Supplementary Information for. Exploring the Capacity Limit: A Layered. Hexacarboxylate-based Metal-Organic Framework for. Advanced Lithium Storage

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1 Supplementary Information for Exploring the Capacity Limit: A Layered Hexacarboxylate-based Metal-Organic Framework for Advanced Lithium Storage Xiaobing Lou, Yanqun Ning, Chao Li, Ming Shen, Bei Hu, Xiaoshi Hu, and Bingwen Hu* State Key Laboratory of Precision Spectroscopy, Shanghai Key Laboratory of Magnetic Resonance, School of Physics and Materials Science, East China Normal University, Shanghai , China. Address correspondence to (B.W.H) bwhu@phy.ecnu.edu.cn. Table of contents 1. Figure S1: Optical micrograph of the Ni-BHC crystal. 2. Table S1: The reported MOFs or CPs materials for LIBs anode. 3. Figure S2: XRD patterns of the annealed Ni-BHC at 800 C. 4. Scheme S1: Schematic diagram of the evacuated and re-established processes of Ni-BHC. 5. Figure S3: SEM micrographs of Ni-BHC and evacuated Ni-BHC. 6. Figure S4: Galvanostatic charge-discharge profiles of evacuated Ni-BHC, Ni-BHC and mellitic acid. 7. Figure S5: Charge-discharge profiles of the evacuated Ni-BHC at various rates. 8. Figure S6: The cyclic voltammetry curves of evacuated Ni-BHC and Ni-BHC. 9. Supplementary references.

2 Figure S1 Optical micrograph of the Ni-BHC crystal.

3 Table S1. MOFs or CPs materials for LIBs anode. Year Materials Performances Refs 2006 MOF mah g -1 at 50 ma g 1 for 2 cycles Zn 3 (HCOO) 6 Co 3 (HCOO) 6 Zn 1.5 Co 1.5 (HCOO) 6 Ni-NTC Li-NTC Li/Ni-NTC Mn-LCP [Li 6 (pda) 3 ] 2EtOH Co 2 (OH) 2 BDC Cu-BDC Mn(3,5-PDC) 2H 2 O Mn 2,5-furandicarboxylate Mn 2 (C 6 H 2 O 4 S) 2H 2 O Ni Me 4 bpz CoC 6 H 2 O 5 (H 2 O) 2 Ni-BDC Mn-BTC Asp-Cu Zn(IM) 1.5 (abim) 0.5 Zn-MOF-Crown Zn-TCPB [Pb(4,4-opybz)(4,3-opybz)] 3DMF 7 H 2 O CoCOP Zn-LCP 560 mah g -1 at 60 ma g 1 for 60 cycles 410 mah g -1 at 60 ma g 1 for 60 cycles 510 mah g -1 at 60 ma g 1 for 60 cycles 248 mah g -1 at 100 ma g 1 for 80 cycles 468 mah g -1 at 100 ma g 1 for 80 cycles 482 mah g -1 at 100 ma g 1 for 80 cycles 390 mah g -1 at 50 ma g 1 for 50 cycles 164 mah g -1 at 30 ma g 1 for 50 cycles 650 mah g -1 at 50 ma g 1 for 100 cycles 161 mah g -1 at 48 ma g 1 for 50 cycles 554 mah g -1 at 100 ma g 1 for 240 cycles mah g -1 at 100 ma g 1 for 206 cycles mah g -1 at 400 ma g 1 for 250 cycles 120 mah g -1 at 50 ma g 1 for 100 cycles mah g -1 at 100 ma g 1 for 99 cycles 620 mah g -1 at 100 ma g 1 for 100 cycles 694 mah g -1 at 100 ma g 1 for 100 cycles 233 mah g -1 at 50 ma g 1 for 200 cycles 190 mah g -1 at 100 ma g 1 for 200 cycles 239 mah g -1 at 500 ma g 1 for 500 cycles 455 mah g -1 at 100 ma g 1 for 100 cycles 405 mah g -1 at 100 ma g 1 for 100 cycles 920 mah g -1 at 100 ma g 1 for 50 cycles 632 mah g -1 at 50 ma g 1 for 100 cycles [Co(H 2 O) 6 ][Co 6 (bpybdc) 2 (N 3 ) 1 0(H 2 O) 4 ] 8H 2 O Zinc 2,6-pyridilinedicarboxylate UiO-66 [Co 1.5 L(H 2 O) 4 ] n Co-LCP Cd-TTPCA Cu-BTC Fe(Zn)-BDC Co-BTC MOF CoBTC-EtOH MnCo-BTC Mn-BDC Co-BDC MOF 510 mah g -1 at 100 ma g 1 for 200 cycles mah g -1 at 100 ma g 1 for 80 cycles 118 mah g -1 at 38.8 ma g 1 for 30 cycles 431 mah g -1 at 50 ma g 1 for 10 cycles 545 mah g -1 at 50 ma g 1 for 50 cycles 302 mah g -1 at 100 ma g 1 for 100 cycles 474 mah g -1 at 383 ma g 1 for 50 cycles mah g -1 at 100 ma g 1 for 120 cycles 750 mah g -1 at 100 ma g 1 for 200 cycles 856 mah g -1 at 100 ma g 1 for 100 cycles 901 mah g -1 at 100 ma g 1 for 150 cycles 974 mah g -1 at 100 ma g 1 for 100 cycles 1090 mah g -1 at 200 ma g 1 for 100 cycles

4 2017 Co-BDC Fe-BDC Fe-BTC BiCPs Co(L) MOF/RGO Co-TFBDC Co 2 (ade) 2 (V 4 O 12 )(H 2 O) 2 Cd 2 (ade) 2 (V 4 O 12 )(H 2 O) 2 Co 2 (DOBDC) ZIF-8 ZIF-67 Co(OH)(OCH 3 ) M-IOHCs CoHNta Co 3 (L 1 )(N 3 ) 4 [Mn 2 (L 1 )(N 3 ) 2 (H 2 O) 2 ] 3H 2 O [Co 4 L 2 (N 3 ) 6 (H 2 O) 2 ] [Mn 4 L 2 (N 3 ) 6 (H 2 O) 2 ] Cobalt 4,5-imidazoledicarboxylate Co 2 (OH) 2 BDC/CGr Co-PTA Evacuated Co-BTC Fe-BTP Mn-NDC Cd-NDC Pb-MOF 1021 mah g -1 at 100 ma g 1 for 200 cycles mah g -1 at 500 ma g 1 for 200 cycles 1021 mah g -1 at 100 ma g 1 for 100 cycles 1211 mah g -1 at 100 ma g 1 for 100 cycles 1185 mah g -1 at 100 ma g 1 for 50 cycles mah g -1 at 100 ma g 1 for 50 cycles 410 mah g -1 at 50 ma g 1 for 80 cycles 485 mah g -1 at 50 ma g 1 for 80 cycles mah g -1 at 100 ma g 1 for 100 cycles mah g -1 at ma g 1 for 70 cycles mah g -1 at 24 ma g 1 for 70 cycles 1150 mah g -1 at 100 ma g 1 for 160 cycles 1043 mah g -1 at 200 ma g 1 for 450 cycles 875 mah g -1 at 500 ma g 1 for 300 cycles 580 mah g -1 at 100 ma g 1 for 200 cycles 358 mah g -1 at 100 ma g 1 for 200 cycles 595 mah g -1 at 100 ma g 1 for 200 cycles 595 mah g -1 at 100 ma g 1 for 200 cycles mah g -1 at 1000 ma g 1 for 143 cycles 818 mah g -1 at 1000 ma g 1 for 400 cycles 692 mah g -1 at 60 ma g 1 for 107 cycles mah g -1 at 100 ma g 1 for 120 cycles 550 mah g -1 at 80 ma g 1 for 25 cycles mah g -1 at 200 ma g 1 for 300 cycles mah g -1 at 200 ma g 1 for 300 cycles 489 mah g -1 at 100 ma g 1 for 500 cycles F-MOF mah g -1 at 100 ma g 1 for 100 cycles 54 [Ni(4,4 -bpy)(tfbdc)(h 2 O) 2 ] 406 mah g -1 at 50 ma g 1 for 50 cycles 55 MIL-88B(Fe) 680 mah g -1 at 200 ma g 1 for 500 cycles 56 Fe-MIL-88B mah g -1 at 60 ma g 1 for 400 cycles 57 Co-TDC 946 mah g -1 at 100 ma g 1 for 100 cycles 58 Zn-ODCP 300 mah g -1 at 50 ma g 1 for 50 cycles 59 MIL-53(Fe)@RGO 530 mah g -1 at 100 ma g 1 for 100 cycles 60 Mn-UMOFNs 1187 mah g -1 at 100 ma g 1 for 100 cycles Co-BDCN CoZn-ZIF 1132 mah g -1 at 100 ma g 1 for 100 cycles mah g -1 at 100 ma g 1 for 100 cycles 62 63

5 C NiO PDF# Intensity (a.u.) Theta (degree) Figure S2 XRD patterns of the annealed Ni-BHC at 800 C, which shows that the annealing product is NiO.

6 Scheme S1 Schematic diagram of the evacuated and re-established processes of Ni-BHC.

7 Figure S3 SEM micrographs of Ni-BHC (a, c and e) and evacuated Ni-BHC (b, d and f) at different magnification. The columnar bulk shows high quality of the Ni-BHC crystal corresponding to its chained-layer microstructure. Quite similar morphology of evacuated Ni-BHC makes it possible that Ni-BHC can re-established upon soaking in water.

8 (a) 3.0 Voltage (V vs. Li/Li + ) st 2nd (b) 0.0 Current Density: 100 ma g Capacity (ma h g -1 ) Voltage (V vs. Li/Li + ) st 2nd (c) 0.0 Current Density: 100 ma g Capacity (ma h g -1 ) Voltage (V vs. Li/Li + ) st 2nd 0.0 Current Density: 100 ma g Capacity (ma h g -1 ) Figure S4 Galvanostatic charge-discharge profiles of evacuated Ni-BHC (a), Ni-BHC (b) and mellitic acid (c) at a current density of 100 ma g -1. The initial two charge-discharge profiles of the three materials are plotted here. It can be seen that the evacuated Ni-BHC electrode exhibits a wide plateau at about 1.5V following by a slope during the first discharge. In the subsequent cycles, the discharge plateau disappeared, demonstrating the formation of SEI films in the first cycle and the activation of the MOF electrode. The Ni-BHC shows similar profiles, while the charge and discharge capacities are

9 relatively lower, indicating a performance-suppression effect of the lattice waters in Ni-BHC structure. For the mellitic acid linker, the charge-discharge profiles are different from that of the MOF and the capacities are quite low, suggesting its negligible electrochemical activity. The initial coulombic efficiencies for evacuated Ni-BHC, Ni-BHC and mellitic acid are 74.17%, 62.44% and 48.86%, demonstrating the higher capability of the evacuated Ni-BHC as superior anode for Li-ion battery. 3.0 Voltage (V vs. Li/Li + ) ma g ma g ma g ma g ma g ma g Capacity (ma h g -1 ) Figure S5 Representative charge-discharge profiles of the evacuated Ni-BHC at various rates. (Voltage window: V)

10 (a) Current (ma) st 2nd Scan Rate: 0.2 mv s -1 (b) Voltage (V vs. Li/Li + ) 0.4 Current (ma) st 2nd Scan Rate: 0.2 mv s Voltage (V vs. Li/Li + ) Figure S6 The cyclic voltammetry curves of (a) evacuated Ni-BHC and (b) Ni-BHC at a scan rate of 0.2 mv s -1 for the first two cycles. A strong cathodic peak located around 1.50 V at the initial cycle could be attributed to the Li intercalation into carboxylated oxygen accompanying by the formation of solid electrolyte interface (SEI). Another cathodic peak centered at 0.62 V indicating a further lithiation of the carboxylate-metal units. The two corresponding anodic peaks at the first cycle were centered at 1.4 and 2.0 V. At the second cycle, the cathodic peaks respectively shift to 1.72 and 0.77 V, while the anodic peak shift to 1.34 and 2.03 V due to the structural modifications of MOF during the first cycle. The CV curves of Ni-BHC are plotted in Figure S6b. For the involving of crystal water in the lithiation-delithiation processes, all peaks get broad indicating a slower kinetic process.

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