Metal-Organic Frameworks, Hydrogen Bonded Organic-Frameworks. Jesse Rowsell
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1 Metal-rganic Frameworks, ydrogen Bonded rganic-frameworks Jesse Rowsell
2 utline 1. Who am I? 2. Who was Jesse Rowsell? 3. What is the crystalline structure of tcpb? 4. Who are our students? NSF-MRI Grants NSF-Grant #
3 berlin Chalk Walk
4 Publications as an undergraduate student Crystallographic investigation of the Co-B- system J.L.C. Rowsell, N.J. Taylor and L.F. Nazar J. Solid State Chem., 174, 189 (2003) Structure and ion exchange properties of a new cobalt borate with a tunnel structure templated by Na+ J.L.C. Rowsell, N.J. Taylor and L.F. Nazar J. Am. Chem. Soc., 124, 6522 (2002) Synthesis, structure, and solid-state electrochemical properties of Cr 3 B 6 : J.L.C. Rowsell and L.F. Nazar J. Mater. Chem., 11, 3228 (2001) Speciation and thermal transformation in alumina sols:.. J. Rowsell and L.F. Nazar J. Am. Chem. Soc., 122, 3777 (2000) Layered lithium iron nitride: a promising anode material for Li-ion batteries J.L.C. Rowsell, V. Pralong and L.F. Nazar J. Am. Chem. Soc., 123, 8598 (2001) A new class of materials for lithium-ion batteries: iron(iii) borates J.L.C. Rowsell, J. Gaubicher and L.F. Nazar J. Am. Chem. Soc., 123, 8598 (2001)
5 Early days of MFs J.L.C. Rowsell et al., Science, 2005.
6 Binding sites in MF-5
7 DRIFTS instrumentation FitzGerald et al., Rev. Sci. Inst., 2006
8 Absorbance 2 2 Interactions in MF per cluster per cluster per cluster per cluster per cluster Frequency (cm -1 )
9 Infrared Spectrum of 2 in Mg-MF-74 FitzGerald et al., JACS, 2011
10 Band intensities plateau as sites fill Liu et al., Langmuir, 2008 FitzGerald et al., JACS, 2011
11 Metal-specific band redshifts
12 1,3,5-Tris(4-carboxyphenyl)benzene tcpb
13 Predict the crystal packing of this molecule
14 Predict the crystal packing of this molecule
15 Predict the crystal packing of this molecule
16 Predict the crystal packing of this molecule
17 Predict the crystal packing of this molecule
18 A starting model?
19 You might have guessed hexagonal
20 Single crystals after evaporation of ethanol
21 Large unit cells, twinning, poor resolution
22 Crystal data Space Group I 2 Cell Parameters a = (6) Å a = 90 b = (6) Å b = (2) c = (9) Å g = 90 Cell Volume (14) Å 3 Z, Z 56, 14 [462 independent non- atoms] Radiation Mo Ka, Incoatec ImS microfocus source Temperature 100 K Structure Solution SELXD Reflections total, unique, (I > 2s[I]) Completeness 98.7% to q = Parameters, Restraints 4201, 1 R1(obs,all) / wr2(obs,all) , / 0.268, Matthias Zeller, Youngstown State University Charles Campana, Bruker Madison, WI
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65 Stacking of hexagonal sheets
66 Catenation of non-parallel layers
67 Remaining void volume is substantial 38% void volume, could be occupied by 167 ethanol molecules, SQUEEZE identifies 1540 e (45 ethanol)
68 Mass (%) eat Flow (W/g) Crystal structure retained after desolvation Phase change Temperature ( o C)
69 Intensity (arb. units) Reversible (de)solvation 200 C, N C, N 2 20 C, ethanol 200 C, N C, N q (deg.), Cu Ka radiation
70 Bulk crystallization from TF/ 2 50/50 Mixture of water and tetrahydrofuran
71 Gas adsorption confirms microporosity rhan Talu, Cleveland State University Initial Isosteric eat 2 = -5.7 kj/mol Initial Isosteric eat C 2 = -22 kj/mol BET surface area 1100 m 2 /g
72 Redshift (cm -1 ) Binding energy trend for 2 VSB Mod-NiMF Mod-CoMF-74 CoMF-74 NiMF MF-5 Mod-MnMF-74 MnMF-74 MgMF-74 KUST-1 ZnMF-74 ZIF-8 tcpb Isosteric heat (kj/mol) 15
73 tcpb derivatives R 1 R 2 R 3 R 4 C 3 C 3 C 3 C 3 N 2 C 3 N 2 N 2 N 2 N 2 C 3 C 3 C 3 C 3
74 Derivative synthesis
75 Derivative synthesis
76 Comparison of local structure tcpb 8-fold catenation
77 Comparison of local structure tcpb-c 3 7-fold catenation, methyls concealed
78 tcpb derivatives R 1 R 2 R 3 R 4 C 3 C 3 C 3 C 3 N 2 C 3 N 2 N 2 N 2 N 2 C 3 C 3 C 3 C 3
79 tcpb-n 2 synthesis
80 Comparison of local structure tcpb-n 2 7-fold catenation, some N 2 exposed
81 berlin student coauthors on our papers Kelty Allen UC Berkeley Jesse opkins Cornell Patrick Landreman Stanford John Matters.C.S. Ross Myers Columbia Brian Burkholder U. Washington Michael Friedman Boston U. Josh Greenfield UC Davis Jenny Schloss M.I.T. Chris Pierce hio State Elizabeth Gilmour U. Memphis Jocienne Nelson Cornell
82 Student leaders on tcpb paper Cassandra Zentner berlin? Ren Wiscons U. Michigan olden Lai U.C. Berkeley
83 Core functionalization: pyrylium intermediate
84 Core functionalization: Suzuki coupling
85 Smaller IR band redshifts for adsorbed 2
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