formula weight Temperature(K) 293(2) Wavelength(Å) Crystal system Orthorhombic Space group C mc2 1 a(å) (8) b(å) (3) c(å) (13) V(Å 3 ) 27228(2) Z 8 Density(calculated g/cm 3 ) Absorbance coefficient(mm -1 ) F(000) 7216 Crystal size(mm 3 ) 0.42Χ0.27Χ0.16 Goodness of fit on F R 1,wR 2 [I>2σ(I)] , R 1,wR 2 (all data) , Largest difference peak and hole(e/å 3 ) CCDC 1.985, S3
4 Intensity (a.u.) Degree/2θ Figure S1. PXRD patterns of ZJU-70 (simulated: black; as-synthesized: red; after the gas sorption experiments: blue) 100 Weight loss (%) Temperature( C) Figure S2. TGA patterns of ZJU-70 S4
5 Differential Pore Volume (cm 3 /g Å) Pore Width (Å) Figure S3. The pore size distribution of ZJU-70 Amount adsorbed [cc(stp)/cc Pressure (bar) Figure S4. High-pressure excess CH 4 sorption isotherm of ZJU-70a at 273 K and 298 K. References (1) CrysAlisPro, version ; Oxford Diffraction Ltd.: Oxfordshire, U.K (2) Sheldrick G. M. Program for Structure Refinement; Germany, 1997 (3) Spek A. L. J. Appl. Crystallogr 2003, 36, S5
6 S6
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