Journal of Inorganic and General Chemistry
ARTICLE
Zeitschrift für anorganische und allgemeine Chemie
stirring. After stirring for 30 minutes the solvent, excess PR3, and
THT is removed in vacuo. The remaining solid was then dissolved in
Elemental analysis (exp): C 26.26%, H 6.10%, (calc) C 26.08%,
H 6.06%.
°
THF and cooled to À 78 C. KGe9(Hyp)3 (211 mg, 147 μmol) is
°
°
dissolved in THF and cooled to À 78 C and then added at À 78 C to
the R3PAuCl solution with a steel cannula while stirring. The mixture
is allowed to reach room temperature over 12 hours while its color
changes from a bright red to a dark red solution. The solvent is
then removed in vacuo and the product extracted with pentane
and crystallized as noted below.
tBu3PAuGe9(Hyp)3
tBu3PAuGe9(Hyp)3 2PtBu3 is crystallized from pentane with a crystal-
°
line yield of 37% at À 30 C.
NMR (C6D6): 1H (300 MHz): 0.51 (s, 81 H, SiMe3), 1.39 (d, 27 H,
3
-C(CH3)3, JH-P =13.26 Hz), 13C{1H} (62.9 MHz): 3.04 (s, Si(CH3)3), 32.61
(d, PC(CH3)3, 2JC-P =5.34 Hz), 40.63 (d, PC(CH3)3, 1JC-P =6.73 Hz), 31P{1H}
(121.5 MHz) 118.71 (s), 29Si-inept-nd (49.7 MHz) À 8.81 (decet, Si-
(SiMe3)3, 2JSi-H =6.44 Hz), À 104.33 (s, Si(SiMe3)3) ppm. Elemental
analysis (exp): C 26.62%, H 6.13%, (calc) C 26.08%, H 6.06%.
Et3PAuGe9(Hyp)3
Et3PAuGe9(Hyp)3 2PEt3 is crystallized from pentane with a crystalline
°
yield of 71% at 6 C.
NMR (C6D6): 1H (300 MHz): 0.51 (s, 81 H, SiMe3), 1.02 (dt, 9 H, CH2CH3,
3JH-H =7.61 Hz, 3JH-P =18.1 Hz), 1.41 (m, 6H PCH2CH3), 13C{1H}
Cy3PAuGe9(Hyp)3
2
(62.9 MHz): 2.95 (s, Si,(CH3)3), 8.56 (d, PCH2CH3, JC-P =1.97 Hz), 19.01
Cy3PAuGe9(Hyp)3 2PCy3 is crystallized from pentane with a crystalline
(d, PCH2CH3, 1JC-P =23.25 Hz), 31P{1H} (121.5 MHz) 79.73 (s), 29Si-inept-
°
yield of 52% at À 30 C.
2
nd (49.7 MHz) À 8.46 (decett, Si(SiMe3)3, JSi-H =6.46 Hz), À 104.17 (s,
1
Si(SiMe3)3) ppm. Elemental analysis (exp): C 23.11%, H 5.70%, (calc)
NMR (C6D6): H (300 MHz): 0.52 (s, 81 H, SiMe3), 1.10–1.27 (m, 9 H),
C 23.15%, H 5.65%.
1.50–1.69 (m, 9 H), 1.76–1.86 (m, 6 H), 2.01–2.11 (m, 6 H), 2.13–2.29
(m, 3 H, PÀ CH-), 13C{1H} (62.9 MHz): 2.96 (s, Si(CH3)3), 26.33 (s), 27.66
(d, J=11.50 Hz), 30.50 (s), 34.68 (d, J=18.03 Hz), 31P{1H} (121.5 MHz)
nPr3PAuGe9(Hyp)3
87.18 (s), 29Si-inept-nd (49.7 MHz) À 8.55 (decet, Si(SiMe3)3, JSi-H
=
2
6.20 Hz), À 104.45 (s, Si(SiMe3)3) ppm. Elemental analysis (exp):
Single crystals of Pr3PAuGe9(Hyp)3 2PnPr3 are obtained from toluene
after extraction of the crude reaction mixture with pentane and
changing the solvent to toluene with a crystalline yield of 54% at
C 29.26%, H 5.95%, (calc) C 28.84%, H 6.14%.
°
À 30 C.
n
iPr2 BuPAuGe9(Hyp)3
NMR (C6D6): 1H (300 MHz): 0.51 (s, 81 H, SiMe3), 0.95 (t, 9 H,
n
iPr2 BuPAuGe9(Hyp)3 2PBuiPr2 is crystallized from pentane with a
PCH2CH2CH3, 3JH-H =7.20 Hz, 1.44–1.65 (m, 12H, PCH2CH2CH3), 13C{1H}
(62.9 MHz): 2.95 (s, Si,(CH3)3), 15.86 (d, PCH2CH2CH3, JC-P =1.97 Hz),
°
crystalline yield of 57% at À 30 C.
NMR (C6D6): 1H (300 MHz): 0.51 (s, 81 H, SiMe3), 1.01 (t, 3 H,
3
2
1
18.27 (d, PCH2CH2CH3, JC-P =3.29 Hz), 29.30 (d, PCH2CH2CH3, JC-P
=
22.66 Hz). 31P{1H} (121.5 MHz) 70.10 (s), 29Si-inept-nd (49.7 MHz)
3
À PCH2CH2CH2CH3, JHH =7.26 Hz), 0.99–1.07 and 1.13–1.21 (m, 12H,
À 8.98 (decett, Si(SiMe3)3, 2JSi-H =6.38 Hz), À 104 (s, Si(SiMe3)3) ppm.
À PCH(CH3)2), 1.36 (m, 2H, À PCH2CH2CH2CH3, 3JHH =7.37 Hz), 1.52–
1.62 (m,
2
H, À PCH2CH2CH2CH3), 1.67–1.81 (m,
2
H,
Elemental analysis (exp): C 24.41%, H 5.82%, (calc) C 24.65%,
H 5.86%.
À PCH2CH2CH2CH3), 2.03 (m, 2H, PCH(CH3)2), 13C{1H} (62.9 MHz): 2.98
(s, Si(CH3)3), 14.04 (s, À PCH2CH2CH2CH3), 18.53 and 19.00 (d, À PCH
(CH3)2), 26.18 (d, À PCH(CH3)2), 31P{1H} (121.5 MHz) 91.11 (s), 29Si-
inept-nd (49.7 MHz) À 8.85 (decet, Si(SiMe3)3, 2JSi-H =6.44 Hz),
À 104.50 (s, Si(SiMe3)3) ppm. Elemental analysis (exp): C 25.54%,
H 5.71%, (calc) C 25.08%, H 6.14%.
iPr3PAuGe9(Hyp)3
iPr3PAuGe9(Hyp)3 2PiPr3 is crystallized from pentane at À 30 C with a
°
crystalline yield of 70.1%.
1
NMR (C6D6): H (300 MHz): 0.51 (s, 81 H, SiMe3), 1.13 (dd, 18 H, PCH
(CH3)2, 3JH-H =7.14 Hz, 2.10 (dq, 1H, PCH(CH3)2, 2JH-P =15.34 Hz, 3JH-H
=
Acknowledgements
7.39 Hz). 13C{1H} (62.9 MHz): 2.99 (s, Si,(CH3)3), 20.03 (d, PCH(CH3)2,
3JC-P =2.867 Hz), 24.29 (d, PCH(CH3)2, 1JC-P =18.36 Hz) 31P{1H}
(121.5 MHz) 99.50 (s), 29Si-inept-nd (49.7 MHz) À 8.84 (decett, Si-
(SiMe3)3, 2JSi-H =7.07 Hz), À 104.43 (s, Si(SiMe3)3) ppm. Elemental
analysis (exp): C 24.93%, H 5.97%, (calc) C 24.65%, H 5.86%.
The authors acknowledge financial support by the Deutsche
Forschungsgemeinschaft through project SCHN738/9-1. We
thank Dr. Claudio Schrenk and Tanja Kunz for helpful discussion
and help during measuring and solving single crystal structures.
Open access funding enabled and organized by Projekt DEAL.
nBu3PAuGe9(Hyp)3
Bu3PAuGe9(Hyp)3 2PnBu3 is crystallized from pentane with a crystal-
Keywords: Germanium · metalloid cluster · gold · ligand ·
molecular structure
°
line yield of 60% at À 30 C.
NMR (C6D6): 1H (300 MHz): 0.51 (s, 81 H, SiMe3), 1.00 (t, 9 H,
PCH2CH2CH2CH3, 3JH-H =7.26 Hz), 1.31–1.43 (m, 6 H, PCH2CH2CH2CH3),
1.53–1.71
PCH2CH2CH2CH3),
(
13C{1H} (62.9 MHz): 2.95 (s, Si(CH3)3), 13.79 (s,
19.99
(s,
PCH2CH2CH2CH3),
22.03
(d,
=
2
PCH2CH2CH2CH3, 2JC-P =14.11 Hz), 24.60 (d, PCH2CH2CH2CH3, JC-P
Int. Ed. 2003 42, 2624–2625.
Angew. Chem. Int. Ed. 2007 46, 5314–5316.
22.71 Hz), 31P{1H} (121.5 MHz) 71.14 (s), 29Si-inept-nd (49.7 MHz)
À 8.17 (decet, Si(SiMe3)3, JSi-H =6.45 Hz), À 104.07 ppm (s, Si(SiMe3)3).
2
Z. Anorg. Allg. Chem. 2021, 1–8
6
© 2021 The Authors. Zeitschrift für anorganische und allgemeine Chemie
published by Wiley-VCH GmbH.
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