Preparation of endohedral fullerene containing lithium 60 ) and isolation as pure hexafluorophosphate salt ([Li 60 ][PF 6 ])

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1 This journal is The Royal Society of Chemistry 212 Supplementary Information Preparation of endohedral fullerene containing lithium ) and isolation as pure hexafluorophosphate salt ([Li ][PF 6 ]) Hiroshi Okada, a,b Takashi Komuro, a Takeshi Sakai, c,d Yutaka Matsuo, b Yoshihiro Ono, e Kenji Omote, e Kuniyoshi Yokoo, e Kazuhiko Kawachi, f Yasuhiko Kasama, f Shoichi Ono, f Rikizo Hatakeyama, g Toshiro Kaneko, g Hiromi Tobita a, * a Department of Chemistry, Graduate School of Science, Tohoku University, Sendai , Japan b Department of Chemistry, School of Science, The University of Tokyo, Tokyo , Japan c New Industry Creation Hatchery Center, Tohoku University, Sendai, , Japan d Foundation for Advancement of International Science, Tsukuba, 5-62, Japan e ideal star inc., Minamiyoshinari, Aoba-ku, Sendai , Japan f Idea International Corporation, Aramaki-Aza-Aoba Aoba-ku, Sendai , Japan g Department of Electronic Engineering, Graduate School of Engineering, Tohoku University, Sendai , Japan tobita@m.tohoku.ac.jp S1

2 This journal is The Royal Society of Chemistry 212 Contents Fig. S1. LDI-TOF mass spectra of -enriched brown solid (B)... p.s3 Fig. S2. Dynamic light scattering of -enriched brown solid (B) and empty C... p.s4 Fig. S3. LDI-TOF mass spectra of ]][PF 6 ]... p.s5 Fig. S4. A 7 Li NMR spectrum of [Li@C ]][PF 6 ]... p.s6 Fig. S5. A 13 C{ 1 H} NMR spectrum of [Li@C ]][PF 6 ]... p.s7 S2

3 This journal is The Royal Society of Chemistry 212 Fig. S1. LDI-TOF mass spectra of -enriched brown solid (B) in the range of m/z 6 to. (a) Linear positive mode and (b) reflectron negative mode. %Int. 1 a 277 mv[sum= mv] Profiles 1-1 Smooth Gauss 7 -Baseline 21 %Int. 693 mv[sum= 693 mv] Profiles 1-1 Smooth Gauss 7 -Baseline %Int. 1 b 1 mv[sum= 127 mv] Profiles 1-1 Smooth Gauss 7 -Baseline 21 %Int. 1 mv[sum= 127 mv] Profiles 1-1 Smooth Gauss 7 -Baseline S3

4 This journal is The Royal Society of Chemistry 212 Fig. S2. Dynamic light scattering of 1-chloronaphthalene solutions of (a) -enriched brown solid (B) and (b) C. a b S4

5 This journal is The Royal Society of Chemistry 212 Fig. S3. LDI-TOF mass spectra of [Li ][PF 6 ]. (a) Reflectron positive mode and (b) reflectron negative mode. The spectra in the range of m/z to are shown in the inset. Data: OxAm-H23solution_LP_posi_ref1 22 May29 13:29 Cal: 19 Feb 21 11:1 %Int. 62mV[sum=619mV] Profiles 1-1SmoothAv2 -Baseline 1 2 a Data: OxAm-H23solution_LP_posi_ref1 22 May29 13:29 Cal: 19 Feb 21 11:1 %Int. 171 mv[sum= 1718 mv] Profiles 1-1 Smooth Av 2 -Baseline Data: OxAm-H23solution_LP87_neg_ref1 22 May29 13:38 Cal: 19 Feb 21 11:4 %Int. 1523mV[sum=152297mV] Profiles 1-1SmoothAv2 -Baseline 1 b Data: OxAm-H23solution_LP87_neg_ref1 22 May29 13:38 Cal: 19 Feb 21 11:4 %Int. 77 mv[sum= 77 mv] Profiles 1-1 Smooth Av2 -Baseline S5

6 This journal is The Royal Society of Chemistry 212 Fig. S4. A 7 Li NMR spectrum of [Li ][PF 6 ] (117 MHz, o-dichlorobenzene-d 4 /acetonitrile-d 3 = 1/1). Current Data Parameters NAME OI1-7Li EXPNO 1 PROCNO 1 F2 - Acquisition Parameters Date_ 22 Time INSTRUM av PROBHD 5 mm BBO BB-1H PULPROG zg TD SOLVENT CD3CN NS 2616 DS 2 SWH Hz FIDRES Hz AQ sec RG 256 DW 17.2 usec DE 6. usec TE. K D1. sec ======== CHANNEL f1 ======== NUC1 7Li P usec PL1 5. db SFO MHz F2 - Processing parameters SI SF MHz WDW EM SSB LB 1. Hz GB PC ppm S6

7 This journal is The Royal Society of Chemistry 212 Fig. S5. A 13 C{ 1 H} NMR spectrum of [Li ][PF 6 ] (151 MHz, o-dichlorobenzene-d 4 /acetonitrile-d 3 = 1/1). The spectrum in the range of 12 to 1 ppm is shown in the inset [Li + C] * * Current Data Parameters NAME I.S-4 EXPNO 3 PROCNO 1 F2 - Acquisition Parameters Date_ 291 Time INSTRUM av PROBHD 5 mm BBO BB-1H PULPROG zgpg TD SOLVENT C6D6 NS DS 4 SWH Hz FIDRES Hz * DW DE 11. usec 6. usec AQ sec * RG ppm * TE. K D1 2. sec d11. sec d12.2 sec ======== CHANNEL f1 ======== NUC1 13C P1 9. usec PL1. db SFO MHz ======== CHANNEL f2 ======== CPDPRG2 waltz16 NUC2 1H PCPD2. usec PL2-1. db PL db PL db SFO MHz F2 - Processing parameters SI SF MHz WDW EM SSB LB 1. Hz GB PC ppm *: solvents S7