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- Earl Hudson
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1 Supporting informtion for Competitive co-dsorption of with H O, NH 3, SO, NO, NO, N, O, nd CH in M-MOF-7 (M= Mg, Co, Ni): the role of hydrogen onding Kui Tn, Sestin Zulug, Qihn Gong, Yuzhi Go, Nour Nijem, ± Jing Li, Timo Thonhuser, Yves J Chl * Deprtment of Mterils Science & Engineering, University of Texs t Dlls, Richrdson, Texs 758 Deprtment of Physics, Wke Forest University, Winston-Slem, North Crolin 719 Deprtment of Chemistry nd Chemicl Biology, Rutgers University, Pisctwy, New Jersey 885 ± Deprtment of Chemistry, University of Cliforni Berkeley, Berkeley, Cliforni, 97 Contents 1. Synthesis nd chrcteriztion of M-MOF-7 (M= Mg, Co, Ni) compounds.... Gs phse nd dsored in Pure nd H O dsorption in M-MOF-7 (M= Mg, Co, Ni) Co-dsorption of nd H O in M-MOF-7 (M= Mg, Co, Ni) Diffusion of SO, NO in M-MOF-7 (M= Mg, Co, Ni) nd H O dsorption in Ni-MOF NO dsorption in the pre-loded nd clen Ni-MOF NO in M-MOF-7 (M= Mg, Co) Co-dsorption of NH 3 nd in Co-dsorption of mixture gses of + SO nd + NH SO dsorption into Co-dsorption of nd N, O, CH in The frequencies of t metl site nd t the secondry site H O nd SO in S1
2 1. Synthesis nd chrcteriztion of M-MOF-7 (M= Mg, Co, Ni) compounds Synthesis: : A mixture of mgnesium nitrte hexhydrte (.6 g, 1 mmol),, 5-dihydroxyterephthlic (.1 g,.5 mmol), 7 ml tetrhydrofurn (THF), 3 ml wter H O nd ml 1 M NOH solution ws prepred in 8 ml Teflon-lined utoclve. The utoclve ws then seled nd heted to 1 C for 3 dys. After filtering nd wshing with ml THF, the product ws collected nd exchnged with methnol every h during dytime for 3 dys. Then the MOFs smple ws stored in N glove ox. Ni-MOF-7: A mixture of nickel nitrte hexhydrte (. g,.8 mmol),, 5-dihydroxyterephthlic (.8 g,. mmol), 9 ml DMF nd 1 ml H O ws prepred in 8 ml Teflon-lined utoclve. The utoclve ws then seled nd heted to 1 C for 3 dys. After filtering nd wshing with ml DMF, the product ws collected nd exchnged with methnol every h during dytime for 3 dys. Then the MOFs smple ws stored in N glove ox. Co-MOF-7: A mixture of colt nitrte hexhydrte (.17 g,.6 mmol),, 5-dihydroxyterephthlic (.6 g,.3 mmol), 9 ml DMF nd 1 ml H O ws prepred in 8 ml Teflon-lined utoclve. The utoclve ws then seled nd heted to 1 C for 3 dys. After filtering nd wshing with ml DMF, the product ws collected nd exchnged with methnol every h during dytime for 3 dys. Then the MOFs smple ws stored in N glove ox. The crystl structures of the three smples M-MOF-7 (M= Mg, Co, Ni) were mesured y PXRD nd compred to the simulted PXRD pttern of Ni-MOF-7 in reference (1), s shown in Figure S1. The XRD diffrction ptterns of the smples we studied re in greement with literture reports. 1 Intensity (. u.) Ni-MOF-7 Co-MOF-7 Simulted Ni-MOF-7 Pttern Thet Figure S1.Power X-ry diffrction pttern of M-MOF-7 smples (fter solvent exchnge) with the simulted pttern from single crystl dt of Ni-MOF-7 tken from reference (1). The BET surfce res of the three compounds re mesured y N isotherm (Figure S). The vlues for Mg-,Ni-, nd Co- MOF-7 re 178, 913, nd 177 m /g, respectively. Tle S1 summrize the vlues mesured in this work nd those mesured in previous literture reports. Note tht there hve een mny studies of MOF-7 with some vritions in the ctivtion processes, resulting in rnge of BET surfce res. Clerly, the ctivtion of MOF-7 structure contining coordintively unsturted metl sites is not s esy s for other MOFs such s M(dc)(ted).5. For instnce, the vlues for reported in the different studies vry significnt (877 to 15 m /g). Our method for synthesizing Mg-MOF- 7 follows the procedure from ref (3). BET vlue reported in the originl work ws 877 m /g, which ws lower thn lter reported vlues nd most likely the result of incomplete solvent exchnge. We used the sme synthetic method ut with modified nd more thorough solvent exchnge s descried ove. As result, the BET surfce re is higher thn the originl reported vlue, though still lower thn other studies. However, the spectroscopic study of this work focuses on the interction of smll molecules with ville open metl sites nd the moleculr exchnge process tking plce with these sites. The interprettion derived from the results will therefore not e influenced if smll frction of other metl sites re not open for dsorption ecuse of possile incomplete ctivtion. S
3 3 Quntity dsored (cc/g, STP) MOF7-Co MOF7-Ni MOF7-Mg Reltive Pressure (P/Po) Figure S. N dsorption isotherm in M-MOF7 (M= Mg, Co, Ni) t 77 K. M=Mg, Co, Ni Tle S1. Summry of BET surfce res of M-MOF-7 (M= Mg, Co, Ni), compred with the vlues in previous studies. BET surfce re (m /g) Ref This work Co-MOF This work Ni-MOF This work The compounds in the tle were synthesized y hydrotherml method. S3
4 The MOF powder ws ttched to the KBr pellet y pressing with pressure of ~6 to 65 psi t room temperture This procedure ws checked not to lter the MOF-7 crystl structure y Rmn mesurements (see Figure S3). After pressing into KBr surfce Co-MOF-7 After pressing into KBr surfce Intensity (. u) MOF powder Intensity (. u) MOF powder Rmn shift (cm -1 ) Rmn shift (cm -1 ) Figure S3. Rmn spectr of s-synthesized powders nd MOFs on the KBr pellet fter ctivtion (18 C, vcuum< mtorr, 3h).. Gs phse nd dsored in.5 C 8 Torr ν s Figure S. IR spectr of 8 Torr gs phse (red line) nd dsored in ctivted (lck line)fter evcution of gs phse for sec. The pek t 35 cm -1 refers to the dsored within MOFs. 35 S
5 3. Pure nd H O dsorption in M-MOF-7 (M= Mg, Co, Ni).1 C Desorption sec min 8 min 3 min 1 h h Co-MOF Time (min) Figure S5. IR sorption spectr of desorption from Co-MOF-7 s function of time. Inset shows the integrted res for the ν 3 nd chnge within h. The gs phse (< mtorr) in the very eginning (< min) ws sutrcted In order to experimentlly determine the preferentil wter dsorption sites, fter ~3 mtorr of wter vpor ws introduced into ctivted M-MOF-7 (M= Mg, Ni, Co), spectr (1 scns per loop) were mesured for min nd recorded s function of time. Figure S6 shows tht the spectr recorded t the end of, 3, nd min. Under such low humidity level, only the dsorption sites with the highest inding energy re occupied (the overll loding corresponds to couple of molecules per unit cell). The spectr in Figure S6, cquired under such low humidity levels, show two shrp peks t 3663, 3576 cm -1 for ; 3668, 358 cm -1 for Co-MOF-7; 361, 355 cm -1 for Ni-MOF-7. The seprtion etween ν s nd ν s modes is 87 cm -1, which is consistent with the clculted vlue of 97 cm -1 for the configurtion wherein wter is onded to metl Mg + sites shown in Tle S. In this geometry, the H tom is pointed towrd the empty chnnel s shown in Figure S6d. Tle S. Summry of virtionl frequencies of H O t the open metl sites (Mg +, Ni +, Co + ) in M-MOF-7 (M= Mg, Co, Ni). MOFs Antisymmetric Sym metric stretching: Seprtion stretching: ν s (cm -1 ) ν s (cm -1 ) etween ν s nd ν s (cm -1 ) (clculted) ( clculted) (clculted) Co-MOF Ni-MOF S5
6 . C ν s ν s. ν s ν s Co-MOF-7 97 K min min min min min 1 min c.3 ν s ν s Ni-MOF-7 97 K d min 3 min min Figure S6. IR sorption spectr of dsored H O into () Mg, () Co, nd (c) Ni-MOF-7 t room temperture fter introducing ~3 mtorr H O to the cell s function of time. (d) Single wter molecule dsored in open metl site. Ornge, rown, red, nd white spheres represent M (Mg, Co, Ni), C, O, nd H toms, respectively..1 Desorption C C 1 C 335 RT.1 8 torr 5 torr 3 torr 1 torr 8 mtorr 6 mtorr mtorr mtorr 15 mtorr 1 mtorr 5 mtorr 3386 Adsorption C mtorr β(h O) Figure S7. IR sorption spectr of H O dsored into s function of wter vpor pressure (ottom), nd upon evcution (< mtorr se pressure) s function of nneling temperture ( C, 1 C, 15 C nd C). Ech temperture ws hold for min. Inset shows the wter sorption nd t 5 mtorr nd nneling in vccum (< mtorr) t 1 C for min. 161 S6
7 . Co-dsorption of nd H O in M-MOF-7 (M= Mg, Co, Ni). 35 cm -1 Time second Time second cm -1 Co-MOF Figure S8. IR sorption spectr of desorption s function of time t 75 C. Pnel () shows the results for, while pnel () shows the results for Co-MOF C under vcuum decrese After exposing to 8 Torr H O C under vcuum decrese After exposing to 8 Torr H O Time (second) Time (second) Figure S9. Integrted res of the ν 3 ( ) nd under vcuum (< mtorr) nd 8 Torr H O. Pnel shows the results for Mg- MOF-7 t C (Figure ), while pnel () shows the results for t 75 C (Figure ) Co-MOF-7 under vcuum C decrese After exposing to 8 Torr H O Time (second) Time (second) Figure S1. Integrted res of ν 3 ( ) nd under vcuum (< mtorr) nd 8 Torr H O in Co-MOF-7. Pnel () shows the result for Co-MOF-7 t C (Figure ), while pnel () shows the results for Co-MOF-7 t 75 C (Figure ) C Co-MOF-7 under vcuum decrese After exposing to 8 Torr H O S7
8 C 35 sec 6 sec 5 C Time (second) Time second c sec 75 C Time (second) Figure S11. Integrted res of dsored wter stretching nd ν(oh) increse in fter introducing 8 Torr H O vpor t () C (Figure ), () 5 C (Figure S1) nd (c) 75 C (Figure ). The equilirium time is leled in ech figure. Co-dsorption experiments of H O nd hve lso een performed in t 5 C nd Ni-MOF-7 t C. After exposing -preloded to 8 Torr H O, the nd grdully shifts to 33 cm -1. Fitting the IR nds y Voigt profile in the region 6 to 7 cm -1 shows the components t 35 nd 33 cm -1, which re due to the dsored in the primry open metl sites nd secondry sites fter eing displced y H O molecules. S8
9 ν(oh) in H.1 O Time (sec) Loding 8 Torr H O H O CO 5 C 35 ν s ( ) 33 sec.5 33 After loding H O for 17 s Wvernumer cm Figure S1. () IR sorption spectr of 8 Torr H O dsored into with pre-loded s function of time t 5 C. All referenced to the ctivted MOF in vcuum (< mtorr). The lck line in the ottom shows the sorption spectrum of efore loding wter. () The deconvoluted components fter fitting the totl pek from 6 to 7 cm -1. Figure S13. The cross section of films on KBr pellets in temperture dependent mesurement. Pictures were tken under microscopy. Figure S1. The cross section of Co-MOF-7 films on KBr pellets in temperture dependent mesurement. Pictures were tken under microscopy. To check the reproduciility nd film thickness dependence, we first mesured the wter molecules diffusion time within ~ mm-thick KBr pellets with sme (~ µm) nd different MOF film thicknesses (~ µm nd ~5 µm) y monitoring the ν(oh) nd intensity s function of time. Note tht the thickness of MOF film is controlled y the mount MOF powders nd pplied pressing force. Figure S15 shows tht the trnsport process (dsorption rte nd diffusion time) for H O in smple is the sme (~35 sec) for two different KBr pellets with the sme MOF film thickness (~ µm), which suggests tht our method of mesuring the H O dsorption is reproducile. At higher temperture (75 C), the S9
10 process is sped up (~ sec) in ech pellet (with the sme thickness). Another wter exposure experiment ws done on the smple with thinner MOF film thickness (~5 µm) s shown inn Figure S15. The resulting equilirium time is shorter (~1 sec less) thn tht on the thicker MOF film. MOF film thicknesses on the KBr pellet used in temperture dependent experiment re similr in ech temperture point (see Figure S13 nd Figure S1). It is therefore resonle to compre the equilirium time t different temperture in the quntittive wy. Figure S15. () Evolution of integrted res of ν(oh) nd t room temperture. The spectr were tken t two different pellets with sme thickness. () Evolution of integrted res of ν(oh) nd t 75 C. The spectr were tken t two pellets with different thickness. The Inset shows the cross section of film on KBr pellet. 5. Diffusion of SO, NO in M-MOF-7 (M= Mg, Co, Ni) SO dsorption in SO dsorption in Co-MOF Time (minute) Time (minute) Figure S16. Evolution of integrted res of SO symmetric stretching nd ν(so ) within 1 min. Pnel () shows the results for, while pnel () shows the results for Co-MOF-7 S1
11 NO in Ni-MOF-7 1 NO in Co-MOF Time (minute) Time (minute) Figure S17. Evolution of integrted res of NO stretching nd ν(no) within min. Pnel () shows the results for Ni-MOF- 7, while pnel () shows the results for Co-MOF nd H O dsorption in Ni-MOF Ni-MOF-7 C 19 min 1 min 8 min min Figure S18. IR sorption spectr of desorption from Ni-MOF-7 s function of time t C (fter the cell is evcuted for 1 h)..1 Time (sec) Loding 8 Torr H O Under vcuum Ni-MOF-7 C ν s ( ) 31 s Time (second) Figure S19. () IR sorption spectr of 8 Torr H O dsored into Ni-MOF-7 with pre-loded s function of time t room temperture. All referenced to the ctivted MOF in vcuum (< mtorr). The lck line in the ottom shows the sorption spectrum of efore loding wter. () Evolution of integrted res of the IR nds of wter ν(oh), lck nd ν s ( ), red over ~ sec in Ni-MOF ν(oh) in H O ν s ( ) S11
12 7. NO dsorption in the pre-loded nd clen Ni-MOF-7 The integrted res of dsored NO nd in 1838 cm -1 were compred fter loding NO t ~5 Torr for ~ min (sufficient to rech stedy stte, see Figure 17) in i) clen MOF nd ii) MOF pre-loded with t 8 Torr on the smple pellet. As we cn see in Figure S, the NO uptke is much less (i.e., ~%) compred to the dsorption in the empty MOFs, which is pprently due to the fct tht the pre-dsored locks the NO molecules occupying the open metl sites. This is lso n indirect evidence tht NO cnnot effectively displce pre-dsored..5 + NO ~6% NO NO lone.5 Pure NO dsorption in Ni-MOF-7 18 Figure S. IR spectr of NO dsorption in Ni-MOF-7 in the clen (lck) nd pre-loded (red) smple. Before introducing NO to MOFs with pre-loded (red), the cell ws evcuted for 1 h. The ottom spectrum (dsh line) shows the gs phse NO spectrum fter introducing 5 Torr NO for ~ min in the clen smple. 8. NO in M-MOF-7 (M= Mg, Co) For the experiment of NO, the ws loded in Mg, Co-MOF-7 t 8 Torr nd evcuted for 1 h until the residul pressure in the cell decresed elow mtorr. Since NO is quite rective within MOF-7, to ensure tht the crystl structure of MOFs smples is not destroyed y NO, Torr NO ws introduced into the cell nd the spectr were recorded for 1 min. As shown in Figure S1 for M-MOF-7 (M= Mg, Co), the nitrte species were oserved t 1516, 193, 11 cm -1 in nd t 178, 193 nd 13 cm -1 in Co-MOF-7. 1 The intensities of these nds incresed once the smple ws exposed to NO gs, chrcterized y gs phse stretching modes t 1617 cm -1 (ν s ) nd 165 cm -1 (ν s ). The 1687 cm -1 oserved in nd 1669 cm -1 in Co-MOF-7 nds re ttriuted to the dsored NO species The 175 cm -1 nd is due to N O nds co-existing in equilirium with NO. 18,19 Correspondingly, the dsored NO species cn e seen t 179 cm -1 in Co-MOF-7. Figure 19 lso shows time-dependent IR sorption spectr of pre-dsored upon NO exposure. The sorption nds ν s ( ) remin mostly unffected in oth nd Co-MOF-7 fter 1 min NO exposure. This cn e confirmed y the differentil spectrum on the top of the figure, otined y sutrcting the spectr efore NO exposure (see the lck spectr in the ottom in Figure 1 nd 1) from those otined fter NO exposure for 1 min nd evcution (see the light lue spectr for Figure 1 nd drk yellow spectr for Figure 1 fter evcution of gs phse). S1
13 Differentl spectr(fter NO-efore NO) Differentl spectr (After NO - Before NO ). C 1 min 7 min min ν s ( ) - (NO CO 3 ) + NO NO (d) Evcution C 1 min 7 min min ν s ( ) Co-MOF-7 + NO (NO - NO(d) NO 3 ) (d) Evcution min.5 min Under vcuum Loding Torr NO ν s N O (g) NO 39 (g) ν s Under vcuum 31 Loding Torr NO ν s NO (g) ν s Figure S1. IR sorption spectr of ctivted () Mg, () Co-MOF-7 with pre-loded molecules exposing to Torr NO. The lck spectrum in the ottom correspond to the MOFs with in vcuum (< mtorr) nd the top one refers to the spectrum fter evcution of residul NO gs for sec. The remining spectr re the time-dependent spectr under the NO gs phse. All the spectr referenced to the ctivted MOF in vcuum except the differentil spectr shown on the top, which re otined y sutrcting the spectr efore Torr NO exposure from the spectr fter evcuting Torr NO gs phse. 9. Co-dsorption of NH 3 nd in In mnner similr to wht ws done with the molecules discussed ove, we further tested the co-dsorption of with NH 3 to compre with H O under vcuum decrese After exposing to 8 Torr H O Time (min) Figure S. Integrted res of ν 3 ( ) nd decreses in vcuum (< mtorr; drk yellow) nd 5 Torr NH 3 (light lue) in t C 1. Co-dsorption of mixture gses of + SO nd + NH 3 Gs mixtures of + SO nd + NH 3 ws introduced to the clen t low pressure (~9 Torr + ~9 Torr SO or NH 3 ) nd compred the dsorption of 9 Torr pure gs in the sme smple. Figure S3 shows the spectr fter loding pure nd mixtures (top) fter sutrction of gs phse gs phse (ottom). The dsored nd is S13
14 oserved t 35 cm -1. The dsored SO cn e chrcterized y ν s (SO ) nd ν s (SO ) t 13 nd 11 cm -1. The dsored NH 3 cn e seen t 111 cm -1,in spectrl region (1 to 16 cm -1 ) overlpping with the MOF phonon modes, which re pertured upon dsorption. The spectroscopic results shows tht dsorption upon exposure to mixtures of oth + SO nd + NH 3 for ~ min (long enough to rech equilirium), is much less compred to tht of pure, i.e., the integrted res of nd decresed y ~5% for + SO nd ~% for NH 3 +. These results re consistent with the hypothesis tht, once dsored, cnnot e removed y SO, nd little y NH 3 within the time of the mesurements. It is difficult to determine if the higher inding energy of SO compred to NH 3 is responsile for higher competitive uptke (less dsored in SO thn in NH 3 mixtures) or just its higher diffusivity in the MOF (Figure. 8 nd S16), ut clerly the dsored remins stle. From the spectroscopic results nd DFT clcultions, we cn conclude tht SO molecules cnnot efficiently replce pre-existing t the open metl sites. However if SO or NH 3 molecules lredy occupy the metl sites, they effectively prevent dditionl dsorption cm -1 lone CO in mixture with SO o C dsored SO.3 35 cm -1 CO lone CO in mixture with NH 3 o C dsored NH 3. Adsored species ν s ( ) + SO Gs phse ν s (SO ). Adsored species ν s ( ) + NH 3 Gs phse Figure S3. IR spectr of dsorption in ctivted for gs mixtures (lck spectr) with ) SO (9 Torr) nd ) NH 3 (9 Torr), compred to the dsorption in pure phse (9 Torr, red), recorded fter ~ min of gses exposures. 11. SO dsorption into Tle S3. Adsorption energies E (in kj/mol) of SO in. Es is lso given corrected y the ZPE nd therml contriution of H t 98 K. O M re the intermoleculr ond-length OSO Mg + -(MOF-7) in Å. Model Loding E E ZPE H 98 O M MOF-7-Mg Mg-O-S-O 1/ Co-dsorption of nd N, O, CH in Adsorption of non-polr molecules such s N, O, nd CH hs een studied y experimentl techniques such s vriletemperture infrred spectroscopy (VTIR), isotherms nd first principle clcultion in M-MOF-7 (M= Mg, Zn, Ni, Co, Mn, Fe). 1-3 Similr to other molecules, the coordintively unsturted metl center is the primry dsorption site for these molecules s well. N nd CH re only wekly dsored in these mterils with hets of dsorption less thn 3 kj/mol derived y VTIR or isotherm. 1, O is chrcterized y lrger het of dsorption (1 kj/mol) in Fe-MOF-7 medited y electron trnsfer interction forming superoxo species in Fe + sites. No ville dt cn e found for O dsorption in S1
15 other M-MOF-7 (M= Mg, Co, Ni). However, due to non-redox rection etween O nd Mg +, Ni + nd Co + t room temperture, the het of dsorption for O in these compounds is expected to e lower thn tht in Fe-MOF-7. Pressure dependence experiments were crried out to study the effect of loding N, O nd CH on the pre-dsored in Mg- MOF-7 y incresing the pressure grdully up to 99 Torr s shown in Figure S, S5, S6. None of them shows tht the spectr of pre-dsored re significntly ffected y loding these gses, indicting tht pre-existing cnnot e removed y N, O, nd CH Co-MOF Evcution 96 Torr 69 Torr 3 Torr Torr Evcution 99 Torr 85 Torr 687 Torr 7 Torr 6 Torr Figure S. IR sorption spectr of ctivted M-MOF-7 (M= Mg, Co) with pre-loded exposing to N s function of pressure (within 15 min). Differentil spectr shown on the top were otined y sutrcting the spectr efore N gs exposure from the spectr fter evcution of N gs exposure. Co-MOF Evcution 98 Torr 7 Torr 5 Torr 5 Torr Evcution 99 Torr 877 Torr 566 Torr 5 Torr Figure S5. IR sorption spectr of ctivted Mg, Co-MOF-7 with pre-loded exposing to O s function of pressure (within 15 min). Differentil spectr shown on the top were otined y sutrcting the spectr efore O gs exposure from the spectr fter evcution of O gs exposure. S15
16 Differentil spectr (fter CH to efore CH ).1 99 Torr 617 Torr 398 Torr Torr Evcution + CH 316 CH (g) ν s After loding CH Under vcuum 35 ν s ( ) Differentil spectr (fter CH to efore CH ).1 Co-MOF-7 31 ν + CH s ( ) Evcution CH (g) 99 Torr 88 Torr 67 Torr Torr 78 Torr After loding CH 316 Under vcuum Figure S6. IR sorption spectr of ctivted () Mg, () Co-MOF-7 with pre-loded exposing to CH s function of pressure (within ~15 min). Differentil spectr shown on the top were otined y sutrcting the spectr efore CH gs exposure from the spectr fter evcution of CH gs exposure. 13. The frequencies of t metl site nd t the secondry site According to experiments shown in Figure, nd 8, there is shift of -7(±1) cm -1 in the virtion frequency of the dsored molecule when H O, SO, or NH 3 is introduced into the system. In order to understnd this effect we hve clculted the virtion frequency of the dsored molecule t the metl center, nd compre it to the virtion frequency of the molecule when the molecule hs een displced from the metl center (see Figure 1) y the wter molecule. This ws done for two different lodings: six molecules plus one molecule of wter (high loding), nd one molecule plus one molecule of wter (low loding). Our results (see Tle S3) re in good greement with experimentl mesurements, indicting red shift of -9 cm -1 nd -1 cm -1 for the low nd high loding cses, respectively. This indictes tht the frequency shift of the displced depends on the occuption of other open metl sites. The simulted frequency shift further confirms our oservtion nd ssignment tht with 3(, 3, ) cm -1 sorption is locted t the secondry sites. Tle S. The frequencies of displced in the secondry sites within. Co-dsored molecules lone + H O Loding per unit cell Clculted vlue (cm -1 ) 1/ / / / Frequency shift (cm -1 ) 1. H O nd SO in S16
17 Figure S7. Top pnels: The nd t 35 cm -1 decrese in s function of time fter H O (Figure ) nd SO (Figure 6) exposure t C. Bottom pnel: rtio of velocity of the desorption. The ctivtion energies lone re not enough to derive the exchnge rtes. However, the rtio of exchnge rte constnt cn e estimted y the Arrhenius eqution, ssuming tht the pre-fctor A of Arrhenius eqution is the sme for the exchnge rection of pre-loded y H O nd SO : = The DFT results indicte tht H O exchnge process hs rte of 17 greter thn the SO t room temperture. Considering tht the dsorption of H O nd SO tkes similr time to rech equilirium (see Figure S11 nd S16), the rtio mesured y spectroscopy cn e estimted y compring the rte of decrese of nds t 35 cm -1 upon H O nd SO exposure, respectively. Reference: (1) Dietzel, P. D. C.; Johnsen, R. E.; Fjellvg, H.; Bordig, S.; Groppo, E.; Chvn, S.; Blom, R. Chem. Commun. 8, 515. () Lee, J. Y.; Olson, D. H.; Pn, L.; Emge, T. J.; Li, J. Adv. Funct. Mter. 7, 17, 155. (3) Dietzel, P. D. C.; Blom, R.; Fjellvåg, H. Eur. J. Inorg. Chem. 8, 8, 36. () Cskey, S. R.; Wong-Foy, A. G.; Mtzger, A. J. J. Am. Chem. Soc. 8, 13, 187. (5) Dietzel, P. D. C.; Besikiotis, V.; Blom, R. J. Mter. Chem. 9, 19, 736. (6) Perry, J. J.; Teich-McGoldrick, S. L.; Meek, S. T.; Grethouse, J. A.; Hrnczyk, M.; Allendorf, M. D. J. Phys. Chem. C. 1, 118, (7) Yng, D.-A.; Cho, H.-Y.; Kim, J.; Yng, S.-T.; Ahn, W.-S. Energy Environ. Sci. 1, 5, 665. (8) Li, L.; Yng, J.; Li, J.; Chen, Y.; Li, J. Microporous Mesoporous Mter. 1, 198, 36. (9) Britt, D.; Trnchemontgne, D.; Yghi, O. M. Proc. Ntl. Acd. Sci. 8, 15, (1) Wu, X.; Bo, Z.; Yun, B.; Wng, J.; Sun, Y.; Luo, H.; Deng, S. Microporous Mesoporous Mter. 13, 18, 11. (11) Bo, Z.; Yu, L.; Ren, Q.; Lu, X.; Deng, S. J. Colloid Interfce Sci. 11, 353, 59. (1) Yzydın, A. O. z. r.; Snurr, R. Q.; Prk, T.-H.; Koh, K.; Liu, J.; LeVn, M. D.; Benin, A. I.; Jkuczk, P.; Lnuz, M.; Gllowy, D. B.; Low, J. J.; Willis, R. R. J. Am. Chem. Soc. 9, 131, (13) Liu, J.; Benin, A. I.; Furtdo, A. M. B.; Jkuczk, P.; Willis, R. R.; LeVn, M. D. Lngmuir 11, 7, S17
18 (1) Nkmoto, K. Infrred nd Rmn Spectr of Inorgnic nd Coordintion Compounds, 6th ed. Wiley & Sons, Inc.,Hooken, New Jersey, United Sttes. 9. (15) Hdjiivnov, K.; Klissurski, D.; Rmis, G.; Busc, G. Appl. Ctl., B 1996, 7, 51. (16) Djonev, B.; Tsyntsrski, B.; Klissurski, D.; Hdjiivnov, K. J. Chem. Soc., Frdy Trns. 1997, 93, 55. (17) Hdjiivnov, K. I. Microporous Mesoporous Mter 1998,, 1. (18) Guttmn, A.; Penner, S. S. J. Chem. Phys 196, 36, 98. (19) Schffert, R. J. Chem. Phys 1933, 1, 57. () Tn, K.; Zulug, S.; Gong, Q.; Cnep, P.; Wng, H.; Li, J.; Chl, Y. J.; Thonhuser, T. Chem. Mter. 1, 6, (1) Vlenzno, L.; Civlleri, B.; Chvn, S.; Plomino, G. T.; Areán, C. O.; Bordig, S. J. Phys. Chem. C 1, 11, () Wu, H.; Zhou, W.; Yildirim, T. J. Am. Chem. Soc. 9, 131, 995. (3) Bloch, E. D.; Murry, L. J.; Queen, W. L.; Chvn, S.; Mximoff, S. N.; Bigi, J. P.; Krishn, R.; Peterson, V. K.; Grndjen, F.; Long, G. J.; Smit, B.; Bordig, S.; Brown, C. M.; Long, J. R. J. Am. Chem. Soc. 11, 133, 181. S18
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