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Volumn 48, Issue 8, 2009, Pages 3520-3522

A Heterobimetallic Gallyl Complex Containing an Unsupported Ga-Y Bond

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EID: 65349166750 PISSN: 00201669 EISSN: None Source Type: Journal
DOI: 10.1021/ic900278t Document Type: Article

Times cited : (72)

References (25)

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19
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- Synthesis of 9: A mixture of [K(BIPM)THF)2, 11.12 g, 15.00 mmol) and YI3(THF)35 (10.83 g, 15.00 mmol) in THF (40 mL) was refluxed for 4 h at 80 °C. The mixture was cooled to room temperature and filtered, and volatiles were removed in vacuo to afford the crude solid, which was washed with hexane (3 × 10 mL) and dried in vacuo. Recrystallization from hot THF (15 mL) yielded colorless crystals of 9. Yield: 8.66 g, 64, Anal. Calcd for C39H55I2N2O 2P2Si2Y: C, 44.84; H, 5.31; N, 2.68. Found: C, 44.80; H, 5.28: N, 2.66. 1H NMR (C6D6, 300 K, δ 5 0.33 (m, 18H, CH3, 1.52 (m, br, 4H. CH2-THF, 1.97 (d, 2JHP, 2.75 Hz, 1H, CH, 2JYH not resolved, 3.64 (m, br, 4H, OCH2-THF, 7.22 (m, 12H, olp-Ar-H, 8.11 m, 8H, m
- -1 (Nujol): 1437 (m). 1261 (s), 1245 (m), 1153 (s), 1113 (s), 840 (s), 694 (s), 661 (m).

20
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- Synthesis of 11:1 (0.50 g, 0.83 mmol) was added to a cold, 78 °C) solution of 10 (0.82 g, 0.08 mmol) prepared in situ from 9 and 1 equiv of benzylpotassium. The mixture was allowed to slowly warm to room temperature with stirring over 18 h and filtered. Volatiles were removed in vacuo, and the resulting deep-yellow solid was recrystallized from toluene (10 mL) to afford 11 as yellow crystals. Yield: 0.25 g, 26, Anal. Calcd for (C65H 90GaN4O2P2Si2Y: C, 61.15; H, 7.34; N, 4.53. Found: C, 63.08; H, 7.24; N, 4.51. Carbon analysis was typically low, which we attribute to carbide formation. 1H NMR (benzene-d6, 298 K, δ 0.33 (s, 18H, NSi(CH 3)3, 1.37 (m, 8H, OC2CH2, 1.54 (dd, 3JHH, 6.80 Hz, 24H, CH(CH 3)3, 4.07 (m. 8H, OCH2CH2, 4.20 sept, 3
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25
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