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      "caption": "Fig. 1 | Structural characterization and electrochemical data for Li 1.2 Ni0.13 Co0.13 Mn0.54 O2. a , Li 1.2 Ni0.13 Co0.13 Mn0.54 O2 with a layered R 3m structure, in-plane ordering of Li/Ni and Co/Mn giving rise to the honeycomb superstructure ordering. Li atoms are represented in blue, TM in purple and oxygen in red. b , PXRD data and refinement to the R 3m crystal structure. c , Load curves for Li 1.2 Ni0.13 Co0.13 Mn0.54 O2, cycled between 2.0 V and 4.8 V at 100 mA g -1 for 100 cycles.",
      "caption_preview": "Fig. 1 | Structural characterization and electrochemical data for Li 1.2 Ni0.13 Co0.13 Mn0.54 O2. a , Li 1.2 Ni0.13 Co0.13 Mn0.54 O2 with a layered R 3m structure, in-plane ordering of Li/Ni and Co/Mn giving rise to the…",
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      "caption": "Fig. 2 | Evolution in bulk O-redox activity over 2nd and 100th cycles. a , d , Load curves for the 2nd ( a ) and 100th ( d ) cycles for Li 1.2 Mn0.54 Co0.13 Ni0.13 O2, with the states of charge studied. b , e , RIXS spectra at 531.5 eV collected over the 2nd ( b ) and 100th ( e ) cycles. c , f , Variation in intensity of the molecular O 2 signal in the RIXS spectra over the 2nd ( c ) and 100th ( f ) cycles, as determined by principal component analysis (Methods). Data are presented as mean ± standard deviation with a sample size of 15. P, pristine.",
      "caption_preview": "Fig. 2 | Evolution in bulk O-redox activity over 2nd and 100th cycles. a , d , Load curves for the 2nd ( a ) and 100th ( d ) cycles for Li 1.2 Mn0.54 Co0.13 Ni0.13 O2, with the states of charge studied. b , e , RIXS spe…",
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      "caption": "Fig. 3 | Evolution in amount of trapped O 2 over cycling. Variation in intensity of the molecular O 2 signal from RIXS over cycling in the fully charged (FC) and fully discharged (FD) states. The amount of O 2 formed in the charged materials decreases with cycling and there is increasing evidence of O 2 that is not reduced on discharge. Data are presented as mean ± standard deviation with a sample size of 15.",
      "caption_preview": "Fig. 3 | Evolution in amount of trapped O 2 over cycling. Variation in intensity of the molecular O 2 signal from RIXS over cycling in the fully charged (FC) and fully discharged (FD) states. The amount of O 2 formed in…",
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      "caption": "Fig. 4 | Formation of voids and large diamagnetic Li-rich regions over cycling. a -c , ADF-STEM images showing single grains of the pristine ( a ), 2nd discharge ( b ) and 100th discharge ( c ) material showing the formation of voids about 4-12 nm in diameter over extended cycling. d , 129 Xe NMR experiments. Samples were extracted from cells and infiltrated with Xe gas to probe the open porosity. e , 129 Xe NMR of the pristine, 2nd discharge and 100th discharge materials. The orange region highlighted indicates the presence of open voids of 17 nm diameter and greater after 100 cycles. δ iso , isotropic chemical shift. f , g , 6 Li ( f ) and 17 O ( g ) NMR isolating slow and fast relaxing environments. The sharp peaks at 0 ppm in the 6 Li and slow relaxing 17 O NMR spectra indicate the formation of large diamagnetic Li-rich regions on extended cycling.",
      "caption_preview": "Fig. 4 | Formation of voids and large diamagnetic Li-rich regions over cycling. a -c , ADF-STEM images showing single grains of the pristine ( a ), 2nd discharge ( b ) and 100th discharge ( c ) material showing the form…",
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      "caption": "Fig. 5 | Partial reduction of O 2 trapped in voids to form Li-coordinated O 2on the 100th discharge. a , b , 17 O NMR spectra isolating fast ( a ) and slow ( b ) relaxing 17 O environments. The sharp peaks in a are assigned to trapped molecular O2, which decrease in intensity on discharge. There is still evidence of some residual molecular O 2 in the discharged sample, δ cg ( 17 O2) = 2,770 ppm. In b the slow relaxation 17 O is dominated by oxide environments coordinated to paramagnetic TM ions (TM-O 2-), δ cg = 2,100-2,300 ppm. After discharge, a new 17 O environment is formed corresponding to oxide surrounded by Li (that is, Li-O 2) created by the reduction of O 2 in the voids and reinsertion of Li + into the voids coordinated by the O 2, centred at δ cg = 0 ppm. D 1 , relaxation delay. c , Large voids accommodating O2 are partially repopulated by Li + on discharge. Most O 2 is reduced to O 2but some residual O 2 remains.",
      "caption_preview": "Fig. 5 | Partial reduction of O 2 trapped in voids to form Li-coordinated O 2on the 100th discharge. a , b , 17 O NMR spectra isolating fast ( a ) and slow ( b ) relaxing 17 O environments. The sharp peaks in a are assi…",
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