ELECTRONIC SUPPLEMENTARY INFORMATION. Highly Porous and Robust Scandium-based Metal-Organic. Frameworks for Hydrogen Storage

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1 ELECTRONIC SUPPLEMENTARY INFORMATION Highly Porous nd Roust Scndium-sed Metl-Orgnic Frmeworks for Hydrogen Storge Ilich A. Irr, Sihi Yng, Xing Lin, Alexnder J. Blke, Pierre J. Rizkllh, Hrriott Nowell, c Dvid R. Alln, c Neil R. Chmpness, * Peter Huerstey nd Mrtin Schröder *. School of Chemistry, University of Nottinghm, Nottinghm NG7 2RD, UK. Fx: ; Tel: Emil: Neil.Chmpness@nottinghm.c.uk; M.Schroder@nottinghm.c.uk. STFC Dresury Lortory, Dresury Science nd Innovtion Cmpus, Wrrington, Cheshire, WA4 4AD, UK c. Dimond Light Source, Hrwell Science nd Innovtion Cmpus, Didcot, Oxfordshire, OX11 0DE, UK 1

2 1. Experimentl Section 1.1 Mterils nd Mesurements All regents nd solvents were used s received from commercil suppliers without further purifiction. Elementl micronlyses for C, H nd N were crried out on CE-440 elementl nlyser t the University of Nottinghm. Powder X-ry diffrction (PXRD) dt were collected under oth mient nd in-situ conditions on Bruker AXS D8 Advnce diffrctometer operted t 40 kv nd 40 ma (Cu Kα 1, λ= Å), with heting rte of 2 C/min nd step size of 0.04 /2θ. An MRI TCP-20 with PtRh strip heter ws used for the in-situ vrile temperture PXRD experiments. Thermogrvimetric nlysis (TGA) ws performed under N 2 t scn rte of 2 C/min using TA Universl Anlysis 2000 system. 1.2 Synthesis of {[Sc 2 (BPTC)(OH) 2 ] (H 2 O) 1.25 } NOTT-400 Scndium triflte (0.030g, mmol) nd H 4 BPTC (0.010 g, mmol) were mixed in THF (4.0 ml), DMF (3.0 ml), wter (1.0 ml) nd HCl (36.5 %, 2 drops). The resultnt slurry mixture ws stirred until complete dissolution occurred. The solution ws then plced in pressure tue nd heted in n oil th to 75 o C for 72 h. The tue ws cooled down to room temperture t rte of 0.1 o C/min, nd the colourless crystlline product ws seprted y filtrtion, wshed with DMF (5.00 ml) nd dried in ir. Yield: 67.6 % (sed on lignd). Elementl nlysis corresponds to Sc 2 C 16 H 10.5 O %: Cl: C, 40.66; H: 2.24; found: C, 40.67; H, Synthesis of {[Sc(TDA)(OH)] (H 2 O) 2.6 } NOTT-401 Scndium triflte (0.057 g, mmol) nd thiophene-2,6-dicroxylic cid, H 2 TDA, (0.01 g, mmol) were dispersed in THF (4.0 ml), DMF (3.0 ml), H 2 O (1.0 ml) nd HCl (36.5 %, 2 drops) nd seled in pressure tue. The cler solution ws heted t 90 o C in n oil th for 72 h. The tue ws cooled to room temperture over period of 12 h nd the colourless crystlline product seprted y filtrtion, wshed with DMF (5.00 ml) nd dried in ir. Yield: 71.1 % (sed on lignd). Elementl nlysis dt corresponds to ScO 7.6 C 6 H 8.2 S%: Cl: C, 25.84; H, 2.75; found: C, 25.82; H,

3 1.4 X-Ry Crystllogrphy Single crystl diffrction dt for NOTT-400 were collected on Sttion 9.8 of the Synchrotron Rdition Source t STFC Dresury Lortory. Diffrction dt for NOTT-401 were collected on Bemline I19 t the Dimond Light Source. The detils for dt collection re included in CIF files in the Supplementry Informtion. Structures were solved y direct methods nd developed y difference Fourier techniques using the SHELXTL softwre pckge. 1 The hydrogen toms on the lignd were plced geometriclly nd refined using riding model. The unit cell volumes include lrge region of disordered solvent which could not e modelled s discrete tomic sites. We employed PLATON/SQUEEZE 2 to clculte the contriution to the diffrction from the solvent region nd therey produced set of solvent-free diffrction intensities. The finl formule were clculted from the SQUEEZE 2 results comined with elementl nlyticl dt. Figure S1: () The inucler uilding lock comprising two Sc(III) centres ech with pproximtely octhedrl geometry; () polyhedrl representtion of the two Sc(III) octhedr shring μ 2 -hydroxo group; (c) the inucler uilding lock of NOTT-400 showing the lignd [BPTC] 4- coordinted to Sc(III) centres nd (d) the uilding lock of NOTT-401 showing the lignd [TDA] 2- coordinted to Sc(III) centres (Sc lue, S yellow, O red, C lck, H smll grey spheres). 3

4 1.5 Nitrogen nd hydrogen dsorption isotherms. N 2 nd H 2 isotherms were recorded on n IGA system (Hidden Isochem, Wrrington, UK) t the University of Nottinghm under ultr high vcuum in clen system with diphrgm nd turo pumping system. Ultr-pure grde ( %) H 2 ws purchsed from BOC nd purified further using clcium luminosilicte nd ctivted cron dsorents to remove trce mounts of wter nd other impurities efore introducing into the IGA system. The density of H 2 t 77 K in the uoyncy correction ws clculted y the Redlich-Kwong-Sove eqution of stte of H 2 incorported in the IGASWIN softwre of the IGA system. The surfce re ws clculted using the BET method sed on dsorption dt in the prtil pressure (P/Po) rnge 0.06 to The pore size distriution (PSD) ws determined y pplying the Duinin-Astkhov nlysis to the N 2 dsorption dt nlysis to the isotherm dt. 2. TGA plots Figure 2S: TGA nlysis of compounds NOTT-400 nd NOTT

5 3. PXRD Ptterns Figure 3S: Experimentl PXRD dt nd simulted pttern derived from the single crystl structures of () NOTT-400 nd () NOTT-401. Figure 4S: In situ PXRD ptterns for () NOTT-400 nd () NOTT-401. Smples held for 5 mins t ech temperture 5

6 4. Nitrogen dsorption isotherms Figure 5S: N 2 sorption isotherms for () desolvted NOTT-400 nd () desolvted NOTT-401 t 77 K. 5. Pore Size Distriution Anlysis Figure 6S: Pore size distriution for () desolvted NOTT-400 nd () desolvted NOTT-401 (). 6

7 6. Derivtion of the isosteric hets of H 2 dsorption. Grvimetric H 2 dsorption ws mesured from 0-20 r t 77K nd 87K for desolvted NOTT-400 nd NOTT-401. All dt were strictly corrected for the uoyncy of system, smples nd sortes. All the H 2 sorption isotherms show good reversiility nd sence of hysteresis (Figures 7S). The H 2 dsorption kinetic dt confirm tht equilirium is chieved within c. 3 mins of the isotherm pressure step. These suggest typicl H 2 dsorption nd exclude ny significnt effect due to the presence of impurities. Figure 7S: H 2 isotherms for () desolvted NOTT-400 nd () desolvted NOTT-401t 77 nd 87 K. The isosteric hets of H 2 dsorption were determined y fitting viril-type eqution to oth 77 nd 87 K dsorption isotherms. The ln(n/p) vlues for given mount dsored (n) were clculted from the liner regressions from the viril eqution nlysis using the following viril eqution: 3, 4 ln(n/p) = A 0 + A 1 n + A 2 n 2 (1) where p is pressure, n is mount dsored nd A 0, A 1 etc. re viril coefficients. A 0 is relted to dsortedsorent interctions, while A 1 descries dsorte-dsorte interctions. 4 Henry s Lw constnt (K H ) is equl to exp(a 0 ), nd t low surfce coverge, A 2 nd higher terms cn e ignored. A plot of ln(n/p) versus n should give stright line t low surfce coverge. Simultion of H 2 dsorption dt t 77 nd 87 K for NOTT-400 nd NOTT-401 etween 50 nd 400 mr using eqution (1) re presented in Figures 8S nd 9S, respectively. All the regression coefficients 7

8 were lrger thn 0.998, showing tht the model fits the dt very well. The viril method sed on eqution (1) is preferred t low pressure ecuse the linerity in the low pressure prt of the isotherm provides direct confirmtion of the ccurcy of the interpoltions. The isosteric hets of dsorption for H 2 on desolvted NOTT-400 nd NOTT-401 were clculted s function of surfce coverge. The estimted error in the mesured isosteric enthlpies is 0.1 kj/mol. Figure 8S: Viril fitting plot for the dsorption of H 2 on NOTT-400 t 77 K () nd 87 K (). Figure 9S: Viril fitting plot for the dsorption of H 2 on NOTT-400 t 77 K () nd 87 K (). 8

9 Adsorption enthlpy kj/mol Electronic Supplementry Mteril (ESI) for Chemicl Communictions NOTT-400 NOTT H 2 uptke (mol/g) Figure 10S: Vrition of dsorption enthlpy t low loding for NOTT-400 nd NOTT-401. References: 1. G. M. Sheldrick, Act Crystllogr. Sect. A, 2008, 64, A. L. Spek, J. Appl. Crystllogr., 2003, 36, 7; P.v.d. Sluis nd A. L. Spek, Act Crystllogr., Sect. A, 1990, 46, X. Zho, S. Villr-Rodil, A. J. Fletcher nd K. M. Thoms, J. Phys. Chem. B, 2006, 110, 9947; X. Zho, B. Xio, A. J. Fletcher nd K. M. Thoms, J. Phys. Chem. B, 2005, 109, 8880; I. P. Okoye, M. Benhm nd K. M. Thoms, Lngmuir, 1997, 13, 4054; C. R. Reid, I. P. OKoye nd K. M. Thoms, Lngmuir, 1998, 14, 2415; C. R. Reid nd K. M. Thoms, Lngmuir, 1999, 15, 3206; C. R. Reid nd K. M. Thoms, J. Phys. Chem. B, 2001, 105, J. H. Cole, D. H. Everett, C. T. Mrshll, A. R. Pniego, J. C. Powl nd Rodrigue.F, J. Chem. Soc., Frdy Trns. I, 1974, 70,

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