An Unusual High Thermal Stable 2D 3D Polycatenated. Fe(II) Metal-Organic Framework Showing. Guest-Dependent Spin-Crossover Behavior and High
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1 Supporting Information for Crystal Growth & Design An Unusual High Thermal Stable 2D 3D Polycatenated Fe(II) Metal-Organic Framework Showing Guest-Dependent Spin-Crossover Behavior and High Spin-Transition Temperature Xiu-Tang Zhang, Di Sun, *, Bao Li, *, Li-Ming Fan, Bin Li and Pei-Hai Wei Advanced Material Institute of Research, Department of Chemistry, Qilu ormal University, Jinan, , China. Key Lab of Colloid and Interface Chemistry, Ministry of Education, School of Chemistry and Chemical Engineering, Shandong University, Jinan, Shandong, , China. School of Chemistry and Chemical Engineering, Huazhong University of Science and Technology, Wuhan, Hubei , P. R. China Content (1) Experiment details... 2 (2) Synthesis of 2-(3-(4-(pyridin-4-yl)phenyl)-1H-1,2,4-triazol-5-yl)pyridine (Hpptp)... 3 (3) Synthesis of 1:... 4 (4) X-ray Crystallography... 5 (5) Table S1: Crystal data for (6) Table S2: The selected bond distances and angles for SDU-1 (Å, )... 7 (7) Fig. S1: XRD pattern of (8) Fig. S2: IR spectrum of
2 (1) Experiment details Materials and General Methods. 4-bromobenzonitrile (I), 2-picolinyl Hydrazide, 4-pyridinylboronic acid, Pd(PPh 3 ) 4 were purchased from Jinan Henghua Sci. & Tec. Co. Ltd. without further purification. Elemental analyses of C,, and H were performed on an EA1110 CHS-0 CE elemental analyzer. IR (KBr pellet) spectra were recorded on a icolet Magna 750FT-IR spectrometer. Thermogravimetric measurements were carried out in a nitrogen stream using a etzsch TG 209 F1 with a heating rate of 10 o C min 1. X-Ray powder diffraction (XRPD) was carried out on a RIGAKU DMAX2500 apparatus. Magnetic measurements were carried out on a Quantum Design SQUID MPMS magnetometer working under magnetic field of 5000 Oe. 2
3 (2) Synthesis of 2-(3-(4-(pyridin-4-yl)phenyl)-1H-1,2,4-triazol-5-yl)pyridine (Hpptp) C H 3 CO H H Br (I) Br (II) Br (III) H (IV) Synthesis of (III). Equimolar amounts of 4-bromobenzonitrile (100 mmol, 19.6 g) and sodium (100 mmol, 2.3 g) were dissolved in 1000 ml methanol and heated under reflux for 3 h. The 2-picolinyl hydrazide (100 mmol, 13.7 g) was added to the solution and further refluxed for 3h. The solution was cooled to room temperature and the precipitate formed (yellow) was filtered off and air-dried for 2 h. The obtained yellow powder was heated under reflux for 2 h in 200 ml ethylene glycol and cooled to room temperature giving the white III with the yield of 82%. EI-MS: m/z [M-H]
4 (calcd for C 13 H 9 Br 4, 300.0). Anal. (%) calcd. for C 13 H 9 Br 4 : C, 51.85; H, 3.01;, Found: C, 51.80; H, 2.98;, Synthesis of (IV). The mixture of III (50 mmol, 15.0 g), 4-pyridinylboronic acid (50 mmol, 6.15 g), and K 3 PO 4 (200 mmol, 42.4 g) were mixed in 1,4-dioxane (500 ml), and the mixture was deaerated using 2 for 10 min. Pd(PPh 3 ) 4 (4 mmol, 5.0 g) was added to the stirred reaction mixture and the mixture was heated to reflux for ca. one week under 2 atmosphere. The crude product of IV was obtained after 1,4-dioxane was removed under a vacuum. Recrystallization from methanol offered the pure IV. EI-MS: m/z [M-H] (calcd for C 18 H 13 5, 299.1). Anal. (%) calcd. for C 18 H 13 5 : C, 72.23; H, 4.38;, Found: C, 72.16; H, 4.31;, (3) Synthesis of 1: The synthesis is performed in 25 ml Teflon-lined stainless steel vessels. A mixture of HL (0.20 mmol, g), oxalic acid (0.40 mmol, g), iron(ii) sulfate (0.20 mmol, g), aoh (0.10 mmol, g), 12mL H 2 O, and 2mL DMF was heated to 170 C for 3 days, followed by slow cooling (a descent rate of 10 o C/h) to room temperature, giving black block crystals. Yield of 89 % (based on Fe). Anal. (%) calcd. for C 36 H 26 Fe 10 O: C, 64.49; H, 3.91;, Found: C, 64.47; H, 3.82;, IR (KBr pellet, cm -1 ): 3435(vs), 1604(vs), 1504(vs), 1424(vs), 991(s), 746(m).. 4
5 (4) X-ray Crystallography Single crystal of the complex 1 with appropriate dimensions was chosen under an optical microscope and quickly coated with high vacuum grease (Dow Corning Corporation) before being mounted on a glass fiber for data collection. Intensity data collection was carried out on a Siemens SMART diffractometer equipped with a CCD detector using MoKα monochromatized radiation (λ = Å) at 298(2) K. The absorption correction was based on multiple and symmetry-equivalent reflections in the data set using the SADABS program. The structures were solved by direct methods and refined by full-matrix least-squares using the SHELX-TL package. Crystallographic data for complexes 1 are given in Table S1. Selected bond lengths and angles for 1 are listed in Table S2. 5
6 (5) Table S1: Crystal data for 1 Empirical formula C 36 H 26 Fe 10 O Formula weight Temperature/K Crystal system orthorhombic Space group Pbcn a/å (2) b/å (9) c/å (2) α/ β/ γ/ Volume/Å (6) Z 4 ρ calc mg/mm m/mm F(000) Crystal size/mm Θ range for data collection 4.16 to 50 Index ranges -23 h 23, -9 k 9, -21 l 23 Reflections collected Independent reflections 2808[R(int) = ] Data/restraints/parameters 2808/0/219 Goodness-of-fit on F Final R indexes [I>=2σ (I)] R 1 = , wr 2 = Final R indexes [all data] R 1 = , wr 2 = Largest diff. peak/hole / e Å /
7 (6) Table S2: The selected bond distances and angles for SDU-1 (Å, ) Fe1 2 i (2) Fe1 5 iii (2) Fe (2) Fe (3) Fe1 5 ii (2) Fe1 1 i (3) 2 i Fe (15) 5 ii Fe (10) 2 i Fe1 5 ii (10) 5 iii Fe (10) 2 Fe1 5 ii (10) 2 i Fe1 1 i (10) 2 i Fe1 5 iii (10) 2 Fe1 1 i (10) 2 Fe1 5 iii (10) 5 ii Fe1 1 i (10) 5 ii Fe1 5 iii (2) 5 iii Fe1 1 i (10) 2 i Fe (10) 1 Fe1 1 i (19) 2 Fe (10) Symmetry codes: (i) x, y, z; (ii) x 1/2, y 1/2, z+1/2; (iii) x+1/2, y+1/2, z 1/2. 7
8 (7) Fig. S1: XRD pattern of 1 8
9 (8) Fig. S2: IR spectrum of 1 9
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