Please do not adjust margins
Dalton Transactions
Page 8 of 9
ARTICLE
Journal Name
(s) ppm. Elemental analysis found (calcd.) (%) for C42H44LaPSeSi
7
8
9
Chem. Eur. J., 2016, 22, 16292–16303.
M. Hatano, Y. Tabata, Y. Yoshida, K. Toh, K. Yamashita, Y.
Ogura and K. Ishihara, Green Chem., 2018, 20, 1193–1198.
S. J. Brown and J. H. Clark, J. Chem. Soc., Chem. Commun.,
1983, 1256.
DOI: 10.1039/D1DT02000E
(825.8 g mol–1): 60.8 (61.0), 5.4 (5.4).
Synthesis of Ph4P[Cp3LaTeSiMe3] (4-Te):
A mixture of
Ph4P[TeSiMe3] (3-Te) (100 mg, 0.185 mmol, 1.0 eq.) and [Cp3La]
(62 mg, 0.185 mmol, 1.0 eq.) was dissolved in thf (10 mL) at -
20°C and heated up to room temperature over 18 h. The
reaction mixture was layered with n-pentane (10 mL) and
stored at –30 °C for a few days obtaining the target compound
as colourless crystals by filtration. Note: Reaction and isolation
was performed under exclusion of light. 1H-NMR (300.13 MHz,
thf-d8): = 7.96-7.92 (m, 4H), 7.80-7.72 (m, 16H), 5.77 (s, 15H,
LaCp3), 0.49 (s, 9H, [TeSiMe3]–). 13C-NMR (75.48 MHz, thf-d8):
= 136.1 (d, 4JPC = 3.1 Hz, 4C), 135.6 (d, 3JPC = 10.5 Hz, 4C), 131.3
(d, 2JPC = 12.9 Hz, 4C), 118.9 (d, 1JCP = 89.4 Hz, 4C), 110.9 (s, 15C),
9.5 (s, 3C, [TeSiMe3]–)).29Si-NMR (99.37 MHz, thf-d8): = –24.0
(s, [TeSiMe3]–) ppm. 139La-NMR (42.41 MHz, thf-d8): -399.9
(broad s) ppm Elemental analysis found (calcd.) (%) for
C42H44LaPSSi (874.4 g mol–1): 57.6 (57.7), 5.0 (5.1).
10 V. Trieu, R. Weber, S. R. Waldvogel, J. Heijl, T. Gieshoff,
WO 2018091370 A1, 2016.
11 J. Guschlbauer, T. Vollgraff and J. Sundermeyer, Dalton
Trans., 2019, 48, 10971–10978.
12 M. Loor, S. Salloum, P. Kawulok, S. Izadi, G. Bendt, J.
Guschlbauer, J. Sundermeyer, N. Perez, K. Nielsch, G.
Schierning and S. Schulz, Inorg. Chem., 2020, 59, 3428–
3436.
13 J. Guschlbauer, T. Vollgraff and J. Sundermeyer, Inorg.
Chem., 2019, 58, 15385–15392.
14 M. R. Russo, N. Kaltsoyannis and A. Sella, Chem. Commun.,
2002, 2458–2459.
15 a) K. Mitchell and J. A. Ibers, Chem. Rev., 2002, 102, 1929–
1952; b) M. W. Degroot and J. F. Corrigan, Z. Anorg. Allg.
Chem., 2006, 632, 19–29.
16 F. Tuna, C. A. Smith, M. Bodensteiner, L. Ungur, L. F.
Chibotaru, E. J. L. McInnes, R. E. P. Winpenny, D. Collison
and R. A. Layfield, Angew. Chem. Int. Ed., 2012, 51, 6976–
6980. Angew. Chem., 2012, 124, 7082–7086.
17 W. Ren, G. Zi, D.-C. Fang and M. D. Walter, J. Am. Chem.
Soc., 2011, 133, 13183–13196.
Conflicts of interest
There are no conflicts to declare.
Acknowledgements
Financial support of the German Research Foundation DFG and
its priority program SPP 1708: “Material Synthesis near Room 18 a) T. Arliguie, M. Blug, P. Le Floch, N. Mézailles, P. Thuéry
Temperature” is gratefully acknowledged. We thank Haowen
Wang and Hui Qu for their synthetic contributions.
and M. Ephritikhine, Organometallics, 2008, 27, 4158–
4165; b) P. C. Leverd, M. Ephritikhine, M. Lance, J. Vigner
and M. Nierlich, J. Organomet. Chem., 1996, 507, 229–
237.
19 a) S. H. Eggers, M. Adam, E. T. Haupt and R. Dieter Fischer,
Inorg. Chim. Acta, 1987, 139, 315–318; b) G. Hanrong, S.
Qi, H. Jingyu, J. Sunchun and L. Yonghua, J. Organomet.
Chem., 1992, 427, 141–149; c) K. Jacob, M. Glanz, K. Tittes,
K.-H. Thiele, I. Pavlik and A. Ly?ka, Z. Anorg. Allg. Chem.,
1989, 577, 145–154; d) C. Qian, B. Wang, Y. Xin and Y. Lin,
J. Chem. Soc., Dalton Trans., 1994, 2109–2112; e) I. P.
Beletskaya, A. Z. Voskoboynikov, E. B. Chuklanova, N. I.
Kirillova, A. K. Shestakova, I. N. Parshina, A. I. Gusev and G.
K. I. Magomedov, J. Am. Chem. Soc., 1993, 115, 3156–
3166; f) G. Bombieri, F. Benetollo, K. W. Bagnall, M. J.
Plews and D. Brown, J. Chem. Soc., Dalton Trans., 1983,
45–49; g) J. G. Brennan, R. A. Andersen and A. Zalkin,
Inorg. Chem., 1986, 25, 1761–1765.
20 C. Bolli, J. Gellhaar, C. Jenne, M. Keßler, H. Scherer, H.
Seeger and R. Uzun, Dalton Trans., 2014, 43, 4326–4334.
21 R. Schwesinger, R. Link, P. Wenzl and S. Kossek, Chem. Eur.
J., 2005, 12, 438–445.
22 H. Schmidbaur, K.-H. Mitschke, W. Buchner, H. Stühler and
J. Weidlein, Chem. Ber., 1973, 106, 1226–1237.
23 D. Mootz and M. Wiebcke, Z. Anorg. Allg. Chem., 1987,
545, 39–42.
References
1
a) J. D. Holbrey, R. D. Rogers, S. S. Shukla and C. D. Wilfred,
Green Chem., 2010, 12, 407–413; b) M. Selva and A.
Perosa, Green Chem., 2008, 10, 457; c) M. Fabris, M. Noè,
A. Perosa, M. Selva and R. Ballini, J. Org. Chem., 2012, 77,
1805–1811; d) T. N. Glasnov, J. D. Holbrey, C. O. Kappe, K.
R. Seddon and T. Yan, Green Chem., 2012, 14, 3071; e) M.
Lissel, Liebigs Ann. Chem., 1987, 1987, 77–79; f) P. Tundo,
Pure Appl. Chem., 2001, 73, 1117–1124; g) M. Lissel, S.
Schmidt and B. Neumann, Synthesis, 1986, 1986, 382–383;
h) A.-A. G. Shaikh and S. Sivaram, Chem. Rev., 1996, 96,
951–976.
2
a) R. Kalb, WO 2008 052 861, 2008; b) R. Kalb, WO 2008
052 860, 2008; c) B. Oelkers and J. Sundermeyer, Green
Chem., 2011, 13, 608-618; d) B. Albert and M. Jansen, Z.
Anorg. Allg. Chem., 1995, 621, 1735–1740.
3
4
R. Kalb, US 8075803 B2, 2004.
L. H. Finger and J. Sundermeyer, Chem. Eur. J., 2016, 22,
4218–4230.
5
6
P. Wasserscheid, ed., Ionic liquids in synthesis, Wiley-VCH,
Weinheim, 2008.
J. D. Holbrey, W. M. Reichert, I. Tkatchenko, E. Bouajila, O.
Walter, I. Tommasi and R. D. Rogers, Chem. Commun.,
2003, 28–29.
24 L. H. Finger, B. Scheibe and J. Sundermeyer, Inorg. Chem.,
2015, 54, 9568–9575.
8 | J. Name., 2012, 00, 1-3
This journal is © The Royal Society of Chemistry 20xx
Please do not adjust margins