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Volumn 26, Issue 7, 2007, Pages 1568-1570

Water-soluble organometallic complexes of tantalum: Can alkyl and aqua ligands coexist in its coordination sphere?

Author keywords

[No Author keywords available]

Indexed keywords

COMPLEXATION; LIGANDS; REACTION KINETICS; SOLUBILITY; TANTALUM COMPOUNDS;

EID: 34047252886     PISSN: 02767333     EISSN: None     Source Type: Journal    
DOI: 10.1021/om0701165     Document Type: Article
Times cited : (25)

References (26)
  • 15
    • 34047260674 scopus 로고    scopus 로고
    • Synthesis of 2: to a solution of [Cp*TaMe(OCH 2)2py]OTf (1; 0.250 g, 0.40 mmol) in 6 mL of CH 2Cl2 was slowly added triflic acid (0.038 mL, and the mixture was stirred for 1 h at room temperature. The solvent was removed under vacuum and the residue washed with 5 mL of pentane to yield 0.230 g (75, of complex 2. 1H NMR (CDCl3, room temperature, 200 MHz, δ 2.34 (s, 15 H, Cp*, 6.32, s, 4 H, CH2, 7.38 (d, 3JH-H, 8.78 Hz, 2 H, Ar, 7.96 (t, 3J H-H, 8.78 Hz, l H, Ar, 13C{1H} NMR (CDCl 3, δ 11.6 (s, Cp*, 83.0 (s, CH2, 117.9 (s, Ar, 129.0 (s, Cp*, 142.4 (s, Ar, 166.4 (s, Aripso, 19F{1H} NMR (CDCl3, δ -77.59 s, CF 3SO3, Anal. Calcd for C19H22O 8F6S
    • 2NTa: C, 30.36; H, 2.95; N, 1.86. Found: C, 30.38; H, 3.11; N, 2.16.
  • 16
    • 34047267087 scopus 로고    scopus 로고
    • Synthesis of 3: to a solution of complex 1 (0.124 g, 0.20 mmol) in THF was added an excess of water, and this mixture was left at room temperature for 12 h. The solvent was removed under vacuum and the residue washed with 5 mL of pentane to yield complex 3 (0.099 g, 77, Colorless crystals of 3 can be obtained by slow diffusion of pentane into a THF solution. 1H NMR (CDCl3, room temperature, 200 MHz, δ -0.41 (s, 3 H, Ta, Me, 2.08 (s, 15 H, Cp*, 2.51 (br, 2 H, H2O, 5.82, d, 2JH-H, 18.33 Hz, 2 H, CH 2, 6.09 (d, 2JH-H, 18.33 Hz, 2 H, CH 2, 7.33 (d, 3JH-H, 8.06 Hz, 2 H, Ar, 7.90 (t, 3JH-H, 8.06 Hz, l H, Ar, 13C{1H} NMR (CDCl3, δ 11.4 (s, Cp*, 37.5 (s, Me, 81.0 (s, CH2, 118.0 (s, Ar, 123.2 (s, Cp*, 140.7 (s, Ar, 165.1 s, Aripso
    • 3SNTa: C, 35.91; H, 4.28; N, 2.20. Found: C, 35.62; H, 4.29; N, 2.15.
  • 22
    • 34047255343 scopus 로고    scopus 로고
    • Synthesis of 4: a suspension of complex 3 (0.103 g, 0.16 mmol) in water was heated to 90°C for 30 min. The solvent was removed under vacuum and the residue washed with 5 mL of Et2O to yield a white compound that was characterized as 4 (0.084 g, 81, Colorless crystals of 4·H2O can be obtained by slow cooling of a saturated solution of 4 in H2O. pH (room temperature, 7.5 mM solution, 4.46. 1H NMR (D2O, room temperature, 200 MHz, δ 1.96 (s, 15 H, Cp*, 5.74, s, 4 H, CH2, 7.36 (d, 3JH-H, 7.5 Hz, 2 H, Ar, 7.94 (t, 3J H-H, 7.5 Hz, 1 H, Ar, 19F NMR (D2O, δ -79.4 (OTf, 13C{1H} NMR (D2O, δ 9.9 (s, Cp*, 79.3 (s, CH2, 118.1 (s, Ar, 124.8 (s, Cp*, 141.4 (s, Ar, 162.6 (s, Aripso, 1H NMR CDCl 3
    • 3SNTa: C, 32.98; H, 4.15; N, 2.13; S, 4.89. Found: C, 33.04; H, 3.88; N, 2.21: S, 5.00.
  • 26
    • 34047249351 scopus 로고    scopus 로고
    • Synthesis of 5: to a solution of [Cp*Ta(OTf) 2(OCH2)2py, 0.323 g, 0.43 mmol) in 6 mL of toluene was added an excess of water (0.5 mL, and the mixture was stirred for 48 h at room temperature. The solvent was filtered off and the residue washed with 5 mL of Et2O and dried under vacuum to yield 0.284 g (84 , of complex 5. pH (room temperature, 7.8 mM solution, 1.81. 1H NMR (D2O, room temperature, 200 MHz, δ 2.00 (s, 15 H, Cp*, 5.93, s, 4 H, CH2, 7.38 (d, 3JH-H, 7.70 Hz, 2 H, Ar, 7.92 (t, 3JH-H, 7.70 Hz, 1 H, Ar, 19F NMR (D2O, δ -79.4 (OTf, 13C, 1H} NMR (D2O, δ 10.1 (s, Cp*, 80.8 (s, CH2, 118.5 (s, Ar, 126.3 (s, Cp*, 142.1 (s, Ar, 162.4 s, Aripso, Anal. Calcd for C19H26O 10F6
    • 2NTa: C, 28.98; H, 3.32; N, 1.77; S, 8.14. Found: C, 29.08; H, 3.35; N, 1.85; S, 7.74.


* 이 정보는 Elsevier사의 SCOPUS DB에서 KISTI가 분석하여 추출한 것입니다.