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Volumn 26, Issue 2, 2007, Pages 247-249

Complexation of bis(trimethylsilyl)acetylene by decamethylhafnocene to give the hafnacyclopropene Cp*2Hf(η2-Me 3SiC2SiMe3): An unusually strong metal-alkyne interaction

(7) Beweries, Torsten a Burlakov, Vladimir V a,b Bach, Marc A a Arndt, Perdita a Baumann, Wolfgang a Spannenberg, Anke a Rosenthal, Uwe a

a UNIVERSITY OF ROSTOCK (Germany)

b A N NESMEYANOV INSTITUTE OF ORGANOELEMENT COMPOUNDS (Russian Federation)

Author keywords

[No Author keywords available]

Indexed keywords

COMPLEXATION; HAFNIUM COMPOUNDS; OLEFINS; TITANIUM; ZIRCONIUM;

BIS(TRIMETHYLSILYL)ACETYLENE; DECAMETHYLHAFNOCENE; HAFNACYCLOPROPENE; METAL-ALKYNE INTERACTION;

ACETYLENE;

EID: 33846600923 PISSN: 02767333 EISSN: None Source Type: Journal
DOI: 10.1021/om0609259 Document Type: Article

Times cited : (39)

References (14)

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7
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- Preparation of Cp2Hf(PMe3)(Me3SiC≡ CSiMe3, 3, to a suspension of Cp2HfCl2 (3.0 g, 7.90 mmol) and Mg turnings (0.13 g, 8.02 g atom) in 50 mL of THF were added at room temperature bis(trimethylsilyl)acetylene (1.85 mL, 8.19 mmol) and PMe3 (8.0 mL of a 1.0 M solution in THF, 8.00 mmol, The colorless mixture became deep red as it was stirred for 16 h. All volatiles were removed under vacuum, and the residue was extracted with 4 × 15 mL of n-hexane. The solvent was again removed from the obtained solutions, giving the red crude product material, which was recrystallized from n-hexaneATHF to give yellow prisms of 3: yield 2.24 g (51, mp 118 °C dec under Ar. Anal. Calcd for C21H37HfPSi2 (555.15, C, 45.43; H, 6.72. Found: C, 40.27; H, 5.84 (because of partial dissociation of PMe3, better data could not be obtained, IR Nujol mull, cm-1, 124
- +.

8
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- Preparation of 4: a suspension of Cp*2HfCl2 (1.773 g, 3.41 g atom, finely sliced lithium wire (0.103 g, 14.8 mmol, and bis(trimethylsilyl)-acetylene (0.80 mL, 3.56 mmol) in 15 mL of toluene was stirred for 10 days at 60 °C. The resulting dark blue solution was filtered and evaporated to dryness under vacuum. The residue was extracted with 15 mL of n-hexane at 55 °C. The resulting blue solution was filtered and concentrated under vacuum to a total of 10 mL. After the concentrated solution stood for 24 h at -78 °C, dark blue crystals formed, which were separated, washed with cold n-hexane, and dried under vacuum to give complex 4: yield 0.951 g (45, mp 242-243 °C under Ar. Anal. Calcd for C28H 48HfSi2: C, 54.30; H, 7.81. Found: C, 54.54; H, 7.97. IR (Nujol mull, cm-1, 1470 (v(C≡ C, NMR (400 MHz, 298 K, C6D6, 1H, δ 0.26 s, 18H, SiMe 3
- +.

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